INKJET INK AND INKJET RECORDING DEVICE

专利摘要:
inkjet ink and inkjet recording device. provide an inkjet ink containing: a water-dispersible colorant; a surfactant; a penetration agent; a water-dispersible resin; a wetting agent containing at least polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity; a compound represented by the general formula (1); Water; and at least one selected from the group consisting of a compound represented by the general formulas (2) to (4), wherein the water-dispersible colorant is at least one selected from the group consisting of a self-dispersing pigment, a pigment dispersed by a pigment dispersing agent, and resin particles each containing a pigment, wherein a total amount of the water-dispersible colorant and the water-dispersible resin is 8% by mass to 35% by mass, and in that a mass ratio of the water-dispersible resin to the water-dispersible colorant is 2 to 8.
公开号:BR112014018176B1
申请号:R112014018176-4
申请日:2013-01-25
公开日:2021-08-10
发明作者:Hiroshi Goto
申请人:Ricoh Company, Ltd；
IPC主号:

专利说明:

Technical Field
[0001] The present invention relates to an inkjet ink and an inkjet recording device. Background of the technique
[0002] An inkjet recording device is a device for forming an image by ejecting a small amount of an ink using bubbles generated by heat, piezoelectric or electrostatic, to deposit the ink onto a recording medium, such as like paper, followed by drying the ink.
[0003] Recently, there have been high demands of inkjet recording devices for industrial use, and inkjet recording devices that can be matched with high speed printing and use of various recording media are desired. As print speed increases, an inkjet printer equipped with a line head is desired.
[0004] In addition, due to environmental safety and environmental protection, there is a need for aqueous inkjet inks.
[0005] PTL 1 discloses an aqueous paint composition containing a pigment, water, an organic solvent, a resin, and a surface adjusting agent for the paint composition, wherein the organic solvent is a compound represented by the following formula general: R1OCH2CH2CONR2R3
[0006] (where R1 is a C1 to C8 alkyl group; and R2 and R3 are each independently a hydrogen atom, a C1 to C6 alkyl group, or a group containing an ether bond in a C1 to alkyl group C6), and in which an amount of the organic solvent is 10% by mass to 49% by mass with respect to a total amount of the water and the organic solvent.
[0007] However, an image having a large amount of aqueous ink deposition, such as a photograph, and a figure, is printed on a commercial printing sheet, gloss and smear fixing ability cannot be achieved at the same time in which it avoids wrinkling and beading. Appropriately, it is currently desired to provide an inkjet ink that can achieve gloss and smudge-fixing ability while avoiding wrinkling and pearling, when an image having a large amount of deposition of an aqueous ink, such as a photograph, and a figure, is formed on a commercial printing sheet. Citation ListPatent Literature
[0008] PTL 1: Japanese Patent Application Open Filed (JP-A) No. 2011-68838 Invention Summary Technical Problem
[0009] The present invention aims to solve the various problems in the art and achieve the following objective. An object of the present invention is to provide an inkjet ink that has excellent gloss and smudge-fixing ability and is capable of preventing the occurrence of wrinkling and pearling even when an image having a large amount of inkjet ink deposition is formed on a commercial printing sheet. Solution to Problem
[0010] The means to solve the aforementioned problem are as follows:
[0011] The inkjet ink of the present invention contains:
[0012] An inkjet ink containing:
[0013] a water-dispersible colorant;
[0014] a surfactant;
[0015] a penetration agent;
[0016] a water-dispersible resin;
[0017] a wetting agent containing at least polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity;
[0018] a compound represented by the following general formula (1);
[0019] water; and
[0020] at least one selected from the group consisting of a compound represented by the following general formula (2), a compound represented by the following general formula (3), and a compound represented by the following general formula (4),
[0021] wherein the water-dispersible colorant is at least one selected from the group consisting of a self-dispersing pigment, a pigment dispersed by a pigment dispersing agent, and resin particles each containing a pigment,
[0022] wherein a total amount of the water-dispersible colorant and the water-dispersible resin is 8% by mass to 35% by mass, and
[0023] wherein a mass ratio of the water-dispersible resin to the water-dispersible colorant is 2 to 8:

[0024] where R1 is an alkyl group from C4 to C6,
General Formula (2)
[0025] where R2 is a hydrogen atom, a methyl group, or an ethyl group, and R3 is an alkyl group from C1 to C4,
General Formula (3)
[0026] where R4 is either a methyl group or an ethyl group, and R5 is a hydroxyl group, a C1 to C8 alkyl group, a cycloalkyl group, or an aryl group,
General Formula (4)
[0027] where R6 and R7 are each independently a C1 to C8 alkyl group. Advantageous Effects of the Invention
[0028] The present invention can solve the various problems in the art, and can provide an inkjet ink that has excellent gloss and smear fixing ability and is able to prevent wrinkling and pearling occurrences even when an image having a large Inkjet ink deposition amount is formed on a commercial printing sheet. Brief Description of Drawings
[0029] FIG. 1 is a view designed to explain an ink jet recording device in the state where a cover of an ink cartridge loading area opens.
[0030] FIG. 2 is a schematic diagram for explaining an entire structure of an inkjet recording device. Description of Modalities (Inkjet ink)
[0031] Inkjet ink contains: a water-dispersible colorant; a surfactant; a penetration agent; a water-dispersible resin, a wetting agent containing at least polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity; a compound represented by the General Formula (1); Water; and at least one selected from the group consisting of a compound represented by the General Formula (2), a compound represented by the General Formula (3), and a compound represented by the General Formula (4). The inkjet ink can additionally contain 3-methoxy-N,N-dimethylpropionamide, and other components, if necessary.
[0032] The water-dispersible colorant is a self-dispersing pigment, a pigment dispersed with a pigment dispersing agent, or resin particles each containing a pigment.
[0033] A total amount of the pigment and a water-dispersible resin in the inkjet ink is 8% by mass to 35% by mass. When the total amount thereof is less than 8% by mass, gloss and smear fixing ability are transmitted as an image having a large amount of inkjet ink deposition is formed on a commercial printing sheet. When the total amount of it is greater than 35% by mass, a resulting ink has poor jet stability.
[0034] A mass ratio of the water-dispersible resin to the pigment is 2 to 8. When the mass ratio of the same is less than 2, gloss as obtained is low when an image having a large amount of deposition. Inkjet ink is formed into a commercial printing sheet. When its mass ratio is more than 8, a resulting ink has poor jet stability.
[0035] The inkjet ink contains at least one selected from the group consisting of the compounds represented by the General Formulas (2) to (4), together with the compound represented by the General Formula (1), and therefore occurrences Ink jet ink wrinkling and pearling can be avoided when an image having a large amount of ink jet ink deposition is formed on a commercial printing sheet. <Compound represented by the General Formula (1)>
The compound represented by the General Formula (1) is appropriately selected depending on the intended purpose without any limitation, and examples thereof include compounds represented by the following chemical formulas (1-1) to (1-3). These can be used alone or in combination.

<Compound represented by the General Formula (2)>
[0037] The compound represented by the General Formula (2) is appropriately selected depending on the intended purpose without any limitation, and examples thereof include compounds represented by the following chemical formulas (2-1) to (2-4). These can be used alone or in combination.

<Compound represented by the General Formula (3)>
The compound represented by the General Formula (3) is appropriately selected depending on the intended purpose without any limitation, and examples thereof include compounds represented by the following chemical formulas (3-1) to (3-6). These can be used alone or in combination.


The compound represented by the General Formula (4) is suitably selected depending on the intended purpose without any limitation, and examples thereof include compounds represented by the following chemical formulas (4-1) to (4-5). These can be used alone or in combination.


[0040] A total amount of the compounds represented by General Formulas (1) to (4) contained in the inkjet ink is preferably 1% by mass to 50% by mass, more preferably 2% by mass to 40% by mass. When the total amount of it is less than 1% by mass, wrinkling or beading may be caused, as an image having a large amount of deposition of an inkjet ink is formed on a commercial printing sheet. When the total amount of it is greater than 50% by mass, the jet stability of a resulting ink may be degraded. <3-methoxy-N,N-dimethylpropionamide>
[0041] The inkjet ink preferably additionally contains a compound (3-methoxy-N,N-dimethylpropionamide) represented by the following chemical formula: CH3OCH2CH2CON(CH3)2
[0042] 3-Methoxy-N,N-dimethylpropionamide has a high boiling point (ie 216°C), high equilibrium moisture content (ie 39.2% by mass) at 23°C, 80% relative humidity, and very low viscosity (1.48 mPa-s) at 25°C. Furthermore, 3-methoxy-N,N-dimethylpropionamide is very easily dissolved in the compounds represented by General Formulas (1) to (4) and in water. Properly, 3-methoxy-N,N-dimethylpropionamide can reduce inkjet ink viscosity, and therefore improve stability
[0043] A jet of the ink amount of 3-methoxy-N,N-dimethylpropionamide in the ink jet ink is preferably 1% by mass to 50% by mass, more preferably 2% by mass to 40% by mass. When the amount of it is less than 1% by mass, jet stability may be insufficient. When the amount of it is greater than 50% by mass, wrinkling or beading may be caused, as an image having a large amount of deposition of an inkjet ink is formed on a commercial printing sheet. <water>
[0044] Water is appropriately selected depending on the intended purpose without any limitation, and examples thereof include pure water or ultra pure water, such as ion exchange water, ultra filtered water, milli-Q water, and distilled water. These can be used alone or in combination.<Wetting agent>
[0045] The wetting agent contains at least polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity, and may additionally contain another wetting agent if necessary.
[0046] The wetting agent may be composed of polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity, alone. <<Polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity>>
[0047] Polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity (may simply be referred to as "polyhydric alcohol" hereinafter) is selected suitably depending on the intended purpose without any limitation, and examples thereof include 1,2,3-butanetriol (38% by mass), 1,2,4-butanetriol (41% by mass), glycerin (49% by mass). ), diglycerin (38% by mass), triethylene glycol (39% by mass), tetraethylene glycol (37% by mass), diethylene glycol (43% by mass), and 1,3-butanediol (35% by mass). These can be used alone or in combination. As for polyhydric alcohol, among the polyhydric alcohol compounds listed above, glycerin and 1,3-butanediol are preferable. Note that the value in parentheses above denotes the equilibrium moisture content at 23°C, 80% relative humidity.
[0048] An amount of the polyhydric alcohol in the inkjet ink is preferably 2% by mass to 50% by mass, more preferably 5% by mass to 40% by mass. When the amount of the same is less than 2% by mass, jet stability may be insufficient. When the amount thereof is greater than 50% by mass, wrinkling or beading may be caused, as an image having a large amount of deposition from an inkjet ink is formed on a commercial printing sheet.
[0049] The equilibrium moisture content of polyhydric alcohol can be determined by storing a Petri dish in which 1 g of the polyhydric alcohol is weighed and placed in a desiccator where the internal temperature and humidity are kept at 23° C ± 1°C, and 80% relative humidity ± 3% relative humidity, respectively, using a saturated aqueous solution of potassium chloride/sodium chloride. The equilibrium moisture content of polyhydric alcohol can then be calculated using the following formula:
[0050] (Mass of moisture absorbed by polyhydric alcohol) / (Mass of polyhydric alcohol + Mass of moisture absorbed by polyhydric alcohol) x 100 <<Other wetting agents>>
[0051] Examples of other wetting agents include: polyhydric alcohol having equilibrium moisture content of less than 30% by mass at 23°C, 80% relative humidity, such as dipropylene glycol, 1,5-pentanediol , propylene glycol, 2-methyl-2,4-pentanediol, ethylene glycol, tripropylene glycol, hexylene glycol, polyethylene glycol, polypropylene glycol, 1,10-hexanediol, 1,2,10-hexanetriol, trimethylol ethane, and trimethylol propane; polyhydric alcohol alkyl ether, such as ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, ethylene glycol mono-2-ethylhexyl ether, and propylene glycol monoethyl ether ; polyhydric alcohol aryl ether, such as ethylene glycol monophenyl ether, and ethylene glycol monobenyl ether; a nitrogen-containing heterocyclic compound such as 2-pyrrolidone, N-methyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolidinone, ε-caprolactam, and Y-butyrolactone; amide, such as formamide, N-methylformamide, N,N-dimethylformamide, and N,N-diethylformamide; amine, such as monoethanol amine, diethanol amine, triethanol amine, N,N-dimethyl monoethanol amine, N-methyl diethanol amine, N-methyl ethanol amine, N-phenyl ethanol amine, and 3-aminopropyl diethyl amine; a sulfur-containing compound such as dimethyl sulfoxide, sulfolane, and thiodiglycol; and others such as propylene carbonate, and ethylene carbonate. These can be used alone or in combination.
[0052] As for the other wetting agents mentioned above, saccharides and derivatives thereof are used appropriately.- Saccharides and Derivatives thereof -
[0053] Saccharides are appropriately selected depending on the intended purpose without any limitation, and examples thereof include: monosaccharides, such as glucose, mannose, fructose, ribose, xylose, arabinose, and galactose; disaccharides, such as maltose, cellobiose, lactose, sucrose, and trahalose; oligosaccharides such as maltotriose; and polysaccharide, such as α-cyclodextrin, and cellulose. These can be used alone or in combination.
[0054] Examples of saccharide derivatives include: saccharide reducing sugars such as sugar alcohol (eg maltitol, and sorbitol); oxidized sugar obtained with aldonic acid or uronic acid; and others such as amino acid, and thio acid. These can be used alone or in combination. <Water-dispersible resin>
[0055] The state of the water-dispersible resin in water is emulsion, which can be a single-layer structure emulsion, core and shell emulsion, or power-supply emulsion.
[0056] A water-dispersible resin is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: a resin synthesized based on condensate, such as polyester, polyurethane, an epoxy resin, polyamide, polyether, a resin ( met)acryl, a siliconized acrylic resin, and a fluororesin; an addition-based synthesized resin such as polyolefin, a polystyrene-based resin, a polyvinyl alcohol-based resin, a polyvinyl ester-based resin, a polyacrylic acid-based resin, and a carboxylic acid-based resin unsaturated; natural, such as cellulose, rosin, and natural rubber. These can be used alone or in combination. Among those listed above, silicone acrylic resin and fluororesin are preferable as a water-dispersible resin. <<Fluororesin>>
[0057] The fluororesin is preferably a fluororesin having a constitutional unit derived from fluoro-olefin, more preferably a fluororesin having a constitutional unit derived from fluoro-olefin and a constitutional unit derived from vinyl ether, and still more preferably n alternating fluoro-olefin and vinyl ether copolymers.
[0058] - Constitutional Unit derived from fluoro-olefin -
[0059] The constitutional unit derived from fluoro-olefin is appropriately selected depending on the intended purpose without any limitation, and examples thereof include the constitutional unit represented by the following formulas: -CF2CF2-, -CF2CF(CF3)-, -CF2CFCl-.- Constitutional unit derived from VinylEther
[0060] The constitutional unity derived from vinyl ether is appropriately selected depending on the intended purpose without any limitation, and examples thereof include the constitutional unity represented by the following formulas:

[0061] Examples of commercial fluororesin products include: FLUONATE (registered trademark) FEM-500, FEM-600, DIC GUARD F-52S, F-90, F-90M, F-90N, and AQUAFURFURAN TE-5A (all manufactured by DIC Corporation); and LUMIFLON FE4300, FE4500, FE4400, AsahiGuard AG-7105, AG-950, AG-7600, AG-7000, and AG-1100 (all manufactured by ASAHI GLASS CO., LTD.).
[0062] A water-dispersible resin can be either a homopolymer or a copolymer.
[0063] A water-dispersible resin can be a resin that can be self-dispersing, or a resin dispersed with a dispersing agent. Among these, a water-dispersible resin obtained by emulsification polymerization or suspension polymerization or unsaturated polyester or polyurethane iomer or monomer is preferred. In the case where a water-dispersible resin is prepared by emulsion polymerization of unsaturated monomers, a water-dispersible resin is obtained by carrying out a reaction in water in which the unsaturated monomers, a polymerization initiator, a surfactant, an agent chain transfer, a chelating agent, a pH regulator, and the like are added. <<Unsaturated monomer>>
[0064] The unsaturated monomer is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: unsaturated carboxylic acid, such as acrylic acid, methacrylic acid, itaconic acid, fumaric acid, and maleic acid; to monofunctional (meth)acrylic acid ester, such as methyl methacrylate, ethyl methacrylate, isopropyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, n-amyl methacrylate, isoamyl methacrylate, n-hexyl methacrylate, 2-ethylhexyl methacrylate, octyl methacrylate, decyl methacrylate, dodecyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, phenyl methacrylate, benzyl methacrylate, glycidyl methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, dimethylaminoethyl methacrylate, methacryloxyethyltrimethyl ammonium salt, 3-methacryloxypropyl methylacrylate acrylate, isopropyl acrylate, n-butyl acrylate, isobutyl acrylate, n-amyl acrylate, isoamyl acrylate, n-hexyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, decyl acrylate, dodecyl acrylate, octadecyl acrylate, cyclohexyl acrylate, phenyl acrylate , benzyl acrylate, glycidyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, dimethylaminoethyl acrylate, and acryloxyethyltrimethyl ammonium salt; polyfunctional (meth)acrylic acid ester such as ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, triethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, 1,3-butylene glycol dimethacrylate, 1,4-butylene glycol dimethacrylate, 1,10-hexanediol dimethacrylate, neopentyl glycol dimethacrylate, dipropylene glycol dimethacrylate, polypropylene glycol dimethacrylate, polybutylene glycol dimethacrylate, 2,2'-bis(4-methacryloxydiethoxyphenyl)propane, trimethylol propane trimethacrylate, trimethylol ethane trimethacrylate, polyethylene glycol diacrylate, triethylene glycol 1,3 diacrylate, glycol diacrylate, 1,4-butylene glycol diacrylate, 1,10-hexanediol diacrylate, neopentyl glycol diacrylate, 1,9-nonanediol diacrylate, polypropylene glycol diacrylate, 2,2'-bis(4-acryloxypropyloxyphenyl)propane, 2.2' -bis(4-acryloxydiethoxyphenyl)propane trimethylolpropane triacrylate, trimethylol ethane triacrylate, tetramethylol methane triacrylate, ditrimethylol tetraacrylate, tetramethylol meta in tetraacrylate, pentaerythritol tetraacrylate, and dipentaerythritol hexaacrylate; (meth)acrylic acid amide, such as acrylamide, methacrylamide, N,N-dimethylacrylamide, methylene bisacrylamide, and 2-acrylamide-2-methylpropane sulfonic acid; a vinyl aromatic compound, such as styrene, α-methylstyrene, vinyl toluene, 4-t-butylstyrene, chlorostyrene, vinyl anisole, vinyl naphthalene, and divinyl benzene; a cyanovinyl compound such as acrylonitrile and methacrylonitrile; a vinyl compound, such as vinyl acetate, vinylidene chloride, vinyl chloride, vinyl ether, vinyl ketone, vinyl pyrrolidone, vinyl sulfonic acid or salts thereof, vinyl trimethoxy silane, and vinyl triethoxy silane; an allyl compound, such as allyl sulfonic acid and salts thereof, allyl amine, allyl chloride, diallyl amine, and diallyldimethyl ammonium salts; olefin, such as ethylene, and propylene; a diene compound such as butadiene and chloroprene; and oligomers, such as a styrene oligomer having a methacryloyl group, a styrene-acrylonitrile oligomer having a methacryloyl group, a methyl methacrylate oligomer having a methacryloyl group, a dimethyl siloxane oligomer having a methacryloyl group, and the polyester oligomer an acryloyl group. These can be used alone or in combination. <<Physical Properties of Water Dispersible Resin>>
[0065] The average particle diameter (D50) of the water-dispersible resin is preferably 50 nm to 200 nm. When the mean particle diameter (D50) thereof is less than 50 nm, the viscosity of the inkjet ink of the present invention may increase. When its mean particle diameter (D50) is greater than 200 nm, a resulting ink can cause poor jet stability.
[0066] A water-dispersible resin has a function of allowing the water-dispersible colorant to set on the paper, and improves the fixing ability of the water-dispersible colorant by forming a film at an ambient temperature. For this reason, a minimum film forming temperature (MFT) of the water-dispersible resin is preferably 30°C or less.
[0067] The glass transition temperature of the water-dispersible resin is preferably -40°C or greater. When a water-dispersible resin glass transition temperature is less than -40°C, the viscosity of a resin film increases, which can provide adhesion (ie dry ink adhesion) to the etched matter.
[0068] An amount of the water-dispersible resin contained in the inkjet ink is preferably 2% by mass to 30% by mass, more preferably 5% by mass to 25% by mass. <Water-dispersible colorant>
[0069] As described above, the water-dispersible colorant is at least one selected from the group consisting of a self-dispersing pigment, a pigment dispersed with a pigment dispersing agent, and resin particles each containing a pigment . <<Pigment>>
[0070] The pigment can be an organic pigment or an inorganic pigment. These can be used alone or in combination. Note that the pigment can be used in combination with a colorant to adjust a color tone.
[0071] The inorganic pigment is appropriately selected depending on the intended purpose without any limitation, and examples thereof include titanium oxide, iron oxide, calcium carbonate, barium sulfate, aluminum hydroxide, barium yellow, cadmium red , chrome yellow, and carbon black. These can be used alone or in combination.
[0072] As for carbon black, carbon black having the DBP absorption number of 25 ml/100g to 400 ml/100g is preferable, more preferably 30 ml/100g to 200 ml/100g, and even more preferably 50 mL/100g to 150 mL/100g.- Organic pigment -
The organic pigment is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: an azo pigment, such as azo lake, an insoluble azo pigment, a condensed azo pigment, and an azo chelate pigment; a polycyclic pigment, such as a phthalocyanine pigment, a perylene pigment, a perinone pigment, an anthraquinone pigment, a quinacridone pigment, a dioxazine pigment, an indigo pigment, a thioindigo pigment, an iso-indolinone pigment, and a quinoftarone pigment; dye chelate, such as basic dye chelate, and acid dye chelate; and others such as a nitro pigment, a nitrous pigment, and aniline black. These can be used alone or in combination. Among these organic pigments, azo pigment and polycyclic pigment are preferable.
Examples of the organic pigment black include: carbon black (C.I. 7 BLACK PIGMENT) such as furnace black, lamp black, acetylene black, and channel black; metals such as copper, iron (C.I. 11 BLACK PIGMENT), and titanium oxide; and organic pigment such as aniline black (BLACK PIGMENT C.I. 1).
[0075] Examples of organic pigment of color, other than black include: YELLOW PIGMENT CI 1, 3, 12, 13, 14, 17, 24, 34, 35, 37, 42 (yellow oxide), 53, 55, 74, 81, 83, 95, 97, 98, 100, 101, 104, 408, 109, 110, 117, 120, 128, 138, 150, 151, 153, and 183; ORANGE PIGMENT C.I. 5, 13, 16, 17, 36, 43, and 51; RED PIGMENT CI 1, 2, 3, 5, 17, 22, 23, 31, 38, 48:2, 48:2 (permanent red 2B(Ca)), 48:3, 48:4, 49:1, 52 :2, 53:1, 57:1(bright carmine 6B), 60:1, 63:1, 63:2, 64:1, 81, 83, 88, 101 (red ocher), 104, 105, 106, 108 (cadmium red), 112, 114, 122 (quinacridone magenta), 123, 146, 149, 166, 168, 170, 172, 177, 178, 179, 185, 190, 193, 209, and 219; VIOLET PIGMENT C.I. 1 (Lake Rhodamine), 3, 5:1, 16, 19, 23, and 38; BLUE PIGMENT CI 1, 2, 15 (phthalocyanine blue), 15:1, 15:2, 15:3 (phthalocyanine blue), 16, 17:1, 56, 60, 63; and CI GREEN PIGMENT 1, 4, 7 , 8, 10, 17, 18, and 36.
The BET specific surface area of the pigment is preferably 10 m2/g to 1500 m2/g, more preferably 20 m2/g to 600 m2/g, and even more preferably 50 m2/g to 300 m2/g.
[0077] Note that, the BET specific surface area of the pigment can be measured by a nitrogen gas absorption method.
[0078] A method for adjusting the BET specific surface area of the pigment is appropriately selected depending on the intended purpose without any limitation, and examples thereof include spherical mill spray, jet mill spray, and a wave treatment ultrasonic.
[0079] As for the pigment, a composite pigment, in which an inorganic pigment is covered with an organic pigment or carbon black, can be used.- Compound pigment -
[0080] A method for producing the composite pigment is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: a method for precipitating an organic pigment under mechanochemistry wherein an inorganic pigment and an organic pigment are mixed and mechanically ground.
[0081] When the composite pigment is produced, a layer of an organosiloxane compound formed from polysiloxane or alkyl silane can optionally be provided between the inorganic pigment and the organic pigment to improve the adhesion between the inorganic pigment and the pigment organic.
The organic pigment constituting the composite pigment is appropriately selected depending on the intended purpose without any limitation, and examples thereof include aniline black, anthraquinone, phthalocyanine blue, phthalocyanine green, diazo, monoazo, pyrantrone, perylene, heterocyclic yellow, quinacridone, and (thio)indigo. Of these, carbon black, a phthalocyanine-based pigment, a quinacridone-based pigment, a monoazo yellow-based pigment, a disazo yellow-based pigment, and a heterocyclic yellow pigment are preferable because of the image density .
[0083] Examples of phthalocyanine blue include copper phthalocyanine blue and derivatives thereof (C.I. BLUE PIGMENT 15:3, 15:4), and aluminum phthalocyanine.
[0084] Examples of quinacridone include ORANGE PIGMENT CI 48, ORANGE PIGMENT CI 49, RED PIGMENT CI 122, RED PIGMENT CI 192, RED PIGMENT CI 202, RED PIGMENT CI 206, RED PIGMENT CI 207, RED PIGMENT CI 209, CI VIOLET PIGMENT 19, and VIOLET PIGMENT CI 42.
Examples of monoazo yellow include C.I. YELLOW PIGMENT 74, C.I. YELLOW PIGMENT 109, C.I. YELLOW PIGMENT 128, and C.I. YELLOW PIGMENT 151.
Examples of disazo yellow include C.I. YELLOW PIGMENT 14, C.I. YELLOW PIGMENT 16, and C.I. YELLOW PIGMENT 17.
Examples of heterocyclic yellow include C.I. YELLOW PIGMENT 117, and C.I. YELLOW PIGMENT 138.
The inorganic pigment constituting the composite pigment is suitably selected depending on the intended purpose without any limitation, and examples thereof include titanium dioxide, silica, alumina, iron oxide, iron hydroxide, and tin oxide.
[0089] The inorganic pigment constituting the composite pigment is preferably spherical particles.
[0090] In the case where organic pigment of color other than black is deposited on the inorganic pigment, the color of the inorganic pigment constituting the composite pigment is preferably clear or white. In the case where organic pigment black or carbon black is deposited on surfaces of inorganic pigment particles, the color of the inorganic pigment constituting composite pigment may be black.
[0091] The average primary particle diameter of the inorganic pigment constituting the composite pigment is preferably 100 nm or smaller, more preferably 5 nm to 50 nm.
[0092] A mass ratio of the organic pigment or carbon black to the inorganic pigment in the composite pigment is preferably 1/3 to 3, more preferably 2/3 to 2. When the mass ratio is less than 1/3 , sufficient image density may not be achieved. When its mass ratio is greater than 3, desirable transparency and color tone may not be achieved.
[0093] Examples of a commercial pigment composite product include a silica/carbon black composite material, a silica/phthalocyanine composite material PB 15:3, a silica/disazo yellow composite material, and a silica/silica composite material/ quinacridone PR122 (all manufactured by TODA KOGYO CORPORATION).
[0094] An amount of pigment in the inkjet ink is preferably 1% by mass to 15% by mass, more preferably 2% by mass to 10% by mass. When the amount of it is less than 1% by mass, sufficient image density may not be achieved. When the amount of the same is greater than 15% by mass, jet stability of a resulting ink may be impaired.<<Self-dispersing pigment>>
[0095] The self-dispersing pigment is appropriately selected depending on the intended purpose without any limitation, provided that it is a pigment each particle surface of which is modified by binding at least one hydrophilic group directly or through another atomic group to the surface thereof, is stably dispersible without a dispersing agent.
[0096] The volume mean particle diameter (D50) of the self-dispersing pigment is preferably 0.01 µm to 0.16 µm.
[0097] As for the self-dispersing pigment, it is preferred that an anionic group or a cationic group has been introduced to each surface of the particles of the same.- Anionic group -
[0098] The anionic group is appropriately selected depending on the intended purpose without any limitation, and examples thereof include groups represented by the following formulas: -COO-M+, -SO3-M+, -PO3H-M+, and -(PO3 )2-M+2 (where M+ is a proton, alkali metal ion, ammonium ion, or organic ammonium ion).
[0099] The alkali metal ion for M+ is appropriately selected depending on the intended purpose without any limitation, and examples thereof include lithium ion, sodium ion, and potassium ion.
[00100] The organic ammonium ion for M+ is appropriately selected depending on the intended purpose without any limitation, and examples thereof include mono-, di-, or trimethyl ammonium ion, mono-, di-, or triethyl ammonium ion, and mono-, di-, or trimethanol ammonium ion.
[00101] A method for introducing the anionic group to each surface of the pigment particles is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: a method in which the pigment is subjected to an oxidation treatment with Sodium hypochlorite; a method by sulfonating the pigment; and a method in which the pigment is allowed to react with diazonium salt.- Cationic group -
[00102] The cationic group is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a combination of a quaternary ammonium group represented by any of the following formulas with a counter ion.

[00103] As for the self-dispersing pigment, carbon black in which a cationic group has been introduced onto the particle surfaces of the same can be used.
[00104] A method for introducing a cationic group to each particle surface of carbon black is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a method in which carbon black is subjected to a treatment with 3-amino-N-ethylpyridinium bromide.
[00105] In the self-dispersing pigment, an ionic group can bind to a surface of the same through another atomic group.- Another atomic group -
[00106] The other atomic group mentioned above is suitably selected depending on the intended purpose without any limitation, and examples thereof include a C1 to C12 alkyl group, a phenyl group, which may be substituted with a substituent, and a group naphthyl, which may be substituted with a substituent.
[00107] The ionic group bonded through the other atom group mentioned above is appropriately selected depending on the intended purpose without any limitation, and examples thereof include groups represented by the following formulas:- CH2CH2COO-M+(where, M+ is ion of alkali metal or quaternary ammonium ion) - R-SO3-M+
[00108] (where, R is a phenylene group, and M+ is alkali metal ion or quaternary ammonium ion).
[00109] A geminal bisphosphonic group or geminal bisphosphonic acid salt group is preferably introduced to each surface of self-dispersing pigment particles. As a result of this modification, jet stability of a resulting ink can be guaranteed.<<Pigment Dispersing Agent>>
[00110] The pigment dispersing agent is preferably an anionic surfactant, or a nonionic surfactant having an HLB number from 10 to 20.- Anionic surfactant -
[00111] The anionic surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include polyoxyethylene alkyl ether acetic acid salt, alkylbenzene ammonium sulfonate, sodium alkylbenzene sulfonate, calcium alkylbenzene sulfonate, calcium disulfonate alkyldiphenyl ammonium ether, sodium alkyldiphenyl ether disulfonate, calcium alkyldiphenyl ether disulfonate, sodium dialkyl succinate sulfonate, a sodium salt of naphthalene sulfonate condensate - formalin, an ammonium salt of polyoxyethylene phenyl ether sulfuric acid ester polycyclic, a sodium salt of polyoxyethylene phenyl ether sulfuric acid ester, polycyclic acid salt, polyoxyethylene alkyl ether sulfate salt, and oleic acid salt. These can be used alone or in combination. Of these, sodium dioctylsulfosuccinate, and polyoxyethylene styrene phenyl ether ammonium sulfonate are preferable.- Nonionic surfactant having HLB Number from 10 to 20
[00112] The nonionic surfactant having an HLB number from 10 to 20 is appropriately selected depending on the intended purpose without any limitation, and examples thereof include polyoxyethylene alkyl ether, polyoxyalkylene alkyl ether, polyoxyethylene phenyl polycyclic ether, acid ester sorbitan fatty acid, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkylphenyl ether, polyoxyethylene alkyl amine, polyoxyethylene alkyl amide, and acetylene glycol. These can be used alone or in combination. Among these, polyoxyethylene lauryl ether, polyoxyethylene-β-naphthyl ether, polyoxyethylene sorbitan monooleate, and polyoxyethylene styrene phenyl ether are preferred.
[00113] When the pigment is dispersed using the pigment dispersing agent, a mass ratio of the pigment dispersing agent to the pigment is preferably 0.01 to 1, more preferably 0.10 to 0.50. When the mass ratio is less than 0.01, the pigment's dispersibility may be low. When its mass ratio is more than 1, color enhancement can occur.
[00114] A method for dispersing the pigment using the pigment dispersing agent is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a method, in which a pigment dispersing agent is dissolved in water, followed by adding and dispersing the pigment therein.
[00115] A device used to disperse the pigment is suitably selected depending on the intended purpose without any limitation, and examples thereof include: a high speed stirrer, such as a homogenizer; a disperser using beads, such as a bead mill and a ball mill; a kneading disperser using shear force, such as a roller mill; and an ultrasonic disperser.
[00116] Note that, it is preferred that, after pigment dispersion, coarse particles can be removed by means of a filter, or a centrifuge if necessary.
[00117] When the pigment is dispersed using the pigment dispersing agent, the volume mean particle diameter (D50) of the pigment in water is preferably 150 nm or less, more preferably 100 nm or less. When the volume mean particle diameter (D50) of the same is greater than 150 nm, a resulting inkjet stability may be impaired.
[00118] The dispersing agent pigment is preferably used in combination with a water-soluble resin. Use of the water-soluble resin in combination with the pigment dispersing agent can improve the dispersion stability of the pigment.- Water-soluble resin -
[00119] The water-soluble resin is appropriately selected depending on the intended purpose without any limitation, and examples thereof include an α-olefin - maleic anhydride copolymer salt, a styrene - (meth)acrylic acid copolymer salt , a polyurethane salt, and a polyester salt. These can be used alone or in combination.
[00120] The α-olefin - maleic anhydride copolymer, styrene - (meth)acrylic acid copolymer, polyurethane, and polyester are neutralized using an equal or greater amount, more preferably 1.0 times to 1.5 times an amount of base to improve water solubility.-- Base -
[00121] The base is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: alkali metal hydroxide, such as sodium hydroxide, potassium hydroxide, and lithium hydroxide; amine alcohol, such as triethanol amine, diethanol amine, N-methyldiethanol amine, 2-amino-2-ethyl-1,3-propanediol, and choline; and others, such as ammonium, triethyl amine, and morpholine.
[00122] Examples of a commercial α-olefin-maleic anhydride copolymer product include T-YP110, T-YP111, T-YP112, and T-YP113 (all manufactured by SEIKO PMC CORPORATION).
[00123] Examples of a commercial styrene - (meth)acryl copolymer product include: JC-05 (manufactured by SEIKO PMC CORPORATION); and ARUFON (registered trademark) UC-3900, ARUFON UC-3910, and ARUFON UC-3920 (all manufactured by TOAGOSEI CO., LTD.).
[00124] Examples of a commercial polyurethane product include TAKELAC (registered trademark) W-5025, TAKELAC W-6010, and TAKELAC W-5661 (all manufactured by Mitsui Chemicals, Inc.).
[00125] Examples of a commercial polyester product include: NICHIGO POLYESTER (registered trademark) W-0030, NICHIGO POLYESTER W-0005S30WO, and NICHIGO POLYESTER WR-961 (all manufactured by Nippon Synthetic Chemical Industry Co., Ltd.); and PESRESIN (registered trademark) A-210, and PESRESIN A-520 (manufactured by TAKAMATSU OIL & FAT CO., LTD.).
[00126] An acid value of the water-soluble resin before neutralization is preferably 40 mg KOH/g to 400 mg KOH/g, more preferably 60 mg KOH/g to 350 mg KOH/g. When the acid value of the same is less than 40 mg KOH/g, the dispersion stability of the pigment may be impaired. When the acid value of the same is greater than 400 mg KOH/g, jet stability of a resulting ink and pigment dispersion stability may be impaired.
[00127] The mass average molecular weight of the water-soluble resin before neutralization is preferably 20,000 or less, more preferably 5,000 to 20,000. When the mass average molecular weight of the same is less than 5,000, pigment dispersion stability may be impaired. When the mass average molecular weight of the same is greater than 20,000, a resulting ink jet stability and pigment dispersion stability may be impaired.
[00128] When the pigment is dispersed using the pigment dispersing agent, a mass ratio of the water-soluble resin, which is used in combination with the pigment dispersing agent, to the pigment is preferably 0.01 to 1, more preferably 0.05 to 0.50. When the mass ratio of the same is less than 0.01, pigment dispersion stability may be impaired. When its mass ratio is greater than 1, a resulting inkjet stability may be impaired. <<Resin particles each containing Pigment>>
[00129] In the resin particle containing a pigment, the pigment can be dispersed in the resin particle, or deposited on a surface of the resin particle.
[00130] A resin that constitutes the resin particles is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a vinyl-based resin, a polyester-based resin, and a polyurethane-based resin . Of these, vinyl-based resin and polyester-based resin are preferable (see, for example, JP-A Nos. 2000-53897 and 2001-139849). <Surfactant>
[00131] The surfactant is appropriately selected depending on the intended purpose without any limitation, provided it is able to improve leveling, and examples thereof include a fluorosurfactant, a silicone surfactant, an acetylene alcohol surfactant, an anionic surfactant, and a non-ionic surfactant. These can be used alone or in combination. Among these, a silicone based surfactant, a fluorine based surfactant, and an acetylene alcohol based surfactant are preferable. <<Fluoride-based surfactant>>
[00132] In fluorine-based surfactant, the number of carbon atoms substituted with a fluoro group is preferably 2 to 16, more preferably 4 to 16. When the number of carbon atoms is less than 2, desirable leveling may not be achieved. When the number of carbon atoms is more than 16, a resulting ink jet stability may be impaired.
[00133] The fluorine-based surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a fluorine-based anionic surfactant, a fluorine-based nonionic surfactant, an amphoteric fluorine-based surfactant, and a fluorine-based oligomer-type surfactant. These can be used alone or in combination.- Anionic fluoride based surfactant -
[00134] The fluorine-based anionic surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include perfluoroalkyl sulfonic acid, perfluoroalkyl sulfonic acid salt, perfluoroalkyl carboxylic acid, perfluoroalkyl carboxylic acid salt, an ester salt of perfluoroalkyl phosphoric acid, and a polyoxyalkylene ether sulfuric acid ester salt having a perfluoroalkyloxy group in its side chain.
[00135] A fluorine-based anionic surfactant counter ion is appropriately selected depending on the intended purpose without any limitation, and examples thereof include lithium ion, sodium ion, potassium ion, ammonium ion, monoethanol ammonium ion, diethanol ammonium ion, and ammonium ion triethanol.
[00136] As for the fluorine-based anionic surfactant, compounds represented by the following General Formulas (5) to (8) are suitably used.
General Formula (5)
[00137] In General Formula (5), Rf represents a mixture of hydrophobic groups containing fluorine represented by the following structural formulas; and A is -SO3-M+, -COO-M+, or -PO3-M+, where M+ is a proton, lithium ion, sodium ion, potassium ion, ammonium ion, monoethanol ammonium ion, diethanol ammonium ion, or triethanol ammonium ion.

General Formula (6)
[00138] In the General Formula (6), Rf' represents a fluorine-containing group represented by the following formula; M+ is a proton, lithium ion, sodium ion, potassium ion, ammonium ion, monoethanol ammonium ion, diethanol ammonium ion, or triethanol ammonium ion; n is 1 or 2; m represents 2-n.

[00139] In the formula above, n is an integer from 3 to 10.
General Formula (7)
[00140] In General Formula (7), Rf' represents the same as Rf' in General Formula (6); and M+ is a proton, lithium ion, sodium ion, potassium ion, ammonium ion, monoethanol ammonium ion, diethanol ammonium ion, or triethanol ammonium ion.
General Formula (8)
[00141] In the General Formula (8), Rf’ represents the same as Rf’ in the General Formula (6); and M+ is a proton, lithium ion, sodium ion, potassium ion, ammonium ion, monoethanol ammonium ion, diethanol ammonium ion, or triethanol ammonium ion.- Fluorine-based non-ionic surfactant -
[00142] The fluorine-based nonionic surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include perfluoroalkyl phosphoric acid ester, perfluoroalkyl ethylene oxide adduct, and polyoxyalkylene ether having a perfluoroalkyloxy group in its chain side. Among these, polyoxyalkylene ether having a perfluoroalkyloxy group in its side chain is preferable because of its low foaming ability, and compounds represented by the following General Formulas (9) to (12) are more preferable.
General Formula(9)
[00143] In the General Formula (9), m is an integer from 0 to 10, and n is an integer from 0 to 40.
General Formula (10)
[00144] In the General Formula (10), n is an integer from 2 to 6; m is an integer from 15 to 50; and R is a C11 to C19 alkyl group or a group represented by the following general formula.

[00145] In the General Formula above, p is an integer from 2 to 6.
General Formula (11)
[00146] In General Formula (11), Rf represents the same as Rf in General Formula (5); en is an integer from 5 to 20.
General Formula (12)
[00147] In the General Formula (12), Rf’ represents the same as Rf’ in the General Formula (6); and n is an integer from 1 to 40.
[00148] A ratio of a molecular weight of the polyoxyethylene group to a molecular weight of the fluoroalkyl group in the compound represented by the General Formula (9) is preferably 2.2 to 10. When the ratio thereof is less than 2.2, or more than 10, a resulting paint may not be able to achieve desirable leveling.
[00149] The compound represented by the General Formula (10) is preferably compounds represented by the following chemical formulas (10-1) to (10-22) by virtue of leveling, more preferably compounds represented by the chemical formulas (10-1) to ( 10-3), and (10-14) to (1022).a. C4F9CH2CH(OH)CH2O(CH2CH2O)21C12H25 (10-1)b. C4F9CH2CH(OH)CH2O(CH2CH2O)25C12H25 (10-2)c. C4F9CH2CH(OH)CH2O(CH2CH2O)30C12H25 (10-3) d. C4F9CH2CH(OH)CH2O(CH2CH2O)20C14H29 (10-4)e. C4F9CH2CH(OH)CH2O(CH2CH2O)30C14H29 (10-5)f. C4F9CH2CH(OH)CH2O(CH2CH2O)20C16H33 (10-6)g. C4F9CH2CH(OH)CH2O(CH2CH2O)23C16H33 (10-7)h. C4F9CH2CH(OH)CH2O(CH2CH2O)25C16H33 (10-8)i. C4F9CH2CH(OH)CH2O(CH2CH2O)30C16H33 (10-9)j. C4F9CH2CH(OH)CH2O(CH2CH2O)40C16H33 (10-10)k. C4F9CH2CH(OH)CH2O(CH2CH2O)20C18H37 (10-11)1. C4F9CH2CH(OH)CH2O(CH2CH2O)30C18H37 (10-12)m. C4F9CH2CH(OH)CH2O(CH2CH2O)40C18H37 (10-13)n. C4F9CH2CH(OH)CH2O(CH2CH2O)23CH2CH(OH)CH2C4F9
[00150] (10-14)a. C4F9CH2CH(OH)CH2O(CH2CH2O)35CH2CH(OH)CH2C4F9(10-15)b. C4F9CH2CH(OH)CH2O(CH2CH2O)45CH2CH(OH)CH2C4F9(10-16)c. C6F13CH2CH(OH)CH2O(CH2CH2O)21C12H25 (10-17)d. C6F13CH2CH(OH)CH2O(CH2CH2O)25C12H25 (10-18)e. C6F13CH2CH(OH)CH2O(CH2CH2O)30C12H25 (10-19)f. C6F13CH2CH(OH)CH2O(CH2CH2O)23CH2CH(OH)CH2C6F13(10-20)g. C6F13CH2CH(OH)CH2O(CH2CH2O)35CH2CH(OH)CH2C6F13(10-21)h. C6F13CH2CH(OH)CH2O(CH2CH2O)45CH2CH(OH)CH2C6F13(10-22) - Amphoteric surfactant based on fluor -
[00151] The fluorine-based amphoteric surfactant is preferably a compound represented by the following general formula (13).
General Formula (13)
[00152] In General Formula (13), Rf represents the same as Rf in General Formula (5).- Fluorine-based surfactant of oligomer type -
[00153] The fluorine-based oligomer-type surfactant is preferably compounds represented by General Formulas (14) to (15).
General Formula (14)
[00154] In the General Formula (14), Rf is a group represented by the following general formula:
(in the General Formula above, n is an integer from 1 to 4);
[00155] A is a group represented by any of the following General Formulas: -COO-M+, -SO3-M+, -SO4-M+, -PO4-M+ (in the General Formulas above, M+ is an alkali metal ion (for example , sodium ion, and potassium ion) or a quaternary ammonium group (eg, triethyl ammonium, and triethanol ammonium)); eq is an integer from 1 to 6.
The. General Formula (15)
[00156] In General Formula (15), Rf' is a perfluoroalkyl group from C2 to C22; m is an integer from 6 to 25; and 1 and n are each independently an integer from 1 to 10.
[00157] Examples of a commercial fluorine-based surfactant product include: SURFLON (registered trademark) S-111, S-112, S-113, S-121, S-131, S-132, S-141, S-145 (all manufactured by AGC SEIMI CHEMICAL CO., LTD.); FLOURAD FC-93, FC-95, FC-98, FC-129, FC-135, FC-170C, FC-430, FC-431 (all manufactured by Sumitomo 3M Limited); MEGAFACE (registered trademark) F-470, F-1405, F-474 (all manufactured by DIC Corporation); ZONYL (registered trademark) TBS, FSP, FSA, FSN-100, FSN, FSO-100, FSO, FS-300, UR (all manufactured by Du Pont Co., Ltd.); FT-110, FT-250, FT-251, FT-400S, FT-150, FT-400SW (all manufactured by NEOS COMPANY LIMITED); and PolyFox (registered trademark) PF-136A, PF-156A, PF-151N, PF-154, PF-159 (manufactured by Omnova Solutions, Inc.); eUNIDYNE (registered trademark) DSN-403N (manufactured by DAIKIN INDUSTRIES, LTD.).<<Silicone-based surfactant>>
[00158] The silicone based surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include side chain modified polydimethylsiloxane, both end-modified polydimethylsiloxane, one-end modified polydimethylsiloxane, and both end-modified polydimethylsiloxane modified and modified side chain. These can be used alone or in combination. Among these, a polyether-modified silicone-based surfactant having as a modified group, a polyoxyethylene group and/or a polyoxyethylene polyoxypropylene group is preferred.-Polyether-modified silicone-based surfactant-
[00159] The polyether-modified silicone-based surfactant is preferably a compound represented by General Formula (16).

General Formula (16) X = -R(QzH^O), (C3HEO)b R'
[00160] In General Formula (16), R represents an alkylene group; R' represents an alkyl group; and m, n, a and b each independently represent an integer.
[00161] Examples of a commercial polyether-modified silicone surfactant product include: KF-618, KF-642, and KF-643 (all manufactured by Shin-Etsu Chemical Co., Ltd.); EMALEX-SS-5602, and SS-1906EX (all manufactured by Nihon-Emulsion Co., Ltd.); FZ-2105, FZ-2118, FZ-2154, FZ-2161, FZ-2162, FZ-2163, and FZ-2164 (all manufactured by Dow Corning Toray Co., Ltd.); BYK-33, and BYK-387 (all manufactured by BYK Japan K.K.); and TSF4440, TSF4452, and TSF4453 (all manufactured by Momentive Performance Materials Inc.).
[00162] <<Acetylene alcohol based surfactant>>
[00163] The acetylene alcohol based surfactant is appropriately selected depending on the intended purpose without any limitation, but a compound represented by the following chemical formula is preferred:
and compounds represented by the following General Formulas (17) to (18). These can be used alone or in combination.
The. General Formula (17)
[00164] In the General Formula (17), men each independently represents an integer.
General Formula (18)
[00165] In General Formula (18), R1 and R2 are each independently an alkyl group.
[00166] Examples of a commercial acetylene alcohol based surfactant product include: Dynol (registered trademark) 604, and Dynol 607 (both manufactured by Air Products Japan Inc.); SURFYNOL (registered trademark)104, SURFYNOL 420, SURFYNOL 440, and SURFYNOL SE (all manufactured by Nissin Chemical Industry Co., Ltd.); and OLFINE E1004, OLFINE E1010, OLFINE EXP.4001, OLFINE EXP.4200, OLFINE EXP.4051F, and OLFINE EXP.4123 (all manufactured by Nissin Chemical Industry Co., Ltd.). <<Anionic surfactant>>
[00167] The anionic surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include an acetic acid salt of polyoxyethylene alkyl ether, dodecylbenzene sulfonic acid salt, succinic ester sulfonic acid salt, lauryl acid salt , and a polyoxyethylene alkyl ether sulfate salt. These can be used alone or in combination. <<Non-ionic surfactant>>
[00168] The nonionic surfactant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include polyoxyethylene alkyl ether, polyoxypropylene polyoxyethylene alkyl ether, polyoxyethylene alkyl ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkylphenyl ether, polyoxyethylene alkyl amine , and polyoxyethylene alkyl amide. These can be used alone or in combination.
[00169] An amount of the surfactant in the inkjet ink is preferably 0.001% by mass to 5% by mass, more preferably 0.05 to 1% by mass. When the amount of the same is less than 0.001% by mass, a resulting paint may not be able to achieve the desired level. When the same amount is greater than 5% by mass, sufficient image density may not be achieved with a resulting ink. <penetration agent>
[00170] The penetration agent is appropriately selected depending on the intended purpose without any limitation, and examples thereof include Polyol from C8 to C11, and Polyol ether from C8 to C11. These can be used alone or in combination. The penetrating agent is preferably a compound represented by the following general formula (19), and more preferably 2-ethyl-1,3-hexanediol, and 2,2,4-trimethyl-1,3-pentanediol.
General Formula (19)
[00171] In General Formula (19), R' is a methyl group or an ethyl group; R' is a hydrogen atom or a methyl group; and R' is an ethyl group or a propyl group.
The penetration agent preferably has a solubility of 0.2% by mass to 5.0% by mass for water at 25°C.
[00173] The solubilities of 2-ethyl-1,3-hexanediol and 2,2,4-trimethyl-1,3-pentanediol for water at 25°C are 4.2% by mass and 2.0% by mass , respectively.
[00174] Other examples of polyol from C8 to C11 propanediol, 3,3-dimethyl-1,2-butanediol, 2,2-diethyl-1,3-propanediol, 2-methyl-2-propyl-1,3-propanediol , 2,4-dimethyl-2,4-pentanediol, 2,5-dimethyl-2,5-hexanediol, and 5-hexene-1,2-diol.
[00175] Examples of Polyol Ether from C8 to C11 include diethylene glycol monophenyl ether, ethylene glycol monophenyl ether, ethylene glycol monoallyl ether, diethylene glycol monophenyl ether, diethylene glycol monobutyl ether, propylene glycol monobutyl ether, and tetraethylene glycol chlorophenyl ether.
[00176] Other examples of the penetration agent include lower alcohol such as ethanol.
[00177] An amount of the inkjet ink penetrating agent is preferably 0.1% by mass to 4.0% by mass. When the amount of it is less than 0.1% by mass, color spots may occur. When the amount of the same is greater than 4.0% by mass, sufficient jet stability and image density may not be achieved. <Other components>
[00178] Other components are appropriately selected depending on the intended purpose without the intended purpose, and examples thereof include a pH regulator, foam inhibitor (anti-foaming agent), a preservative and fungicide, a chelating reagent, an anti-rust agent, an antioxidant, and an ultraviolet absorber. These can be used alone or in combination.<<pH Regulator>>
[00179] The pH regulator is appropriately selected depending on the intended purpose without any limitation, provided that it is capable of controlling the pH to the range of 7 to 11. Examples of the same include: alcohol amine, such as diethanol amine, triethanol amine, and 2-amino-2-ethyl-1,3-propanediol; alkali metal hydroxide, such as lithium hydroxide, sodium hydroxide, and potassium hydroxide; ammonium hydroxide, such as ammonium hydroxide, and quaternary ammonium hydroxide; phosphonium hydroxide, such as quaternary phosphonium hydroxide; and alkali metal carbonate, such as lithium carbonate, sodium carbonate, and potassium carbonate. These can be used alone or in combination. <<Foam inhibitor>>
[00180] The foam inhibitor is suitably selected depending on the intended purpose without any limitation, but preferably it is a compound represented by the following general formula (20).

[00181] In General Formula (20), R1 and R2 each independently represent a C3 to C6 alkyl group; R3 and R4 each independently represent a methyl group or an ethyl group; and n is an integer from 1 to 6.
[00182] Examples of the compound represented by General Formula (20) include 2,4,7,9-tetramethyldecane-4,7-diol, and 2,5,8,11-tetramethyldodecane-5,8-diol. Of these, 2,5,8,11-tetramethyldodecane-5,8-diol is preferable.
[00183] An amount of the foam inhibitor in the inkjet ink is preferably 0.01% by mass to 10% by mass, more preferably 0.1% by mass to 5% by mass. When the amount of the same is less than 0.01% by mass, a foaming inhibiting effect cannot be achieved. When the amount of the same is greater than 10% by mass, a resulting inkjet stability may be impaired. <<Preservative and Fungicide>>
The preservative and fungicide are appropriately selected depending on the intended purpose without any limitation, and examples thereof include sodium dehydroacetate, sodium sorbate, sodium-2-pyridinethiol-1-oxide, sodium benzoate, and pentachlorophenol of sodium. These can be used alone or in combination.<<Chelating Reagent>>
The chelating reagent is appropriately selected depending on the intended purpose without any limitation, and examples thereof include sodium tetra-ethylenediamine acetate, sodium nitrilotriacetate, sodium hydroxyethylethylene diaminetriacetate, sodium diethylenetriaminepentaacetate, and sodium uramildiacetate. These can be used alone or in combination. <<Anti-rust agent>>
[00186] The anti-rust agent is appropriately selected depending on the intended purpose without any limitation, and examples thereof include acid sulfite salt, sodium thiosulfate, ammonium thiodiglylate, diisopropyl ammonium nitride, pentaerythritol tetranitrate, and dicyclohexyl ammonium nitride . These can be used alone or in combination. <<Antioxidant>>
[00187] The antioxidant is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: a phenol-based antioxidant such as butylated hydroxyanisole, 2,10-di-tert-butyl-4-ethyl phenol , stearyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, 2,2'-methylenebis(4-methyl-10-tert-butylphenol), 2,2'-methylenebis(4-ethyl) -10-tert-butylphenol), 4,4'-butylidenebis(3-methyl-10-tert-butylphenol), 3,9-bis[1,1-dimethyl-2-[β-(3-tert-butyl- 4-hydroxy-5-methylphenyl)propionyloxy]ethyl]2,4,8,10-tetraoxaspiro[5.5]undecane, 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 1,3,5-trimethyl-2,4,10-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, and tetrakis[methylene-3-(3',5'-di- tert-butyl-4'-hydroxyphenyl)propionate]methane; an amine-based antioxidant such as phenyl-β-naphthyl amine, α-naphthyl amine, N,N'-di-sec-butyl-p-phenylene diamine, phenothiazine, N,N'-diphenyl-p-phenylene diamine , 2,10-di-tert-butyl-p-cresol, 2,10-di-tert-butylphenol, 2,4-dimethyl-10-tert-butyl-phenol, butyl-hydroxyanisole, 2,2'-methylenebis( 4-methyl-10-tert-butylphenol), 4,4'-butylidenebis(3-methyl-10-tert-butylphenol), 4,4'-thiobis(3-methyl-10-tert-butylphenol), tetrakis[methylene -3(3,5-di-tert-butyl-4-dihydroxyphenyl)propionate]methane, and 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane; a sulfur-based antioxidant, such as dilauryl-3,3'-thiodipropionate, distearylthiodipropionate, laurylstearylthiodipropionate, dimyristyl-3,3'-thiodipropionate, distearyl-β,β'-thiodipropionate, 2-mercaptobenzoimidazole, and dilauryl sulfide; and a phosphorus-based antioxidant such as triphenyl phosphate, octadecyl phosphate, tri-isodecyl phosphate, trilauryltrithio phosphate, and trinonylphenyl phosphate. These can be used alone or in combination. <<Ultraviolet absorber>>
[00188] The ultraviolet absorber is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: an ultraviolet absorber based on benzophenone, such as 2-hydroxy-4-n-octoxybenzophenone, 2-hydroxy -4-n-dodecyloxybenzophenone, 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, and 2,2',4,4'-tetrahydroxybenzophenone; a benzotriazole based ultraviolet absorber such as 2-(2'-hydroxy-5'-tert-octylphenyl)benzotriazole, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 2-(2'-hydroxy -4'-octoxyphenyl)benzotriazole, and 2-(2'-hydroxy-3'-tert-butyl-5'-methylphenyl)-5-chlorobenzotriazole; a salicylate-based ultraviolet absorber such as phenyl salicylate, p-tert-butylphenyl salicylate, and p-octylphenyl salicylate; a cyanoacrylate-based ultraviolet absorber such as ethyl-2-cyano-3,3'-diphenyl acrylate, methyl-2-cyano-3-methyl-3-(p-methoxyphenyl)acrylate, and butyl-2-cyano -3-methyl-3-(p-methoxyphenyl)acrylate; and a complex nickel salt based ultraviolet absorber such as nickel bis(octylphenyl) sulfide, nickel(II) 2,2'-thiobis(4-tert-octylferrate)-n-butyl amine, nickel(II) 2, 2'-thiobis(4-tert-octylferrate)-2-ethylhexyl amine, and nickel(II) 2,2'-thiobis(4-tert-octylferrate)triethanol amine. These can be used alone or in combination. <Inkjet Ink Physical Properties>
[00189] The inkjet ink viscosity at 25°C is preferably 5 mPa-s to 25mPa-s. When the viscosity of the same is less than 5 mPa-s, sufficient image density may not be achieved. When the viscosity of the same is greater than 25mPa-s, a resulting inkjet stability may be impaired.
[00190] The viscosity of inkjet ink at 25°C can be measured by means of a RE-550L viscometer (manufactured by Toki Sangyo Co., Ltd.).
[00191] The pH of the inkjet ink at 25°C is preferably 4 to 12, and by virtue of the miscibility with the water-dispersible colorant, more preferably 6 to 11, even more preferably 7 to 10. When the pH of the even if it is less than 4, or greater than 12, the dispersion state of the water-dispersible resin can be destroyed, or a molecular chain thereof can be cleaved due to hydrolysis or the like.
[00192] The pH of inkjet ink at 25°C can be measured by an HM-30R pH meter (manufactured by DKK-TOA CORPORATION).
[00193] The static surface tension of inkjet ink at 25°C is preferably 30 mN/m or less, more preferably 28 mN/m or less. When static surface tension is greater than 30 mN/m, beading may be caused.
[00194] The dynamic surface tension of an inkjet ink with a surface lifetime of 15 ms as measured by the maximum bubble pressure method is preferably 35 mN/m or less, more preferably 33 mN/m or any less. When the dynamic surface tension of the same is greater than 35 mN/m, beading can occur as an image having a large amount of deposition of an inkjet ink is formed on a commercial printing sheet.
[00195] The dynamic surface tension of the inkjet ink with the surface lifetime of 15 ms as measured by the maximum bubble pressure method can be measured by means of SITA DynoThester (manufactured by SITA Messtechnik GmbH). <Inkjet ink production method>
[00196] Inkjet ink can be produced by dispersing or dissolving, in water, a composition containing a water-dispersible colorant, a surfactant, a penetration agent, a water-dispersible resin, polyhydric alcohol having a equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity, one compound represented by the General Formula (1), and at least one selected from the group consisting of compounds represented by the General Formulas (2) to (4), and optionally other components.
[00197] A device for dispersing or dissolving the composition in water is appropriately selected depending on the intended purpose without any limitation, and examples thereof include a sand mill, a homogenizer, a ball mill, a paint agitator, and a disperser ultrasonic.
[00198] In the course of inkjet ink production, stirring and mixing may optionally be carried out by means of a stirrer having a stirring blade, a magnetic stirrer, or a high-speed disperser. inkjet)
[00199] The inkjet recording device is a device containing an inkjet head configured to eject the inkjet ink, and can additionally contain other units if necessary.
[00200] An inkjet recording device system of the present invention is suitably selected depending on the intended purpose without any limitation, and examples thereof include a system for scanning a head, and a system for using heads that are aligned in a row.<Inkjet Head>
[00201] The inkjet head is configured to apply stimuli (energy) to the inkjet ink and eject the inkjet ink, to thereby form an image of a recording medium.
[00202] The inkjet head is appropriately selected depending on the intended purpose without any limitation, and examples thereof include: a piezo inkjet head that uses a piezoelectric element configured to pressurize ink into an ink channel to deform an oscillating plate constituting an ink channel wall so that the internal volume of the ink channel is changed to eject ink droplets (see JP-A No. 02-51734); a thermal inkjet head, which uses a heat-generating resistor to heat the ink in the ink channel to generate bubbles (see JP-A No. 61-59911); and an electrostatic inkjet head, in which an oscillating plate constituting a wall of an ink channel and an electrode are provided to face each other, electrostatic force generated between the oscillating plate and the electrode deforms the oscillating plate to form that the internal volume of the ink channel is changed to eject ink droplets (see JP-A No. 10-71882).
[00203] The inkjet recording device may additionally contain a dryer configured to dry a recording medium on which an image has been formed.
[00204] The dryer is appropriately selected depending on the intended purpose without any limitation, and examples thereof include an infrared ray dryer, a microwave dryer, a roller heater, a drum heater, and a drum heater. hot air.
[00205] The ink jet recording device may additionally contain a holding device configured to fix a formed image on a recording medium.
[00206] The fixture is suitably selected depending on the intended purpose without any limitation, and examples thereof include a roller heater having a heated mirror surface, and a drum heater having a heated mirror surface.
[00207] It is preferred that a surface of the recording medium on which the image was formed is placed in contact with the mirror surface (smooth surface) of the roller heater or drum heater, and heated to 100°C to 150°C . As a result of this, image brightness can be improved.
[00208] The inkjet ink is preferably housed in a container, such as an ink cartridge.
[00209] The recording medium is appropriately selected depending on the intended purpose without any limitation, and examples thereof include plain paper, glossy paper, special paper, a cloth, a film, an OHP sheet, and a printing sheet commercial. Among these, commercial printing sheet is preferable as it is excellent in gloss, and capable of inhibiting wrinkling and pearling even when an image having a large amount of inkjet ink deposition is formed thereon.
[00210] A commercial printing sheet is a recording medium in which a coating layer is formed on a substrate.
[00211] A transfer amount of pure water from the surface of the commercial printing sheet on which the coating layer is provided is preferably 1 mL/m2 to 35 mL/m2, more preferably 1 mL/m2 to 10 mL/m2, and even more preferably 2 ml/m2 to 10 ml/m2 with the contact time of 100 ms. When the transfer amount is less than 1 mL/m2, beading may occur as an image having a large amount of inkjet ink deposition is formed. When the transfer amount is more than 35 mL/m2, image density may be low as an image having a large amount of inkjet ink deposition is formed.
[00212] A transfer amount of pure water from a surface of the commercial printing sheet on which a coating layer is provided is preferably 3 ml/m2 to 40 ml/m2 with the contact time of 400 ms.
[00213] Note that, the transfer amount of pure water from the surface of the commercial printing sheet on which the coating layer is provided can be measured by means of a D-type K350 series dynamic scanning absorptiometer (manufactured by Kyowa Co. , Ltd.). In addition, the transfer amount of pure water with the contact time of 100 ms can be determined by interpolating the measured values from the transfer amounts of pure water from adjacent contact times.
[00214] Examples of a commercial commercial printing sheet product include: Ricoh Business Cogloss 100 (manufactured by Ricoh Company Limited); OK Top Coat+, OK Kanefuji +, SA Kanefuji + (all manufactured by Oji Paper Co., Ltd.); Super MI Dull, Aurora Coat, Space DX (all manufactured by Nippon Paper Co., Ltd.); Mat, and Mu Coat (all manufactured by Hokuetsu Paper Mills, Ltd.); RAICHOU ART, and RAICHOU SUPER ART (all manufactured by Chuetsu Pulp & Paper Co., Ltd.); Pearl Coat N (manufactured by Mitsubishi Paper Mills, Ltd.).
[00215] Schematic diagrams (explanatory diagrams) illustrating an example of the imaging device according to the present invention are represented in FIGs. 1 and 2.
[00216] The image forming apparatus (may also be referred to as the "ink jet recording device" hereinafter) illustrated in FIG. 1 contains a device body 101, a paper feed tray 102 for feeding paper loaded into the device body 101, a paper disposal tray 103 for stacking the paper loaded into the device body 101 and engraved (formed) with an image , and an ink cartridge loading section 104. On the top face of the ink cartridge loading section 104, a control section 105, such as operating keys and an indicator, is arranged. The ink cartridge loading section 104 is provided with a front cover 115, which can be opened and closed, for removing and loading an ink cartridge 200. In FIG. 1, 111 is a top cover, and 112 is a front face cover. Instead of or in addition to an ink cartridge 200, a cartridge housing an aftertreatment liquid can be mounted to eject the aftertreatment liquid.
[00217] In the device body 101 as illustrated in FIG. 2, a carriage 133 is maintained to slide freely in the main scan direction through a guide rod 131 and a support 132 which are guide members deposited on side plates (not shown). Scanning is performed via a main scan motor (not shown).
[00218] In transport 133, a recording head 134 including four inkjet recording heads which discharge recording ink droplets for the respective colors, yellow (Y), cyan (C), magenta (M), and black (Bk) is charged, so that a plurality of ink discharge openings are arranged in the direction that crosses the main sweep direction, and the ink droplet discharge direction is placed below.
[00219] As the ink jet recording head constituting the recording head 134, an ink jet recording head including a piezoelectric actuator such as a piezoelectric device, a thermal actuator which uses phase shift due to boiling liquid film through the use of an electrochemical conversion device such as a resistive heating element, a memory metal actuator that uses metal phase change due to temperature change, an electrostatic actuator that uses electrostatic energy, or the like as a unit to generate power to discharge recording ink can be used.
[00220] Additionally, the carrier 133 is provided with a subtank 135 for each color to supply ink for each color to the recording head 134. The subtank 135 is supplied and replenished with the recording ink of the present invention from the recording cartridge. ink 200 which is loaded into the ink cartridge loading section 104 through a recording ink supply tube (not shown).
[00221] Meanwhile, as a paper feed unit for feeding paper 142 loaded into a paper loading section (press plate) 141 of the paper feed tray 103, a semi-lunar roller (paper feed roller) is provided 143) which separately feeds the paper 142 piece by piece from the paper loading section 141 and a separation block 144 made of a material having a large coefficient of friction, which faces the paper feed roller 143. This separation block 144 is mounted to press against the side of the paper feed roller 143.
[00222] As a transport part for transporting the paper 142 fed from this paper feed unit below the recording head 134, a transport belt 151 for electrostatically absorbing and transporting the paper 142, a counter roller 152 for transporting the paper 142 fed from the paper feed section through a guide 145 by sandwiching the paper 142 between the counter roll 152 and the conveyor belt 151, a transport guide 153 for changing the direction of the paper 142 fed approximately vertically over the section of paper feed at an angle of about 90°, and let the paper 142 be taken along the conveyor belt 151, and an end pressure roller 155 pressed against the side of the conveyor belt 151 by a pressure member 154 are provided. Additionally, a loading roller 156 which is an electrification measurement for loading a surface of the conveyor belt 151 is provided.
[00223] The conveyor belt 151 is an endless belt. The conveyor belt 151 is stretched between a conveyor roller 157 and a tension roller 158, and can bypass in the conveyor direction of the belt. This conveyor belt 151 has a surface layer formed from a resin material (no resistance control) having a thickness of about 40 µm, eg a tetrafluoroethylene-ethylene (ETFE) copolymer and which serves as an absorbing surface. of paper, and a back layer (medium resistance layer, ground layers) provided with resistance control by carbon, which is the same material as used in the surface layer. A guide member 161 corresponding to a region of printing by the recording head 134 is arranged on the rear side of the conveyor belt 151. As a paper ejecting part for ejecting the paper 142 engraved by the recording head 134, a claw separator 171 for separating the paper 142 from the conveyor belt 151, a paper discharge roller 172, and a paper discharge roller 173 are provided, and the paper eject tray 103 is arranged below the eject roller. of paper 172.
[00224] A two-sided paper feed unit 181 is detachably loaded on the rear face portion of the apparatus body 101. The two-sided paper feed unit 181 collects the returned paper 142 by counter-rotating the belt. conveyor 151, reverses the paper 142, and feeds the paper 142 again between the counter roller 152 and the conveyor belt 151. A manual paper feed section 182 is provided on the top face of the double-sided paper feed unit 181 .
[00225] In this inkjet recording device, paper 142 is fed separately piece by piece from the paper feed section. Then, the paper 142 fed approximately vertically over the paper feed section is guided by the guide 145, and transported by being sandwiched between the transport belt 151 and the counter roller 152. Additionally, one end of the paper 142 is guided by the transport guide. 153, and is pressed onto the conveyor belt 151 by the end pressure roller 155. Then, the transport direction of the paper 142 is changed at an angle of about 90°.
[00226] At this time, the conveyor belt 157 is loaded by the loading roller 156, and therefore, the paper 142 is conveyed in the state where the paper 142 is electrostatically absorbed by the conveyor belt 151. Through the drive of the recording head 134 which corresponds to image signals while moving the transport 133, ink droplets are discharged onto the stationary paper 142 and a line is recorded. After paper 142 is transported in a given quantity, the next line is recorded. When a recording end signal or a signal that a trailing end of the paper 142 reaches the recording region is received, the recording operation is finished, and the paper 142 is discharged to the paper discharge tray 103.
[00227] When a near-end amount of recording ink remains within the subtank 135 is detected, a required amount of the recording ink is replenished from the ink cartridge 200 to the subtank 135.
[00228] In this inkjet recording device, when recording ink in the ink cartridge 200 is used, it is possible to disassemble the ink cartridge housing 200 and replace only the inner ink bag. Additionally, ink cartridge 200 can stably supply recording ink even when ink cartridge 200 is positioned vertically and has a front loading construction. Therefore, even when the installation is done in the state where a space on the top face of the device body 101 is blocked, for example when the device body 101 is housed in a support, or objects are placed on the top face of the device body 101, the ink cartridge 200 is easily replaceable.
[00229] Here, descriptions have been given for the case where a serial inkjet recording device type (transport type) is applied where the transport performs scanning. However, an in-line type inkjet recording device using a similar line head can be used.
[00230] Examples of the present invention will be explained hereinafter, but Examples should not be interpreted as limiting the scope of the present invention. Note that, “part(s)” in the following description denote “part(s) by mass” unless otherwise stated.[Preparation of Self-Dispersing Black Pigment Dispersion Liquid 1]
[00231] By means of Silverson Mixer (from Silverson), 100 g carbon black, Black Pearls (registered trademark) 1000 (manufactured by Cabot Corporation) having BET specific surface area of 343 m2/g, and number of 105 mL/100g DBP absorption, 0.1 mol of the compound represented by the following chemical formula (A), and 1 L of ultra pure ion exchange water were mixed at 6,000 rpm for 30 minutes at room temperature.
Chemical Formula (A)
[00232] When pH of the resultant was greater than 4, 0.1 mol of nitric acid was added. Next, a 20% by mass solution in which 0.1 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise into the resulting mixture for 15 minutes, and the resultant was heated to 60°C with stirring and was allowed to react for 1 hour. After adjusting the pH of the mixture to 10 with an aqueous solution of sodium hydroxide and stirring the resulting mixture for 30 minutes, the mixture was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a Self-Dispersing Black Pigment Dispersion Liquid 1. A Level of Self-Dispersing Black Pigment Surface Treatment 1 was 0.75 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Black Pigment 1 was 120 nm, a sodium ion content of it was 27.868 ppm, and a phosphorus content of it was 2.31% in pasta.
[00233] Note that the volume mean particle diameter (D50) was measured using a Nanotrac UPA-EX150 particle size distribution analyzer (manufactured by Nikkiso Co., Ltd.). In addition, sodium ion was measured by means of an IM-32P ion meter (manufactured by DKK-TOA CORPORATION), and the phosphorus content was measured by elemental analysis.[Preparation of Self-Dispersing Black Pigment Dispersion Solution 2 ]
The ProcessAll 4HV (4 L) mixer (manufactured by Processall Inc.) was loaded with 500 g of carbon black, Black Pearls 880 (manufactured by Cabot Corporation) having the BET specific surface area of 220 m2/g , and the DBP absorption number of 105 mL/100g, 1 L of ultra pure ion exchange water, and 1 mol of the compound represented by the Chemical Formula (A), followed by stirring and heating the mixture to 60°C to mix the mixture at 300 rpm for 10 minutes. Next, a 20% by mass solution in which 1 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise for 15 minutes, followed by heating the mixture to 60°C with stirring to allow this way. the reaction to react for 3 hours. The resulting reaction product was removed while diluting the reaction mixture with 750 mL of ultra pure ion exchange water, followed by subjecting the resultant to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a Self-Dispersing Black Pigment 2 dispersion liquid. A Level of Self-Dispersing Black Pigment Surface Treatment 2 was 0.5 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Black Pigment 2 was 104 nm, a sodium ion content of it was 19.940 ppm, and a phosphorus content of it was 2.20% in pasta.
[00235] [Preparation of Self-Dispersing Black Pigment Dispersion Solution 3]
[00236] The ProcessAll 4HV mixer (4 L) was loaded with 500 g of Black Pearls 880, 1 L of ultra pure ion exchange water, and 0.175 mol of the compound represented by the following chemical formula (B), followed by stirring and then heating the mixture to 60°C to mix the mixture at 300 rpm for 10 minutes. Next, a 20% by mass solution in which 0.175 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise for 15 minutes, followed by heating the mixture to 60°C with stirring to allow this way. the reaction to react for 3 hours.
Chemical Formula (B)
[00237] The resulting reaction product was withdrawn while diluting the reaction mixture with 750 mL of ultra pure ion exchange water, followed by subjecting the resultant to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Next, the resultant was dispersed using ultrasonic waves, and then concentrated to give a solids content of 20% by mass, to thereby obtain a Self-Dispersing Black Pigment dispersion liquid 3. A Level of Self-Dispersing Black Pigment Surface Treatment 3 was 0.35 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Black Pigment 3 was 114 nm, a sodium ion content of it was 12.792 ppm, and a phosphorus content of it was 1.08% in bulk.[Preparation of Self-Dispersing Magenta Pigment Dispersing Solution 1]
[00238] By means of a Silverson Mixer, 100 g of Pigment Red 122 (manufactured by Sun Chemical Corporation), 0.05 mol of the compound represented by the Chemical Formula (B), and 1 L of ultra pure ion exchange water were mixed in 6,000 rpm for 30 minutes at room temperature. Next, a 20% by mass solution in which 0.05 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise into the resulting mixture for 15 minutes, and the resultant was heated to 60°C with stirring and was left to react for 1 hour. After adjusting the pH of the mixture to 10 with an aqueous solution of tetramethyl ammonium hydroxide and stirring the resulting mixture for 30 minutes, the mixture was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a self-dispersing magenta pigment 1 dispersion liquid. was 0.50 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Magenta Pigment 1 was 111 nm, and a phosphorus content thereof was 0.26% by mass.[Preparation of Magenta Pigment Dispersing Solution 1 was Self-dispersing 2]
[00239] By means of Silverson Mixer, 690 g of a surface treated Pigment Red 122 dispersion liquid having a solids content of 14.5% by mass, SMART Magenta 3122BA (manufactured by Sensient Technologies Corporation), 0, 05 mol of the compound represented by the Chemical Formula (B), and 500 mL of ultra pure ion exchange water were mixed at 6,000 rpm for 30 minutes at room temperature. Next, a 20% by mass solution in which 0.05 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise into the resulting mixture for 15 minutes, the resultant was heated to 60°C with stirring and was left to react for 1 hour. After adjusting the pH of the mixture to 10 with an aqueous solution of tetramethyl ammonium hydroxide and stirring the resulting mixture for 30 minutes, the mixture was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a self-dispersing magenta pigment 2 dispersion liquid. was 0.50 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Magenta Pigment 2 was 106 nm, and a phosphorus content thereof was 0.25% by mass.
[00240] [Preparation of Self-Dispersing Cyan Pigment Dispersion Solution 1]
[00241] By means of a Silverson Mixer, 690 g of a 15:4 Pigment Blue dispersion liquid with surface treated having a solids content of 14.5% by mass, SMART Ciano 3154BA (manufactured by Sensient Technologies Corporation), 0.05 mol of the compound represented by the Chemical Formula (A), and 500 mL of ultra pure ion exchange water were mixed at 6,000 rpm for 30 minutes at room temperature. Next, a 20% by mass solution in which 0.05 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise into the resulting mixture for 15 minutes, the resultant was heated to 60°C with stirring and was left to react for 1 hour. After adjusting the pH of the mixture to 10 with an aqueous solution of tetramethyl ammonium hydroxide and stirring the resulting mixture for 30 minutes, the mixture was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a Self-Dispersing Cyan Pigment Dispersion Liquid 1. A Level of Self-Dispersing Cyan Pigment 1 Surface Treatment 1 was 0.50 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Cyan Pigment 1 was 113 nm, and a phosphorus content of it was 0.27% by mass. Self-dispersing 1]
[00242] By means of a Silverson Mixer, 690 g of a surface treated pigment Yellow 74 dispersion liquid having a solids content of 14.5% by mass, SMART Yellow 3074BA (manufactured by Sensient Technologies Corporation), 0, 05 mol of the compound represented by the Chemical Formula (B), and 500 mL of ultra pure ion exchange water were mixed at 6,000 rpm for 30 minutes at room temperature. Next, a 20% by mass solution in which 0.05 mol of sodium nitride was dissolved in ultra pure ion exchange water was added dropwise into the resulting mixture for 15 minutes, the resultant was heated to 60°C with stirring and was left to react for 1 hour. After adjusting the pH of the mixture to 10 with an aqueous solution of tetrabutyl ammonium hydroxide and stirring the resulting mixture for 30 minutes, the mixture was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. Then, the resultant was dispersed using ultrasonic waves, and concentrated to give a solids content of 20% by mass, to thereby obtain a Self-Dispersing Yellow Pigment Dispersion Liquid 1. A Level of Self-Dispersing Yellow Pigment Surface Treatment 1 was 0.50 mmol/g, the volume mean particle diameter (D50) of Self-Dispersing Yellow Pigment 1 was 142 nm, and a phosphorus content of it was 0.26% by mass. Self-dispersing 4]
[00243] In 3 L of a 2.5N sodium sulfate solution, 90 g of carbon black having CTAB specific area of 150 m2/g, and the DBP absorption number of 100 mL/100 g was added, and the resulting mixture was heated to 60°C with stirring at 300 rpm to thereby allow the reaction for 10 hours. The resulting reaction mixture was subjected to filtration, and then the filter cake was neutralized with an aqueous solution of sodium hydroxide. The resultant was subjected to ultrafiltration using ultra pure ion exchange water and a dialysis membrane. After further filtration was carried out, the filter cake was washed with ultra pure ion exchange water and then dried. Next, the dry filter cake was dispersed in ultra pure ion exchange water to give a solids content of 20% by mass, to thereby obtain a dispersion liquid of Self-Dispersing Black Pigment 4. The Self-Dispersing Black Pigment 4 had the volume mean particle diameter (D50) of 103 nm.[Preparation of Dispersion Liquid from Resin Particles Containing Magenta Pigment 1]
[00244] After replacing an internal atmosphere of a 1 L flask, which was equipped with a mechanical stirrer, a thermometer, a nitrogen inlet tube, a condensing tube and a dropping funnel, with nitrogen gas, 11, 2 g of styrene, 2.8 g of acrylic acid, 12.0 g of lauryl methacrylate, 4.0 g of polyethylene glycol methacrylate, 4.0 g of styrene micromer, and 0.4 g of mercaptoethanol, and the mixture was heated to 65°C. Then a mixed solution of 100.8 g of styrene, 25.2 g of acid acryl, 108.0 g of lauryl methacrylate, 36.0 g of polyethylene glycol methacrylate, 60.0 g of hydroxylethyl methacrylate, 36.0 g of styrene macromer, 3.6 g of mercaptoethanol, 2.4 g of azobismethyl valeronitrile, and 18 g of methylethyl ketone were dropped into the flask for 2.5 hours. Additionally, a mixing solution of 0.8 g of azobismethyl valeronitrile and 18 g of methylethyl ketone was dropped into the flask for 0.5 hours. The resulting mixture in the flask was aged at 65°C for 1 hour, and then 0.8 g of azobismethyl valeronitrile was added, followed by aging for a further 1 hour. Next, 364 g of methylethyl ketone was added to the flask, to thereby obtain 800 g of a resin solution having a concentration of 50% by mass.
[00245] After mixing and stirring 28 g of the resin solution, 42 g of RED PIGMENT CI 122, 13.6 g of aqueous potassium hydroxide solution 1 mol/L, 20 g of methyl ethyl ketone, and 13, 6 g of ultra pure ion exchange water, the mixture was kneaded by means of a roller mill to obtain a paste in this way. The slurry obtained was then added to 200 g of ultra pure ion exchange water, and the mixture was stirred, followed by removal of the methylethyl ketone and water by means of an evaporator. The resultant was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average opening diameter of 5.0 µm, to thereby obtain a liquid dispersion of the resin particles containing Magenta 1 Pigment having a content of pigment solid of 15% by mass, and a solids content of 20% by mass. Resin particles containing Pigment Magenta 1 had a volume mean particle diameter (D50) of 127 nm.[Preparation of Liquid Dispersion of Resin Particles containing Pigment Cyan 1]
[00246] A liquid dispersion of the resin Particles containing Pigment Magenta 1 was obtained in the same manner as in the preparation of the liquid dispersion of the resin Particles containing Pigment Magenta 1, provided that PIGMENT RED CI 122 was replaced with PIGMENT BLUE CI 15:3. Resin particles containing Pigment Cyan 1 had a volume mean particle diameter (D50) of 93 nm.[Preparation of Dispersing Liquid of Resin Particles containing Pigment Yellow 1]
[00247] A dispersion liquid of the resin particles containing Pigment Yellow 1 was obtained in the same manner as in the preparation of the dispersion liquid of the resin particles containing Pigment Magenta 1, provided that RED PIGMENT CI 122 was replaced with PIGMENT YELLOW CI 74. Resin particles containing Pigment Yellow 1 had a volume mean particle diameter (D50) of 76 nm.
[00248] A dispersion liquid of Resin Particles containing Pigment Black 1 was obtained in the same manner as in the preparation of the dispersion liquid of Resin Particles containing Pigment Magenta 1, provided that RED PIGMENT CI 122 was replaced with carbon black FW100 (manufactured by EVONIK DEGUSSA JAPAN CO. LTD.). Resin particles containing Pigment Black 1 had a volume mean particle diameter (D50) of 104 nm.[Preparation of Pigment Yellow 1 Dispersed with Dispersing Agent]
[00249] After dissolving 10 parts of a nonionic surfactant, NOIGEN EA-177 (polyoxyethylene styrenephenyl ether) (DAI-ICHI KOGYO SEIYAKU CO., LTD.), having the HLB number of 15.7 in 60 parts of water of Ultra pure ion exchange, 30 parts YELLOW PIGMENT CI 74 (manufactured by Dainichiseika Color & Chemicals Mfg. Co., Ltd.) was added to the mixture. Next, the mixture was dispersed by a wet type disperser, DYNO MILL KDL type A (manufactured by WILLY A. BACHOFEN AG MASCHINENFABRIK) filled with zirconia beads having a diameter of 0.5 mm for 2 hours at 2000 rpm. To this, 4.26 parts of a water-soluble polyurethane resin, TAKELAC W-5661 (manufactured by Mitsui Chemicals, Inc.), having an active ingredient of 35.2% by mass, acid value of 40 mg of KOH µg, and mass average molecular weight of 18,000 was added and stirred, to thereby obtain a dispersing liquid of Pigment Yellow 1 dispersed with a pigment dispersing agent. The volume mean particle diameter (D50) of Pigment Yellow 1 dispersed with the dispersing agent pigment was 62 nm.[Preparation of Magenta 1 Pigment Dispersed with dispersing agent]
[00250] After dissolving 10 parts of a nonionic surfactant, RT-100 (polyoxyethylene-β-naphthyl ether) (manufactured by TAKEMOTO OIL & FAT CO., LTD.), having the HLB number of 18.5 in 60 parts of ultra pure ion exchange water, 30 parts of RED PIGMENT CI 122 (manufactured by Dainichiseika Color & Chemicals Mfg. Co., Ltd.) was added to the mixture. Next, the mixture was dispersed by a wet type disperser, DYNO MILL KDL type A (manufactured by WILLY A. BACHOFEN AG MASCHINENFABRIK) filled with zirconia beads having a diameter of 0.5 mm for 2 hours at 2000 rpm. To this, 7.14 parts of a styrene - water soluble (meth)acrylic acid copolymer, JC-05 (manufactured by SEIKO PMC CORPORATION), having an ingredient of 21% by mass, acid value of 170 mg of KOH µg, and mass average molecular weight of 16,000 was added and stirred, to thereby obtain a dispersing liquid of Pigment Magenta 1 dispersed with a pigment dispersing agent. Magenta 1 pigment dispersed with a pigment dispersing agent had the volume mean particle diameter (D50) of 83 nm.[Preparation of Cyan Pigment 1 Dispersed with Dispersing Agent]
[00251] After dissolving 10 parts of a nonionic surfactant, NOIGEN EA-177 (polyoxyethylene styrenephenyl ether) (DAI-ICHI KOGYO SEIYAKU CO., LTD.), having the HLB number of 15.7 in 60 parts of water of Ultra pure ion exchange, 30 parts of PIGMENT BLUE CI 15:3 (manufactured by Dainichiseika Color & Chemicals Mfg. Co., Ltd.) was added to the mixture. Next, the mixture was dispersed by a wet type disperser, DYNO MILL KDL type A (manufactured by WILLY A. BACHOFEN AG MASCHINENFABRIK) filled with zirconia beads having a diameter of 0.5 mm for 2 hours at 2000 rpm. To this, 5.02 parts of water-soluble polyester, NICHIGO POLYESTER W-0030 (manufactured by Nippon Synthetic Chemical Industry Co., Ltd.), having an active ingredient of 29.9% by mass, acid value of 100 mg of KOH/g, and mass average molecular weight of 7,000 was added and stirred, to thereby obtain a dispersion liquid of Pigment Cyan 1 dispersed with a pigment dispersing agent. Pigment Cyan 1 dispersed with the pigment dispersing agent had a volume mean particle diameter (D50) of 78 nm.[Example 1]
[00252] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a foam regulator pH which was 2-amino-2-ethyl-1,3-propanediol, and 16.94 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a 1.2 μm average aperture diameter to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.6 mPa-s, a pH of 9.7, and a dynamic surface tension of 33.9 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.
[00253] Note that, the inkjet ink viscosity was measured at 25°C by means of a RE-550L viscometer (manufactured by Toki Sangyo Co., Ltd.). In addition, the pH of the inkjet ink was measured at 25°C by means of an HM-30R pH meter (manufactured by DKK-TOA CORPORATION). Additionally, the dynamic surface tension of the inkjet ink with the surface life of 15 ms as measured by the maximum bubble pressure method was measured at 25°C by means of SITA DynoThester (manufactured by SITA Messtechnik GmbH). [Example 2]a. After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 2 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39, 9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-2), 10.00 parts of the compound represented by the Chemical Formula (3-1), 5.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.20 parts of a pH regulator that was i 2-amino-2-ethyl-1,3-propanediol, and 21.94 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a diameter of average aperture of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.5 mPa-s, a pH of 9.6, and a dynamic surface tension of 33.7 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 3]
[00254] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 3 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-3), 10, 00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 5.00 parts of 1.3 -butanediol having an equilibrium moisture content of 35% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2.5 ,8,11-tetramethyldodecane-5,8-diol, 0.20 parts of a pH regulator which was 2-amino-2-ethyl-1,3-propanediol, and 21.94 parts of ultra pure ion exchange water , the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 10.1 mPa-s, a pH of 9.4, and a dynamic surface tension of 34.6 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure. [Example 4]
[00255] After mixing and stirring 17.50 parts of Self-Dispersing Magenta Pigment 1 dispersion liquid, 20.05 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (4-5), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 15.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent that was 2-ethyl-1,3-hexanediol, 2.50 parts of a fluorine-based surfactant, ZONYL FS-300 (polyoxyethyleneperfluoroalkyl ether) (Du Pont Co., Ltd.) having an active ingredient of 40% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of an i foam inhibitor which was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.10 parts of a pH adjuster which was 2-amino-2-ethyl-1,3-propanediol, and 12.40 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 8.3 mPa-s, a pH of 9.4, and a dynamic surface tension of 32.9 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 5]
[00256] After mixing and stirring 37.50 parts of Self-Dispersing Magenta Pigment Dispersion Liquid 2, 30.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a content of solids of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 5.00 parts of the compound represented by the Chemical Formula (1-1), 5.00 parts by mass of the compound represented by Chemical Formula (3-1), 8.00 parts by mass of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% of relative humidity, 2.00 parts by mass of a penetration agent which was 2,2,4-trimethyl-1,3-pentanediol, 0.10 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts by weight of fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.10 parts of a pH regulator that was 2-amino o-2-ethyl-1,3-propanediol, and 1.85 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 15.2 mPa-s, a pH of 9.2, and a dynamic surface tension of 34.8 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 6]
[00257] After mixing and stirring 12.50 parts of Self-Dispersing Cyan Pigment 1 dispersion liquid, 18.80 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2,2,4-trimethyl-1,3-pentanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0. 10 parts of a regulation pH which was 2-amino-2-ethyl-1,3-propanediol, and 15.80 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter. having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 8.1 mPa-s, a pH of 9.5, and a dynamic surface tension of 34.6 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 7]
[00258] After mixing and stirring 12.50 parts of Self-Dispersing Yellow Pigment 1 dispersion liquid, 18.80 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.10 parts of a foam regulator and pH which was 2-amino-2-ethyl-1,3-propanediol, and 15.80 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 μm to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.1 mPa-s, a pH of 9.3, and a dynamic surface tension of 34.7 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 8]
[00259] After mixing and stirring 10.00 parts of Self-Dispersing Cyan Pigment 1 dispersion liquid, 24.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a content of solids of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 1.25 parts of a silicone-based surfactant, a KF-643 polyether-modified silicone compound (manufactured by Shin-Etsu Chemical Co. ., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator that was 2-amino-2-ethyl-1,3-propanediol, and 22.10 parts of ultra ion exchange water pure, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 9.5 mPa-s, a pH of 9.5, and a dynamic surface tension of 32.6 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 9]
[00260] After mixing and stirring 7.50 parts of Self-Dispersing Yellow Pigment 1 dispersion liquid, 30.08 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10, 00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C , 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.10 parts of a powder regulator H which was 2-amino-2-ethyl-1,3-propanediol, and 19.52 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a 1.2 μm average aperture diameter to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.9 mPa-s, a pH of 9.2, and a dynamic surface tension of 31.5 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 10]
[00261] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent that was 2-ethyl-1,3-hexanediol, 2.00 parts of a surfactant, SOFTANOL EP-7025 (polyoxyalkylene alkyl ether) (manufactured by Nippon Shokubai Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator which was 2-amino-2-ethyl-1,3-propanediol, and 15, 29 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink . The inkjet ink had a viscosity of 8.7 mPa-s, a pH of 9.1, and a dynamic surface tension of 38.2 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 11]
[00262] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10, 00 parts of the compound represented by the Chemical Formula (2-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C , 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 3.00 parts of an acetylene alcohol based surfactant, SURFYNOL 104E (manufactured by Nissin Chemical Industry Co ., Ltd.) having an active ingredient of 50% by mass, 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH adjuster which was 2-amino-2-ethyl-1,3-propanediol, and 14.29 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 8.8 mPa-s, a pH of 9.6, and a dynamic surface tension of 33.4 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 12]
[00263] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 20.00 parts of a polyurethane emulsion, HYDRAN APX-101H (manufactured by DIC Corporation) having a solids content of 45 % by mass, average particle diameter of 160 nm, and minimum film forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula (3-1), 5.00 parts of the compound represented by the Chemical Formula (3-3), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having the content equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 1.00 part of a base surfactant of silicone which was a KF-643 polyether modified silicone compound (manufactured by Shin-Etsu Chemical Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide which and was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor which was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.20 parts of a pH regulator which was 2-amino-2-ethyl-1,3-propanediol, and 13.85 parts of ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a diameter opening of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 11.9 mPa-s, a pH of 9.7, and a dynamic surface tension of 34.5 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 13]
[00264] After mixing and stirring 23.33 parts of the resin Particles containing Pigment Magenta 1, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator that was 2-amino-2-ethyl-1,3-propanediol, and 11.11 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a diameter opening of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 15.2 mPa-s, a pH of 9.5, and a dynamic surface tension of 34.6 mN/m with a surface lifetime of 15 ms as measured by the method. of maximum bubble pressure.[Example 14]
[00265] After mixing and stirring 16.67 parts of Resin Particles containing Cyan Pigment 1, 18.80 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39 .9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C , 80% relative humidity, 2.00 parts of a penetration agent which was 2,2,4-trimethyl-1,3-pentanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.10 parts of a regulator of pH which was 2-amino-2-ethyl-1,3-propanediol, and 11.64 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 μm to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 15.2 mPa-s, a pH of 9.3, and a dynamic surface tension of 34.8 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 15]
[00266] After mixing and stirring 16.78 parts of Resin Particles containing Pigment Yellow 1, 18.80 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23° C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.10 parts of a foam regulator pH that was 2-amino-2-ethyl-1,3-propanediol, and 11.53 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a diameter opening of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 4.5 mPa-s, a pH of 9.6, and a dynamic surface tension of 34.4 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 16]
[00267] After mixing and stirring 23.33 parts of Resin Particles containing Pigment Black 1, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator that was i 2-amino-2-ethyl-1,3-propanediol, and 11.11 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a diameter opening of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 15.1 mPa-s, a pH of 9.5, and a dynamic surface tension of 34.2 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure. [Example 17]
[00268] After mixing and stirring 25.00 parts of Self-Dispersing Black Pigment 4 dispersion liquid, 25.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a content of solids of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH adjuster which was 2-amino-2- ethyl-1,3-propanediol, and 7.00 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 13.5 mPa-s, a pH of 9.5, and a dynamic surface tension of 33.6 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 18]
[00269] After mixing and stirring 12.17 parts of the dispersion liquid of Pigment Yellow 1 dispersed with a pigment dispersing agent, 28.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a solids content of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.60 parts of a foam inhibitor that was it was 2,5,8,11 you tramethyldodecane-5,8-diol, 0.10 parts of a pH adjuster that was 2-amino-2-ethyl-1,3-propanediol, and 6.33 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 14.5 mPa-s, a pH of 9.7, and a dynamic surface tension of 33.4 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 19]
[00270] After mixing and stirring 17.86 parts of the pigment dispersion liquid of Pigment Magenta 1 dispersed with a pigment dispersing agent, 20.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a solids content of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C , 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a foam regulator pH which was 2-amino-2-eth il-1,3-propanediol, and 19.14 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 13.8 mPa-s, a pH of 9.7, and a dynamic surface tension of 33.2 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Example 20]
[00271] After mixing and stirring 12.25 parts of Cyan Pigment 1 dispersion liquid dispersed with a pigment dispersing agent, 28.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a solids content of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 20.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C , 80% relative humidity, 2.00 parts of a penetration agent which was 2,2,4-trimethyl-1,3-pentanediol, 0.15 parts of the compound represented by the Chemical Formula (10-17), 0, 05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.60 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.10 parts of a pH regulator that was 2-a mino-2-ethyl-1,3-propanediol, and 6.85 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a medium aperture diameter. of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 14.7 mPa-s, a pH of 9.8, and a dynamic surface tension of 33.2 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 1]
[00272] After mixing and stirring 37.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 9.40 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a siliconized acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10 .00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23 °C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.10 parts of the compound represented by the Chemical Formula (1017), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a foam regulator pH that which was 2-amino-2-ethyl-1,3-propanediol, and 10.35 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a 1.2 μm average aperture diameter to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 9.9 mPa-s, a pH of 9.4, and a dynamic surface tension of 34.5 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 2]
[00273] After mixing and stirring 37.50 parts of the dispersion liquid of Self-Dispersing Black Pigment 1, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula ( 3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2 .00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 0.10 parts of the compound represented by the Chemical Formula (10-17), 0.05 parts of a fungicide which was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator which was 2-amino-2 -ethyl-1,3-propanediol, and 19.75 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1, two µm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 7.2 mPa-s, a pH of 9.4, and a dynamic surface tension of 33.8 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 3]
[00274] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 15, 00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 15.00 parts of 1,3-butanediol having an equilibrium moisture content of 35% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent that was 2-ethyl-1,3-hexanediol, 2.00 parts of a surfactant, SOFTANOL EP-7025 (polyoxyalkylene alkyl ether) (manufactured by Nippon Shokubai Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of an inhibitor of foam which was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH adjuster which was 2-amino-2-ethyl-1,3-propanediol, and 15.29 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 7.6 mPa-s, a pH of 9.0, and a dynamic surface tension of 38.6 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 4]
[00275] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (3-1), 10 .00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 10.00 parts of 1, 3- butanediol having an equilibrium moisture content of 35% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 2.00 parts of a surfactant, SOFTANOL EP-7025 (polyoxyalkylene alkyl ether) (manufactured by Nippon Shokubai Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator that was 2- amino-2-ethyl-1,3-propanediol, and 15.29 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having a medium aperture diameter. of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.4 mPa-s, a pH of 9.1, and a dynamic surface tension of 38.4 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 5]
[00276] After mixing and stirring 17.50 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 22.56 parts of POLYZOL ROY6312 (manufactured by SHOWA DENKO KK) which was a silicone acrylic resin emulsion having a solids content of 39.9% by mass, the average particle diameter of 171 nm, and the minimum film-forming temperature (MFT) of 20°C, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10, 00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 10.00 parts of 1.3 -butanediol having an equilibrium moisture content of 35% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 2.00 parts of a surfactant, SOFTANOL EP-7025 (polyoxyalkylene alkyl ether) (manufactured by Nippon Shokubai Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (f abridled by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator that was 2-amino -2-ethyl-1,3-propanediol, and 15.29 parts of very ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 μm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 8.9 mPa-s, a pH of 9.2, and a dynamic surface tension of 38.3 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 6]
[00277] After mixing and stirring 10.00 parts of Self-Dispersing Cyan Pigment 1 dispersion liquid, 36.00 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a content of solids of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 10.00 parts of the compound represented by the Chemical Formula (1-1), 10.00 parts of the compound represented by the Chemical Formula (3-1), 10.00 parts of 3-methoxy-N,N-dimethylpropionamide, 10.00 parts of glycerin having an equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 2.00 parts of a penetration agent which was 2-ethyl-1,3-hexanediol, 1.25 parts of a silicone-based surfactant, a KF-643 polyether-modified silicone compound (manufactured by Shin-Etsu Chemical Co. ., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor that was 2,4,7,9-tetramethyldecane-4,7-diol, 0.20 parts of a pH regulator which was 2-amino-2-ethyl-1,3-propanediol, and 10.10 parts of exchange water ultra pure ionic, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1.2 µm, to thereby obtain an inkjet ink. The inkjet ink had a viscosity of 18.4 mPa-s, a pH of 9.6, and a dynamic surface tension of 34.8 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.[Comparative Example 7]a. After mixing and stirring 35.00 parts of Self-Dispersing Black Pigment 1 dispersion liquid, 57.40 parts of a fluororesin emulsion, LUMIFLON FE4300 (manufactured by ASAHI GLASS CO., LTD.) having a solids content of 45 % by mass and average particle diameter of 160 nm, and having a solids content of 50% by mass, average particle diameter of 150 nm, and MFT of 30°C or less, 1.00 part of the compound represented by the Formula Chemistry (1-1), 1.00 part of the compound represented by the Chemical Formula (3-1), 1.00 part of 3-methoxy-N,N-dimethylpropionamide, 1.00 part of glycerin having equilibrium moisture content of 49% by mass at 23°C, 80% relative humidity, 1.00 part of a penetration agent which was 2-ethyl-1,3-hexanediol, 1.25 parts of a silicone-based surfactant which was a KF-643 polyether modified silicone compound (manufactured by Shin-Etsu Chemical Co., Ltd.) having an active ingredient of 100% by mass, 0.05 parts of a fungicide that was Proxel GXL (manufactured by Arch Chemicals, Inc.), 0.40 parts of a foam inhibitor that was 2,5,8,11-tetramethyldodecane-5,8-diol, 0.20 parts of a pH regulator that was 2-amino- 2-ethyl-1,3-propanediol, and 0.70 part ultra pure ion exchange water, the resulting mixture was subjected to pressure filtration using a polyvinylidene fluoride membrane filter having an average aperture diameter of 1, 2 µm, to obtain an inkjet ink in this way. The inkjet ink had a viscosity of 14.3 mPa-s, a pH of 9.4, and a dynamic surface tension of 34.1 mN/m with a surface life of 15 ms as measured by the method. of maximum bubble pressure.
[00278] Physical properties of the above inkjet inks are shown in Table 1.
[00279] Table 1

[00280] In an adjusted environment where the temperature was 23°C ± 0.5°C and the relative humidity was 50% ± 5%, the drive voltage of a piezoelectric element was changed such that the amount of jet ink ink deposited on a recording medium becomes uniform using an inkjet printer (IPSIO GXe-5500, produced by Ricoh Company, Ltd.), and then the print mode is set to “high quality printing” mode of gloss paper”.
[00281] As for the recording medium, used was POD Gloss Coat (manufactured by Oji Paper Co., Ltd.) having a basis weight of 100 g/m2, pure water transfer amount of 3.1 mL/m2 with 100 ms contact time, and 3.5 mL/m2 pure water transfer amount with 400 ms contact time.
[00282] Image Density, Beading, Impulse Blot, Wrinkle, Gloss, and Blot Fixing Ability were evaluated in the following methods.[Image density]
[00283] A graphic including a solid image of a 64-dot “■” color, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), was printed on a recording medium, and the image density of the solid image area of one color was measured using the X-Rite 938 hydrometer (manufactured by X-Rite Co.). For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that, the image density of the image was judged as “A,” when the image density of black was 2.0 or more, the image density of yellow was 1.25 or more, and the image density of magenta was 2.0 or more, and the cyan image density was 2.0 or more; judged as “B,” when the image density of black was 1.7 or more but less than 2.0, the image density of yellow was 1.1 or more but less than 1.25, the density of magenta image was 1.7 or more but less than 2.0, and cyan image density was 1.7 or more but less than 2.0; judged as “C,” when the image density of black was 1.5 or more but less than 1.7, the image density of yellow was 0.95 or more but less than 1.1, the density of yellow magenta image was 1.5 or more but less than 1.7, and cyan image density was 1.5 or more but less than 1.7; and judged as “D,” when the image density of black was less than 1.5, the image density of yellow was less than 0.95, the image density of magenta was less than 1.5, and the cyan image density was less than 1.5.[Beading]
[00284] A graphic including a solid image of a 64-dot “■” color, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), was printed on a recording medium, and density inequality in the solid image area of a color was observed visually for evaluation. For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that, the state where there was no density inequality was judged as “A,” the state where there was a slight inequality in density was judged as “B,” the state where there was density inequality was judged as “C,” and the state where there was a significant degree of density inequality was judged as “D.”[Impulse Spots]
[00285] A graphic including a solid image of a 64-dot color “■”, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), was printed on a recording medium, spots shifted from the solid image area to the background area caused by the impulse were visually observed. For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that, the case where the displaced spots were clearly observed was judged as “III,” the case where the displaced spots were slightly observed was judged as “II,” and the case where the displaced spots were not observed per se was judged as “I.”[Wrinkle]
[00286] Right after printing a graphic including a solid image of one color “■■■” having a size of 3 cm x 15 cm, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), on a recording medium, occurrence of wrinkling in the solid image area of a color was visually observed. For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that, the case where wrinkling did not occur was judged as A,” the case where the wrinkling occurred slightly was judged as “B,” the case where the wrinkling occurred was judged as “C,” and the case where the wrinkling occurred from significantly was judged as “D.”[Brightness]
[00287] After printing a graphic including a solid image of one color “■■■” having a size of 3 cm x 15 cm, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), on a recording medium, 60 The specular brightness of the solid image area of one color and that of the unetched area were measured by means of a 4501 brightness meter (manufactured by BYK Gardner) to assess brightness in this way. For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that, the case where the absolute value of the difference between the 60° specular brightness of the solid image area of a color and that of the unetched area was less than 5 was judged as “A,” the case where the absolute value of the same was 5 or more but less than 10 was judged as “B,” and the case where the absolute value of it was 10 or more but less than 15 was judged as “C,” and the case where the absolute value of it was of the same was 15 or more was judged as “D.”[Spot fixation capacity]
[00288] After printing a graphic including a solid image of one color “■■■” having a size of 3 cm x 15 cm, produced using MICROSOFT WORD 2000 (manufactured by Microsoft Corporation), onto a recording medium, the Printed recording medium was dried for 24 hours in the adjusted environment of 23°C ± 2°C, 50% RH ± 15% RH. Next, JIS L0803 Cotton No. 3 attached to the CM-1 Clock Meter with a double-sided tape was moved against the solid image area of one color in 10 returns, followed by measuring the density of the spots deposited on the cotton cloth. and that the bottom of the cotton cloth by means of X-Rite939 (manufactured by X-Rite Co.), to thereby assess the stain-fixing ability. For printing, the print mode has been changed from "high quality gloss paper print" to "no color correction." Note that the case where the difference between the density of the stains deposited on the cotton cloth and the density of the bottom of the cotton cloth was less than 0.05 was evaluated as “A,” the case where the difference was 0.05 or more but less than 0.1 was evaluated as "B," and the case where the difference was 0.1 or more but less than 0.15 was evaluated as "C," and the case where the difference was 0 .15 or more was rated as "D."
[00289] The results of evaluating image density, pearling, impulse smears, wrinkle, gloss, and smear-fixing ability are shown in Table 2.

[00290] It was found from the results presented in Table 2 that the inkjet inks of Examples 1 to 20 had excellent image density, gloss, and smear holding ability and could avoid occurrences of beading, pulse smearing, and wrinkling .
[00291] On the other hand, the inkjet ink of Comparative Example 1 had low gloss in the solid image area of a color, as the mass ratio of the water-dispersible resin to the pigment was 0.5.
[00292] The inkjet ink of Comparative Example 2 had low gloss in the solid image area of one color, as the amount of pigment contained was 7.5% by mass, and a water-dispersible resin was not contained.
[00293] The inkjet inks of Comparative Example 3 to 5 gave low image density and caused beading, impulse smearing, and wrinkling, as these inkjet inks do not contain the compound represented by General Formula (1) and /or the compounds represented by General Formulas (2) to (4).
[00294] The inkjet ink of Comparative Example 6 had low jet stability as the mass ratio of the water-dispersible resin to the pigment was 9.0, and therefore ratings of image density, beading, impulse spotting, wrinkle, shine, and stain-fixing ability cannot be realized.
[00295] The inkjet ink of Comparative Example 7 had low jet stability as a total amount of pigment and a water-dispersible resin was 35.7% by mass, and therefore ratings of image density, beading, speckle per thrust, wrinkle, shine, and spot-holding ability cannot be realized. Modalities of the present invention are as follows:<1>An inkjet ink containing: a water-dispersible colorant; a surfactant; a penetration agent; a water-dispersible resin; a wetting agent containing at least polyhydric alcohol having an equilibrium moisture content of 30% by mass or greater at 23°C, 80% relative humidity; a compound represented by the following general formula (1); water; and at least one selected from the group consisting of a compound represented by the following general formula (2), a compound represented by the following general formula (3), and a compound represented by the following general formula (4), wherein the colorant is dispersible in water is at least one selected from the group consisting of a self-dispersing pigment, a pigment dispersed by a pigment dispersing agent, and resin particles each containing a pigment, wherein a total amount of the water-dispersible colorant and the water-dispersible resin is 8% by mass to 35% by mass, and wherein a mass ratio of the water-dispersible resin to the water-dispersible colorant is 2 to 8:
General Formula (1)where R1 is an alkyl group from C4 to C6,
General Formula (2)
[00296] where R2 is a hydrogen atom, a methyl group, or an ethyl group, and R3 is an alkyl group from C1 to C4,
General Formula (3)
[00297] where R4 is either a methyl group or an ethyl group, and R5 is a hydroxyl group, a C1 to C8 alkyl group, a cycloalkyl group, or an aryl group,
General Formula (4)
[00298] where R6 and R7 are each independently a C1 to C8 alkyl group.< 2>The inkjet ink according to <1>, additionally containing a compound represented by the following chemical formula:CH3OCH2CH2CON(CH3)2< 3>The inkjet ink according to any one of <1> or <2>, wherein a water-dispersible resin is a siliconed acrylic resin, a fluororesin, or a combination of the siliconed acrylic resin and the fluororesin.< 4>The inkjet ink according to any one of <1> to <3>, in which the self-dispersing pigment is anionic.< 5>The inkjet ink according to any one of <1> to <4>, wherein the surfactant is a silicone based surfactant, a fluorine based surfactant, an acetylene alcohol based surfactant, or any combination thereof. < 6>The inkjet ink according to any one of <1> to <5>, wherein the ink has a dynamic surface tension of 35 mN/m or less at 25°C, with a lifetime of 15 ms surface as measured by the maximum bubble pressure method.< 7>An inkjet recording device, containing:
[00299] an ejection unit configured to eject an inkjet ink,
[00300] where the inkjet ink is the inkjet ink according to any one of <1> to <6>.

权利要求:
Claims (7)
[0001]
1. Ink jet ink characterized by the fact that it comprises: a water-dispersible colorant; a surfactant; a penetration agent; a water-dispersible resin; a wetting agent containing at least polyhydric alcohol having a moisture content of balance of 30% by mass or greater, in which the equilibrium moisture content is determined by storing a petri dish, in which 1g of the polyhydric alcohol is weighed and placed in a desiccator where the internal temperature and humidity are kept at 23° C ± 1 °C, and 80% relative humidity ± 3% relative humidity, respectively, using a saturated aqueous solution of potassium chloride/sodium chloride and is calculated by the following formula: (Mass of moisture absorbed by polyhydric alcohol) / (Mass of polyhydric alcohol + Mass of moisture absorbed by polyhydric alcohol) x 100a compound represented by the following general formula (1); water; and at least one selected from the group consisting of a compound represented by the following general formula (2), a compound represented by the following general formula (3), and a compound represented by the following general formula (4), wherein the colorant Water-dispersible is at least one selected from the group consisting of a self-dispersing pigment, a pigment dispersed by a pigment dispersing agent, and resin particles each containing a pigment, wherein a total amount of the colorant dispersible in water and water dispersible resin is 8% by mass to 35% by mass, where a mass ratio of water dispersible resin to water dispersible colorant is 2 to 8:
[0002]
2. Inkjet ink according to claim 1, characterized in that it additionally comprises a compound represented by the following chemical formula: CH3OCH2CH2CON(CH3)2.
[0003]
3. Inkjet ink according to any one of claims 1 or 2, characterized in that the water-dispersible resin is a silicone acrylic resin, a fluororesin, or a combination of silicone acrylic resin and fluororesin.
[0004]
4. Inkjet ink according to any one of claims 1 to 3, characterized by the fact that the self-dispersing pigment is anionic.
[0005]
5. Inkjet ink according to any one of claims 1 to 4, characterized in that the surfactant is a silicone-based surfactant, a fluorine-based surfactant, an acetylene alcohol-based surfactant, or any combination of them.
[0006]
6. Inkjet ink according to any one of claims 1 to 5, characterized in that the ink has a dynamic surface tension of 35 mN/m or less at 25°C, with a surface lifetime 15 ms as measured by the maximum bubble pressure method.
[0007]
7. Inkjet recording device characterized in that it comprises: an ejection unit configured to eject an inkjet ink, wherein the inkjet ink is inkjet ink as defined in claims 1 to 6.

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同族专利:

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公开号 | 公开日

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WO2013115344A1|2013-08-08|

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JP2013177559A|2013-09-09|

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CN104080864A|2014-10-01|

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US9528017B2|2016-12-27|

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BR112014018176A2|2017-06-20|

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EP2809734A1|2014-12-10|

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RU2014135768A|2016-04-10|

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EP2809734B1|2017-10-18|

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US20140368572A1|2014-12-18|

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EP2809734A4|2015-03-11|

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JP6065607B2|2017-01-25|

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CN104080864B|2016-03-02|

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法律状态:
2018-03-27| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2019-08-20| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2021-06-08| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-08-10| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 25/01/2013, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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JP2012022348|2012-02-03|

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JP2012-022348|2012-02-03|

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PCT/JP2013/052293|WO2013115344A1|2012-02-03|2013-01-25|Inkjet ink and inkjet recording device|

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