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    • 专利摘要:
    pretreatment composition and method for printing durable images on a recording medium, a pretreatment composition and a printing method using said pretreatment composition are described. an example described of the pretreatment composition includes a liquid carrier, a polyvalent metal salt as a fixing agent, and a latex resin having an acid number less than 20.
    公开号:BR112012028734B1
    申请号:R112012028734-6
    申请日:2010-06-14
    公开日:2020-01-07
    发明作者:George Sarkisian；Elizabeth Ann Visnyak；Ali Emamjomeh
    申请人:Hewlett-Packard Development Company L.P.；
    IPC主号:
    专利说明:

    PRE-TREATMENT COMPOSITION AND METHOD FOR PRINTING DURABLE IMAGES ON A RECORDING MEDIA
    Background to the invention r The inkjet printer technology has expanded its application to high-speed, commercial and industrial printing, in addition to home and office use.
    This technology is a non-impact printing method in which an electronic signal controls and directs the drops of or a stream of ink that can be deposited on a wide variety of substrates. Current inkjet printing technology involves the force of ink droplets through small nozzles by thermal ejection, piezoelectric pressure or oscillation, on the surface of a medium.
    In addition to the ink composition, a pretreatment composition can be applied before an ink composition is established on the print registration medium in order to improve the printing characteristics and attributes of the image. Said pretreatment composition 20 is often a substantially colored liquid that interacts with the dye and / or the polymeric components of the ink composition to thereby precipitate or otherwise fix the ink composition to the surface. of the media.
    Within the use of the aforementioned pre-treatment composition, the precipitated dye tends to deposit on the surface of the recording medium, which thus results in the improvement of the image quality attributes, such *
    as, for example, good optical density and also t 30 allows printing at high speed. Pre-treatment formulations are therefore desirable because they are more stable and reliable pre-treatment compositions that will produce printed images with higher quality on the surface of the media.
    Brief description of the drawings
    To better understand the present description, some embodiments will be described below through non-limiting examples only, with reference to the figures, in which:
    Figure 1 illustrates a graph depicting the change in black optical density of the 5 inkjet printing medium printed with different pretreatment compositions according to the embodiments of the present invention; and
    Figure 2 illustrates a graph depicting the changes in brightness of the printed inkjet media 10 with different pretreatment compositions according to the embodiment of the present invention.
    Detailed description of the invention
    Before the particular embodiments of the present invention are described and detailed, it is to be understood that the present invention is not limited to the particular process and materials described herein. It should also be understood that the terminology used here is used to describe particular embodiments only and is not intended to be limiting with respect to the scope of protection of the present invention which will be defined only through the claims and equivalents thereof. In describing and claiming the present exemplary composition and method, the following terminology will be used: the singular forms one, one, 25 and the include references to the plural unless the context defines otherwise. Thus, for example, reference to a pigment includes reference to one or more of said materials. Concentrations, quantities, and other numerical data can be present here in a range format. It should be understood that said range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly cited as the range limits, but also to include all individual numeric values or sub-ranges covered within those ranges as if each numerical value and sub-ranges were explicitly cited. For example, a weight range of approximately 1% by weight to about 20% by weight should be interpreted to include not only the explicitly quoted concentration of 1% by weight to about 20% by weight, but also to include 5 individual concentrations such as 2% by weight, 3% by weight, 4% by weight, and sub-bands such as 5% by weight to 15% by weight, 10% by weight to 20% by weight, etc. The weight percentage here means the weight percentages. All percentages are in weights unless otherwise indicated.
    As used here, image refers to the marks, signs, symbols, figures, indications and / or appearance deposited on a material or substrate with both a visible and invisible ink composition.
    Examples of an image can include characters, words, numbers, alphanumeric symbols, punctuation, text, lines, underlines, highlights, and the like.
    In some embodiments, the present invention relates to a pre-treatment composition that includes a liquid vehicle, a polyvalent metal salt as a fixing agent and a latex resin having an acid number less than 20.
    In addition, the present invention relates to a method for printing durable images on a recording medium.
    In some embodiments, said methods include applying a pre-treatment composition to a recording medium, said pre-treatment composition including a liquid carrier, a polyvalent metal salt as a fixing agent, and a latex resin having an acid number less than 20.
    An ink composition, containing an aqueous liquid carrier and a dye, is then applied to a recording medium. In some examples, the overprint ink composition is referred to as the pre-treatment composition.
    In some embodiments, the pre-treatment composition is applied to said recording medium using t
    coating devices and said ink composition are blasted onto said recording medium via ink jet nozzles.
    »Without being bound by any theory, it is believed that after the pre-treatment composition is overprinted with the» ink composition on the substrate or, in other words, when the pre-treatment ink and composition are on the medium surface, an effective immobilization of the ink dye is carried out and almost all 10 dyes are deposited on the surface of the medium instead of penetrating the medium and depositing below the surface. Concomitantly, the vehicle of the pretreatment composition, during mixing with the paint vehicle, becomes highly moist and the mixed vehicle penetrates rapidly through the medium, leaving the dye behind. Thus, in some embodiments, the pretreatment composition, during contact with the ink, induces the dye present in the ink formulation to precipitate and result in the improvement of image quality attributes, such as, for example, optical density, saturation, and durability . Within the said printing method, the combination of pre-treatment composition and ink composition results in the method that provides high quality and durable image prints. The use of the pre-treatment composition as described here results in the improvement of image quality attributes while enabling high-speed printing. In addition, the pre-treatment composition provides good image quality such as *
    permanence and smudge resistance, and does not affect or w 30 controls light stability.
    In addition, the pre-treatment composition is a stable composition, thus meaning that the pre-treatment composition does not present stability problems. In some embodiments, the use of the pre-treatment composition results in printed images having, at the same time, good image quality (such as improved brightness and KOD) and durability. In some other embodiments, the use of the pre-treatment composition is particularly effective on the low absorption medium, such as coated compensation medium.
    v As used here, the pre-treatment composition is used as a fixation fluid composition in a »printing method. The pretreatment composition or fluid fixation composition contains an aqueous vehicle and an effective amount of one or more fixing agents. A fixing agent is an ingredient that initiates a change in the solubility or stability of the dye and fixes the dye in place on the printed image. An effective amount of the fixing agent is an amount that is effective in achieving improved print quality, for example, decreased strikethrough and leakage, increased optical density (OD), saturation, margin sharpness, and improved condensation and stability turbidity when compared to an impression that has not been fixed. The pretreatment composition can be formulated for high spray penetration and rapid penetration, and drying. The surface tension can be less than about 45 mN / m.
    In some examples, the pretreatment composition has a viscosity within the range of about 1.0 to about 2000 cps, and in other examples, about 10 to about 1000 cps. In still other examples, the pretreatment composition has a viscosity within the range of about 40 to about 100, when measured at 25 ° C, in order to achieve the desired rheological characteristics. As indicated above, the viscosity of the composition is suitably regulated, for example, through appropriate choices of the amount and molecular weight of the binder resin, the organic solvent, and other agents.
    In some examples, the pretreatment composition of the present description improves the print quality (such as saturation and flow) and durability of the ink printed on a medium, that is, increased water stability, smudge resistance, and stability of light of the inks.
    Exemplary embodiments of the pretreatment composition include, as a fixing agent, a polyvalent metal salt. The 'polyvalent metal salt component may be a divalent or higher polyvalent metal ion and an anion. In some embodiments, the polyvalent metal salt component is soluble in water. Examples of polyvalent metal ions include divalent metal ions, such as Ca 2+ , Cu 2+ , Ni 2- , Mg 2 ', ZN 2+ and Ba 2+ , trivalent metal ions, such as Al 3+ , Fe 3+ and Cr 3+ . In some examples, the polyvalent metal ion is selected from the group consisting of Ca 2+ , MG 2+ or Zn 2+ . In some other examples, the polyvalent metal ions are Ca2 +. Examples of anions include CI, I, Br, NO 3 or 15 RCOO- (where R is H or any hydrocarbon chain).
    In some embodiments, the polyvalent metal anion is a chloride (Cl) or acetate (CH 3 COO). In some embodiments, the polyvalent metal salt is composed of divalent or polyvalent metal ions and nitrate or 20 carboxylate ions. Carboxylate ions are derived from a saturated aliphatic monocarboxylic acid having 1 to 6 carbon atoms or a carbocyclic monocarboxylic acid having 7 to 11 carbon atoms. Examples of saturated aliphatic monocarboxylic acid having 1 to 6 carbon atoms include formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, isovaleric acid, pivalic acid and hexanoic acid.
    In some embodiments, the fixing agent is a polyvalent metal salt selected from the group consisting of calcium chloride, calcium nitrate, magnesium nitrate, magnesium acetate or zinc acetate. In some other embodiments, the polyvalent metal salt is calcium chloride or calcium nitrate (CaCl 2 or
    Ca (NO3) 2 ) · In yet another embodiment, the polyvalent metal salt is calcium chloride (CaCl 2 ).
    In some examples, the fixing agent is present in the pre-treatment composition in an amount representing from 1 to about 20% by weight of the total weight of the pre-treatment composition. In some other examples, the fixing agent is present in an amount representing from about 3 to about 15% by weight of the total weight of the pretreatment composition. In still other examples, the fixing agent is present in an amount representing from about 5 to about 13% by weight of the total weight of the pretreatment composition. In some other examples, the fixing agent is present in an amount representing from about 7 to about 9% by weight based on the total weight of the pretreatment composition.
    Exemplary embodiments of the pre-treatment composition include latex resin components. In some embodiments, the polymeric latex is a cationic, an anionic or an amphoteric polymeric latex.
    In some other examples, the pretreatment composition contains an anionic latex resin component having a low acid number. In some examples, the term latex refers here to a group of preparations consisting of stable dispersions of polymeric micro-particles dispersed in an aqueous matrix. In some other examples, the latex resin components are present, in the composition, in the form of dispersed latex resin particles.
    According to an exemplary embodiment, the latex resin has an acid number less than 18. As used here, the acid number (NA) refers to the acid number that was measured through the conductivity titration of the latent acid functions of the latex resin with nitric acid. As an example, the sample is made of a strong base with KOH then it is titrated with 1% HNO 3 . The pH and the curves are measured simultaneously.
    In some instances, latex resin is a resin made of polymer and copolymer selected from the group consisting of acrylic polymers and copolymers, vinyl acetate polymers or copolymers, polyester polymers or copolymers, vinylidene chloride polymers or copolymers, butadiene polymers or copolymers , styrene-butadiene polymers or copolymers, polymers or »acrylonitrile-butadiene copolymers. In some other examples, the latex resin component is a latex • containing particles of a vinyl acetate-based polymer, an acrylic polymer, a styrene polymer, an SBR-based polymer, a polyester-based polymer, a polymer based on vinyl chloride, or the like. In some other examples, the latex resin is a polymer or copolymer selected from the group consisting of acrylic polymers, vinylacrylic copolymers and acrylic polyurethane copolymers.
    In some examples, the latex resin particles can have an average molecular weight (Mw) of 5,000 to 500,000. In some other examples, latex resins have an average molecular weight (Mw) ranging from 50,000 to 300,000. In some other embodiments, latex resins have an average molecular weight of about 250,000.
    In some examples, the average particle diameter of the latex resin particles is 10 nm to 1 μπι and, as other examples, 10 to 500 nm, and in yet other examples, from 50 nm to 250 nm. The particle size distribution of the latex is not particularly limited, and either latex having a wide particle size distribution or latex having a monodisperse particle size distribution can be used. It is also possible to use two or more types of fine polymeric particles, each having a monodisperse particle size distribution in combination.
    In some examples, the glass transition temperature (Tg) of the latex resin ranges from -30 ° C to 70 ° C, and in some other examples, it ranges from 0 ° C to 50 ° C. In still other examples, the glass transition temperature of the latex resin is below 40 ° C. In some instances, the glass transition temperature of the latex resin is below 30 ° C. The route parameter to measure the glass transition temperature (Tg) is described in, for example, Polymer Handbook, 3rd edition, written by J. Brandrup, EH Immergut published by Wiley-Interscience, 1989.
    In some embodiments, the latex resin of the present invention has an acid number less than 20 and has a glass transition temperature that is below 40 ° C. In some other embodiments, the pretreatment composition includes an anionic latex resin with an acid number below 20, with a glass transition temperature that is below 40 ° C and a molecular weight of approximately 250,000.
    In some examples, the latex resin is present in the pre-treatment composition in an amount representing from about 1 to about 70% by weight of the total weight of the pre-treatment composition. In some other embodiments, the latex resin is present in an amount representing from about 10 to about 60% by weight of the total weight of the pre-treatment composition. In still other examples, the latex resin is present in an amount representing from about 20 to about 50% by weight of the total weight of the pre-treatment composition.
    According to the exemplary embodiments, the latex resin may include, but is not limited to, the latex resin sold under the trade name Hycar® or Vycar® (at Lubrizol Advanced Materials Inc.); Rhoplex® (from Rohm & Hass Company); Neocar® (from Dow Chemical Company); Aquacer® (from BYC Inc.) or Lucidene® (from Rohm & 30 Haas Company).
    In some examples, the pre-treatment composition contains surfactants. Non-limiting examples of the appropriate surfactants include non-anionic surfactants, cationic surfactants and combinations thereof. In some 35 examples, surfactants are non-anionic surfactants.
    In some other examples, surfactants are non-anionic surfactants selected from the group ►
    consisting of non-ionic fluoro-surfactant, non-ionic acetylenic diol surfactant, non-ionic ethoxylated alcohol surfactant and combinations thereof. In one example, no. limitative, the pretreatment composition contains nonionic ethoxylated alcohol surfactant.
    «The various commercially available nonionic surfactants can be used in the formulation of the pretreatment composition, examples of which include ethoxylated alcohols such as those in the Tergitol® 10 series (eg, Tergitol® 15830, Tergitol® 1589), manufactured by Dow Chemical; Surfynol® series surfactants (eg Surfynol® 440 and Surfynol® 465), manufactured by Air Products and Chemicals, Inc .;
    fluorinated surfactants, such as those in the family
    Zonyl® (for example, Zonyl® FSO and Zonyl® FSN surfactants), manufactured by E.I. DuPont de Nemours and Company; fluorinated Polyfox® nonionic surfactants (for example, PF159 nonionic surfactants), manufactured by Omnova; or combinations thereof. Suitable cationic surfactants that can be used in the pretreatment composition include long chain amines and / or their salts, acrylated diamines, polyamines and / or their salts, quaternary ammonium salts, polyoxyethylene long chain amines, long chain amines quaternary polyoxyethylene, and / or combinations thereof.
    In some examples, the surfactant is present in the pre-treatment composition in an amount of up to about 1.5 weight percent (weight percent). As a non-limitative example, the surfactant is present in an amount ranging from about 0.1% by weight to about 1% by weight. In yet another non-limiting example, the surfactant is present in an amount ranging from about 0.2% by weight to about 0.6% by weight.
    In some embodiments, the pre-treatment composition includes an aqueous vehicle. The term aqueous vehicle as defined herein refers to an aqueous mixture in which the fixing agent is placed to form the pretreatment compositions. Examples of suitable aqueous vehicle components include, but are not limited to, water, co-solvents, surfactants, additives (corrosion inhibitors, salts, etc.), and / or combinations thereof. In some examples, the aqueous vehicle includes a water-soluble organic co-solvent, a surfactant, and water. Non-limiting examples of water-soluble organic co-solvent include 2-ethyl-2-hydroxyethyl-1,3-propanediol, glycerol propylate, tripolyethylene glycol, 1— (2 - hydroxyethyl) 2-pyrrolidinone, 1- (2-hydroxyethyl ) -2imidazolidinone, and / or combinations thereof. The solvents listed previously are suitable for any embodiment of the pretreatment composition described herein, particularly when using embodiments of the pretreatment composition, including amine-N-oxide and cationic polyelectrolytes. Other solvents suitable for embodiments of the pretreatment composition include at least amine-N-oxide and the acid includes ethylene glycol, diethylene glycol, triethylene glycol, l-propoxy-2-propanol (commercially available as Dowanol® PNP, from Down Chemical Co. , Midland, MI), and combinations thereof. In some examples, the organic co-solvent is present in the pretreatment compositions in an amount of up to 25% by weight. In a non-limiting example, the organic co-solvent ranges from about 0% by weight to about 20% by weight.
    One or more additives can also be incorporated into any of the embodiments of the pretreatment composition. As used herein, the term additive refers to a constituent of the fluid that operates to improve performance, effects on the environment, aesthetic effects, or other similar properties of the composition. Examples of suitable additives include biocides, sequestering agents, chelating agents, viscosity modifiers, anti-corrosion agents, marker dyes (e.g., visible, ultraviolet, infrared, fluorescent, etc.), dyes, optical brighteners, luminance agents, and / or gender, and / or combinations thereof. The pretreatment composition can also include a marker dye such as, for example, Basic 16 violet (BV 16). In other examples, the additives are present in the pretreatment composition in an amount ranging from about 0.01% by weight to about 1% by weight. In one example, about 0.05% by weight of the additive is present.
    Examples of methods for printing durable images on a recording medium include: applying the pre-treatment composition, as defined above, on a recording medium and applying an aqueous ink composition on said recording medium, said composition ink including an aqueous liquid carrier and a dye. In some examples, the ink is overprinted in the pre-treatment composition. Said printing method results in a printed medium that has an improved durability, as well as, issues of reduced flow and consequent coalescence. Improved durability means the use of the pretreatment composition that provides strength for the final drying, as well as durability to moisture. In addition, the imaging method described here produces high quality printed images and enables high-speed printing.
    In some embodiments, the printing method provides the printed image while having good image quality (such as improved brightness and KOD) and durability. In some other examples, the printing method is particularly effective on the low absorption recording medium, such as coated compensation medium.
    In some examples, the image-forming method includes depositing a pre-treatment composition onto a recording medium, then blasting an aqueous ink composition that will react with a liquid from the pre-treatment composition.
    In some examples, the method for printing durable images is an inkjet printing method. By means of the inkjet printing method, here means a method where a stream of ink drops is blasted onto a registration substrate or medium to form the desired printed image. The ink composition can be established on the recording medium via any appropriate inkjet printing technique. Examples of the inkjet printing method include methods such as a charge control method that uses electrostatic attraction to eject ink, a drop method, which uses vibration pressure from a piezo element, a method of printing by acoustic inkjet in which an electrical signal is transformed into an acoustic bead and the ink is irradiated with the acoustic bead in order to be ejected through radiation pressure, and a thermal jet injection method that uses pressure induced by bubbles formed through the heated paint. Non-limiting examples such that inkjet printing techniques thus include thermal, acoustic, and piezoelectric inkjet printing. In some examples, the ink composition is blasted onto the recording medium using an ink jet nozzle and / or an ink jet printhead. In some other examples, the inkjet composition is blasted onto the recording medium using thermal inkjet printheads.
    In some examples, the method for printing images with durable inkjet ink is a high-speed printing method. High speed means a method capable of printing more than 50 units (feet - feet) per minute. As an example, the network speed can be from about 50 to about 2000 units (feet) per minute. In some instances, the printing method is well suited for high-speed industry and commercial printing. In some other examples, the printing method is well suited for mail merge applications (in-line) and print transfer applications.
    An exemplary method for printing durable images on a recording medium includes applying the pre-treatment composition, as defined above, on the recording medium using a coating or coating device and blasting an ink composition on the said means of recording via ink jet nozzles, said ink composition including an aqueous liquid carrier and a dye.
    The coating is not particularly limited and can be appropriately selected from known coating equipment according to the intended use. Examples of coating equipment include: a medical air coating equipment, a blade coating, a rod coating, a knife coating, a pressure coating, an impregnation coating, a roller coating reverse, one with transfer roller coating, one with engraving coating, one with Kiss roller coating, one with release coating, one with spray coating, one with canvas coating, and one with extrusion coating. Details of the method can be found in Yuki Harasaki's Coating Kogaku (Coating Engineering). In some examples, the coating equipment is a device with a transfer roller for coating. In order to apply the pretreatment composition to the recording medium with a uniform thickness, an air blade can be used for the coating or a member having an acute angle can be positioned with an interval corresponding to the predetermined amount of the pretreatment composition -treatment, between the member and the means of registration.
    In some other examples, the application of the pretreatment composition can be done through any known commercial method such as engraving, inkjet method, spray coating method, and the cylindrical coating method. In some examples, the pretreatment composition is applied through a coating method using cylinders. Thus, as an example, the pretreatment composition is wound onto the recording medium using commercial roll coating equipment. Exemplary methods for printing durable images with inkjet inks on a recording medium thus include the application of the pre-treatment composition on the recording medium with roller or transfer roller coating devices. In some examples, a set of more than 3 rolls can be used. In some other examples, the printing method uses up to 30 cylinders.
    As an example, within said method, the pre-treatment composition is received on a first surface, and then a contact is formed between the first surface and a transfer roller. The pre-treatment composition is then transferred from a first surface to the transfer roller.
    Finally, the pre-treatment composition is transferred from the transfer roller to a printing medium. In one approach, the pre-treatment composition is applied to a print recording medium just prior to the printing of the inks by the heads. According to this method, one or more cylinders receive the pre-treatment composition and transfer to a printing medium. Therefore, the print medium receives inkjet ink from one or more inkjet printing heads.
    In some examples, the pre-treatment composition is applied to a recording medium using the coating devices and, subsequently, the ink is blasted by ink jet nozzles to register an image. Said inkjet ink composition includes an aqueous liquid carrier and a dye, the inkjet ink on which imprints said pretreatment composition. In some examples, the ink composition is applied to the recording medium using the inkjet nozzles, and is applied after the pretreatment composition is applied.
    In some examples, the time interval between the end point of applying the pretreatment composition on the recording medium and between the starting point of applying the ink composition between 0.0001 seconds and 80 seconds. In some other examples, the time interval is between 0.0001 seconds and 10 seconds. In some other examples, the time interval is between 0.0001 seconds and 1 second. In some examples, the time interval is between 5 seconds. In some other examples, the water-based paint composition is blasted onto a recording medium only after applying the pretreatment composition, while the pre-treatment composition is still wet on the recording medium, ensuring an appropriate mix between the pre-treatment composition. aqueous paint and pre-treatment composition.
    In some examples, the printing method may also include a drying process in which the solvent (especially water) present in the ink composition is removed by drying. Thus, in some instances, as an additional step, the recording medium is subjected to a hot air drying system. Alternatively, or in combination with the drying process, a process can be provided in which the solvent in the paint is removed by absorbing the solvent through the contact of a cylinder made of a porous material or the like with the surface of the recording medium. Additionally, a fixation process can be provided in which the image formed on the recording medium is fixed on at least one of the pressure application medium it applies.
    In some examples, the ink composition is established in at least a portion of the recording medium to form an image. In some other examples, the pretreatment composition can easily be applied to almost the entire area on the registration side of the registration medium, including an image portion to which the ink drop must be applied by the ink ejection unit. In some examples, the pre-treatment composition is set below the ink composition. The amount of the pre-treatment composition and / or the ink composition used depends, at least in part, on the desired image to be formed.
    As an illustrative example, the registration medium or substrate is paper (non-limiting example, which includes the copy plan of the paper or papers having fibers recycled in them), the offset printing plan on the paper in the form of a cylinder or photo- paper, and / or combinations thereof. In some examples, the recording medium has a thickness along substantially the entire length ranging from about 0.025 mm to about 0.5 mm. In some instances, the registration medium is a coated compensation medium. In some other examples, the registration medium is a non-porous registration medium. In some instances, the recording medium is an absorption medium. The absorption medium can be a low absorption medium, such as a coated compensation medium, or it can be a rapid absorption medium such as a flat paper. In some instances, the recording medium used in the present printing method is a low-absorption medium. In some other examples, the recording medium is a low absorption, non-porous recording medium.
    It should be understood that any number of colored ink composition can be used in the method. In addition, any desired combination of colored inks can be used. For example, each of the colored ink compositions may be a different color, or two or more of the inks may have different shades in the same color (that is, light magenta and dark magenta inks). In some examples of the method of the present invention, four different ink colors can be used: a black ink, a yellow ink, a cyan ink, and a magenta ink. In other examples, the method includes using any desired number of inks selected from black ink, yellow ink, cyan ink, magenta ink, orange ink, red ink, green ink, and / or combinations thereof. In some examples, the method includes the use of the pretreatment composition, as described here, and includes the use of at least the inkjet ink composition from a black ink, a yellow ink, a cyan ink, a magenta ink, an orange ink, a red ink, a green ink. In some examples, at least one ink is deposited inside the individual heads. Non-limiting examples of appropriate head configurations include the single head, dual head chambers, three-chamber and / or gender heads, and / or combinations thereof.
    As an example, the pre-treatment composition and ink composition are part of a printing system for printing durable inkjet images. Said printing system includes a pretreatment composition applicator containing at least one transfer cylinder and a pretreatment composition, and contains one or more successive inkjet printheads containing the inkjet ink composition. ink, said inkjet ink composition including an aqueous liquid carrier and a dye. In one example, the inkjet heads are thermal inkjet heads. In some examples, the printing system includes a pre-treatment composition applicator containing at least one transfer cylinder and a pre-treatment composition and at least four successive different inkjet heads containing, respectively, compositions of inkjet inks in black, cyan, magenta and yellow. The ink printing system, including the pre-treatment composition of the present invention, in addition to black and color inks, has excellent printing performance and image characteristics.
    In some examples, the present invention relates to a printing method and a printing system containing an ink composition including a dye dispersed in an ink vehicle and a pre-treatment composition as described above. In some examples, the ink composition includes one or more dyes, an aqueous carrier and, optionally, other ingredients such as surfactants, dispersants, binders, metallic particles (such as those used for MICR), and / or other additives and adjuvants well known in the relevant state of the art. In some examples, the ink composition is an inkjet ink composition. In some other examples, the ink composition is in an aqueous inkjet ink composition.
    In some examples, the dye is selected from a yellow dye, a magenta dye, a cyan dye, and a black dye, and the ink carrier includes at least one solvent present in an amount ranging from about 1 to about 25% by weight, at least one surfactant present in an amount ranging from about 0.1 to about 8% by weight, at least one polymer present in an amount ranging from about 0 to about 6% by weight, at least least one additive present in an amount up to about 0.2% by weight, and water.
    dye for each ink is selected from a pigment, a dye or combination thereof. In some examples, the ink contains pigments as dyes. As used herein, pigment refers to a dye particle that is substantially insoluble in the liquid carrier in which it is used. Pigments can be dispersed using a separate dispersing agent, or they can be self-dispersing, having a dispersing agent attached to the pigment surface. As used herein, self-dispersing generally refers to pigments that have been functionalized with a dispersing agent, such as through chemical bonding of the dispersing agent to the pigment surface. The dispersing agent can be a small molecule or a polymer or an oligomer. Pigments include both, as well as dispersed pigments, for example, pigments dispersed by a separate dispersing agent that is not covalently bonded to the surface. In one example, pigments are not self-dispersing, and dispersion aids can be added to the vehicle. In another example, the pigments are self-dispersing and modified to include at least one polymer chemically bonded to them.
    As noted, the dye pigment can be used in accordance with the embodiments of the present description. Specifically, if black is used, the black pigment can be any commercially available black pigment that has acceptable optical density and printing characteristics. Said black pigments can be manufactured by a variety of known methods, such as channel methods, contact methods, furnace methods, acetylene methods, or thermal methods, and are commercially available from the respective vendors, such as Cabot Corporation, Columbian Chemicals Company, Evonik, Mitsubishi, and EI DuPont de Nemours and Company. For example, commercially available carbon black pigments include: Color Black FW 200, Color Black FW 2V, Color Black FW1, Color Black FW 18, Color Black FW S160, Color Black FW S170, Printex including 95, 85, 75, 55 , 45, 300, 35, 35, 200, 12, and Special Blacks including: 4A, 4, 5, 6, 550, 350, 250, BP1100, BP900, BP800, M1100, M900, M800. Monarch 1400, Monarch 1300, Monarch 1000, Monarch 900, Monarch 880, and Monarch 700; Cab-O-Jet 200 and Cab-OJet 300; Raven 2500ultra, Raven 2000, Raven 7000, Raven 5750, Raven 5250, Raven 500, and Raven 3500; 45B, and combinations thereof. In addition to black, another dye pigment can be used, such as cyan, magenta, yellow, blue, orange, green, Pink, etc. Suitable organic pigments, for example, azo pigments include diazo pigments and monoazo pigments, polycyclic pigments (for example, phthalocyanine pigments such as, blue phthalocyanine and green phthalocyanine, perylene pigments, pyrinone pigments, anthraquinone pigments, quinacridone pigments, diaxozine pigments, thioindigo, isoindolinone pigments, pyrantronone pigments, and quinophthalone pigments), insoluble chelating dyes (e.g., basic dye chelates and acid dye chelates), nitropigments, nitrous pigments, antanthrone pigments, such as PR168, and the like. Representative examples of blue and green phthalocyanine include copper blue phthalocyanine, copper green phthalocyanine and derivatives thereof (blue pigment 15 and green pigment 36). Representative examples of quinacridones include: Pigment Orange 48, Pigment Orange 49, Pigment Red 122, Pigment Red 192, Pigment Red 202, Pigment Red 206, Pigment Red 209, Pigment Violet 19 and Pigment Violet 42. Representative examples of anthraquinones include Pigment Red 43 , Pigment Red 194, Pigment Red 177, Pigment Red 216 and Pigment Red 226. Representative examples of perylenes include Pigment Red 123, Pigment Red 190, Pigment Red 189, and Pigment Red 224. Representative examples of thioindigoids include Pigment Red 86, Pigment Red 87, Pigment Red 198, Pigment Violet 36, and Pigment Violet 38. Representative examples of yellow heterocyclics include Pigment Yellow 1, Pigment Yellow 12, Pigment Yellow 13, Pigment Yellow 14, Pigment Yellow 17, Pigment Yellow 73, Pigment Yellow 90, Pigment Yellow 110, Yellow Pigment 117, Yellow Pigment 120, Yellow Pigment lo 128, Pigment Yellow 138, Pigment Yellow 150, Pigment Yellow 151, Pigment Yellow 155, and Pigment Yellow 213. These pigments are commercially available in powder, pressed cake, or in dispersion form, from various sources. Pigments can be from about 5 nm to about ΙΟμιη; in another example, the pigments can be from 10 nm to about 500 nm in size, although the outer size of this range can be used if the remaining pigment can be dispersed and provide adequate printing property. In some examples, the amount of dye present in the Vaira ink composition is from about 2.0% by weight to about 4.5% by weight. It should be understood that the dye charge can be as much or as little as desired.
    As defined here, an ink vehicle refers to a vehicle in which the dye is placed to form the ink. A wide variety of ink carriers can be used with inks and printing methods according to the embodiments described here. Non-summative examples of components suitable for the paint vehicle include water-soluble polymers, anionic polymers, surfactants, solvents, co-solvents, buffers, biocides, sequestering agents, viscosity modifiers, surface active agents, chelating agents, resins, and / or water, and / or combinations thereof.
    Suitable solvents for the paint vehicle include, but are not limited to, polyoxyethyl glycerol ether, tripropylene glycol, tetraethylene glycol, 1— (2 - hydroxyethyl) -2-imidazolidinone, 1- (2-hydroxyethyl) -2pyrrolidone, 1,6 -hexanediol, 1,2,6-hexanotriol, trimethylolpropane, dipropylene glycol, Dantocol® DHE (Lonza Inc., Fairlawn NJ), and / or combinations thereof. The inks used in combination with the pretreatment composition having at least amine-N-oxide and the acid therein may include one or more of the following solvents: ethylene glycol, diethylene glycol, triethylene glycol, or l-propoxy-2-propanol. In a non-limitative example, the solvents are present in the paint vehicle in an amount ranging from about 15 by weight to about 25% by weight. In another non-limitative example, the solvents are present in the paint vehicle in an amount ranging from about 5% by weight to about 20% by weight. In yet another non-limitative example, the solvents are present in the paint vehicle in an amount ranging from about 8% by weight to about 18% by weight. The amount and type of solvent used depends, at least in part, on desired properties of the paint. In this way, the solvents can vary as desired. In some instances, a bonded solvent is used in the paint carrier for one or more of the colored inks. Examples of such solvents include, but are not limited to, tripropylene glycol, or 1- (2-hydroxyethyl) -2-pyrrolidone. In other examples, the inks include a mixture of two or more of the solvents previously listed.
    In some examples, the total weight percentage of the solvent mixture ranges from about 7% by weight to about 22% by weight. In other examples, the total weight percentage of the solvent mixture ranges from about 12% by weight to about 17% by weight. In yet another example, the total weight percentage of the solvent mixtures ranges from about 6% by weight to about 15% by weight.
    In some embodiments, the ink composition includes water. In some examples, water is used as in the paint vehicle for the composition and is part of the liquid vehicle. In some other examples, water even makes the ink composition balance, and may be present in an amount representing from about 40 to about 90% by weight, or representing from about 50 to about 80 weight% of the total composition.
    The surfactants for the paint vehicle are generally non-ionic or anionic. Suitable nonionic surfactants include, but are not limited to ethoxylated alcohol, fluorinated surfactants, 2diglycol surfactants, and / or combinations thereof. Specific examples of nonionic surfactants include surfactants from the Surfynol® series (for example, Surfynol® CT211, Surfynol® SEE), manufactured by Air Products and Chemicals, Inc., in addition to the surfactants (for example, Tergitol®) provided above, for the aqueous vehicle of the fastener. Non-limiting examples of anionic surfactants suitable for the paint vehicle include those anionic surfactants from the Dowfax® family (eg, Dowfax® 8390), manufactured by the Dow Chemical Company, located in Midland, MI, or anionic Zonyl® surfactants (for example , Zonyl® FSA), manufactured by EI DuPont de Nemours and Company; phosphate ester surfactant including surfactants from the 10 Emphos® series and the DeDophoS® series, both manufactured by Witco Corp., Widdlebury, Connecticut, the Hostaphat® series surfactants, manufactured by Clariant GmbH, Frankfurt, Germany, the ESI- series surfactants Terge®, manufactured by the composites Cook and Polymers Co., Kansas, 15 City, MO, the Emulgen® series surfactants, manufactured by Kao Specialties Americas LLc, High Point, Nalco, the Crodafos® series surfactants, manufactured by Croda Inc. , Edison, NJ, Dephotrope® series surfactants and DePHOS® series, both manufactured by DeForest 20 Enterprises Inc., Boca Raton, FI; alkyl sulfates (for example lauryl sulfate), alkyl ether sulfates (for example, sodium laureth sulfate); Nlauroil sarcosinate; dodecylbenzene sulfonate; and / or combinations of these. In some examples, the paint carrier includes 25 or more surfactants present in an amount of up to about 8% by weight, with other non-limiting examples including from about 0.1% by weight to about 6% by weight and about 1.2% by weight to about 2% by weight.
    In some embodiments, the paint carrier may include a polymer present in an amount ranging from about 0.01% by weight to about 4% by weight. In other examples, the paint vehicle includes at least polymers present in an amount ranging from about 0.1% by weight to about 1.5% by weight. Polymers 35 for the paint vehicle are generally water-soluble, and can be selected from those of the styrene- (meth) acrylate acid copolymer salts, polystyrene-acrylic polymers, polyurethanes, and / or other water-soluble polymeric binders , and / or combinations thereof. Non-limiting examples of suitable polyurethanes include those that are commercially available from Dainippon Ink & Chem., Inc. (DIC), located in Osaka, Japan.
    As a non-limiting example, a class of polymeric binders suitable for use in the paint include salts of styrene (meth) acrylic acid copolymers. A salt of a styrene (meth) acrylic acid copolymer includes at least one styrene backbone and a salt backbone of the styrene (meth) acrylic acid copolymer in its structure. It may also contain a skeleton derived from a monomer having another unsaturated group, such as a (meth) acrylate skeleton, in its structure. Non-limiting examples of styrene (meth) acrylic acid copolymers are commercially available and can be selected from the Joncryl® series (eg, Joncryl® 586 and 683), manufactured by BASF Corp, located in Florham Park, NJ; SMA -1000Na and SMA-1440K, manufactured by Sartomer, located in Exton, PA, Disperbyk 190, manufactured by BYK, Chemicals, located in Wallingford, CT; Polystyrene-acrylic polymers manufactured by Gifu Shellac, located in Japan, or combinations thereof.
    Additives can also be incorporated into the paint vehicle embodiments for the paints. As a non-limiting example, bactericides such as Proxel® GXL can be added to the paint to protect the paint from bacterial growth. Other suitable additives include, but are not limited to, buffers, biocides, sequestering agents, chelating agents, or the like, or combinations thereof. In some examples, the paint vehicle includes one or more additives present in an amount ranging from about 0.1% by weight to about 0.5% by weight. In other examples, no additives are present.
    Inks are generally prepared by combining solvents, surfactants, any additives and water, and adjusting the pH to a basic pH. In some examples, the pH of the ink ranges from about 7.0 to about 11. In other examples, the pH of the ink ranges from about 8.5 to about 9.5. The dyes and polymers are then added to form the paint compositions. Ingredients and abbreviations
    - Rhoplex® E-1691 is available from Rohm & Hass Company.
    - Hycar® 2679, Hycar® 0202, Vycar® 460x63 and Vycar® 460x46 are latex components available from Lubrizol Inc.
    Lucidene® 645 is an acrylic urethane polymer available from Rohm & Hass Company.
    - Neocar® Latex 2300 is available from Dow Chemical Company.
    - Ucar® latex 455 is a self-crosslinking acrylic latex available from Dow Chemical.
    - Suncryl® SV-100 is a styrene-vinyl-acetate available from Omnova Inc.
    - Carboset® As 860 is available from Lubrizol Inc.
    - Acronal® S 760 is a styrene acrylic latex polymer available from BASE.
    - Ucar® DT 400 is available from Dow Chemical.
    - AC 420® is an acrylic polymer available from GB Bond.
    - LEG-1 is a co-solvent available from Liponics.
    - Zonyl® ESQ is a surfactant available from Dupont Inc.
    Surfynol®SEF is a surfactant available from Air Products.
    - CAb-O-Jet®300 is a self-dispersing pigment available from Cabot Corporation.
    - Joncryl®586 is a styrene-acrylic binder available from BASF Corp.
    Example 1 - Preparation of the ink composition
    A black inkjet ink composition was prepared according to table 1 below. All percentages are expressed in percentages by weight (% by weight) based on the total weight of the paint composition.
    TABLE 1
    Component Quantity (% by weight) BP 700 black pigment 3.0 Cab-O-Jet® 300 1.0 Joncry® 586 1.0 2-Pyrrolidone 10.0 LEG-1 1.0 Zonyl® FSO 0.1 Proxel® GXL 0.1 Water Swing
    Example 2 - Preparation of the pre-treatment composition
    Pre-treatment compositions 1, 2 and 3 are prepared according to Table 2. All percentages are expressed by weight (% by weight) based on the total weight of the pre-treatment composition.
    TABLE 2
    Component Composition 1 Composition 2 Composition 3 Calcium chloride 9, 0 7.0 7.0 Latex Neocar® 2300 40.0 - - Rhoplex® E-1691 - 24.0 - Lucideno 645® - - 33.0 Zonyl® FSO 0.5 0.1 0.1 2-pyrrolidone 3.0 3.0 3.0 Surfynol® DF-210 0.5 0, 5 0.5 Proxel GXL® 0.1 0, 1 0.1 Water Up to 100% Up to 100% Up to 100%
    Pre-treatment compositions 1 to 3 were tested in combination with the black ink illustrated in example 1. The pre-treatment ink and composition are established in the coated Hewlett Packard compensation medium using Hewlett Packard type 88 heads. The pre-treatment formulations are coated on the medium (the coating weight for a mobile pretreatment is 0.5 to 10 grams / square meter) so 72mg / 300 dpi of the black ink was printed on top of each pre-treatment formulation .
    Example 3 - Stability of pretreatment compositions
    Pretreatment composition 1, as illustrated in example 2, including CaCls as metal salt, is tested with different resins having different acid numbers, for stability after one week at 60 ° C. The results are shown in table 3 below. These tests demonstrate that resins with a low acid number (ie NA below 20) are stable with the fixing agent while the resin with a high acid number is not.
    TABLE 3
    Resin Type Acid number Stability Rhoplex® E-1691 7.59 Yes Latex Neocar® 2300 11.4 Yes Hycar® 2679 15.7 Yes Vycar® 460x46 16, 2 Yes AC 420® 17, 9 Yes Vycar® 460x63 18.57 Yes Ucar® 455 20.6 No Hycar® 0202 20.6 No Suncryl® SV-100 24.4 No Carboset® AS 860 32.3 No Acronal® S 760 45.7 No Ucar® DT 400 49.4 No
    Example 4 - Performance of pre-treatment compositions
    Compositions I to V (as shown in Table 4) were tested for their printing performance.
    In Table 4, the numbers represent the percentage by weight (% by weight) based on the total weight of the pretreatment composition. The results are shown in TABLE 5.
    Flow control KOD Wet polishing Shine change, steel Dry polishing, rubber Performance good σ> -0, 11 1-Zz2 | -0.02 Composition I good 1.92 1O -1.5 0.07 CompositionII poor 1 1 Poor flow No data Comparative compositionIII good>00 -11, 6 0.32 Comparative compositionIV Poor CTí00 LO cn No data O Comparative composition V
    Water Proxel GXL® Surfynol® DF210 2-Pyrrolidone Zonyl® FSO OQro Lucideno® 645 resin Neocar® 2300 resinUp to 100% 0.1 0.5 CO O 15.0 1 30.0 Composition I Up to 100%0.5 GOO · * 15.0 33.0 1 CompositionII Up to 100%0.5 3.0 O 1 33.0 1 Comparative compositionIII Up to 100% ·> 0.5 3.0 O 15.0 1 1 Comparative compositionIV Up to 100% O cr 3.0 ** 1 1 1 Comparative composition V
    TABLE
    The compositions and comparative compositions I to V were evaluated for resistance to durability as for flow performance. For each impression, before and after the test, the optical density of the black is measured using an X-Rite densitometer to measure the reflection of the filled area.
    KOD reflects the optical density of the printing black. The higher KO value, the darker the black color image obtained.
    The dry polishing and wet polishing test refers to the ability of a printed image to withstand the degradation of the image appearance in dry and wet polishing. The numbers here refer to the difference in optical density that was measured. The lower the number is, the better the performance.
    The brightness change refers to the amount of brightness that the ink has when it has settled on a substrate. The change in brightness of the media sample is evaluated before and after the durability test. The brightness level is measured at 60 degrees using a Micro-HazePlus meter or a Micro-Tri-Gloss meter (manufactured by BYKGardner, Geretsried, Germany).
    The flow control is evaluated visually, the discharge from color to color is evaluated. The fee is based on the flow of ink over the media and the presence of defects. Poor reflects the presence of multiple defective flows; marginal reflects the presence of some flow rates and good does not reflect insignificant defects or defects.
    Example 5 - Composition and pre-treatment performance
    Various pretreatment compositions based on formulation 1 and containing different levels of Neocar® 2300 latex (0, 12, 18, 24, 30, 36, 42 and 48%) were evaluated for their printing performance and their durability. Said different compositions were laminated with an industrial coating machine in the middle. Then, a sequence of identical images was printed with black ink having the formulation as illustrated in Example 1, using an HP T-300 printer.
    The change in black optical density and the change in brightness of the media sample were evaluated. The KOD change and the brightness change were also assessed after the different durability tests using a Taber abrasion test instrument.
    The black optical density (KOD) is the measure of the change in reflection OD = log 10 (Ij / I r ) where li is the incident light intensity and I r is the reflected light intensity. The highest KOD value was for the darkest black color image obtained. For each impression, before and after the durability test, the optical density of the black was measured using an X-Rite densitometer to measure the reflection of the filled area.
    As used here, gloss level refers to the amount of gloss that the paint has when established on a substrate. The change in brightness of the media sample is evaluated: for each print, before and after the durability test, the level of gloss is measured at 60 degrees using a MicroHaze-Pluz meter or a Micro-Tri-Gloss meter (manufactured BYK-Gardner, Geretsried, Germany).
    The resistance tests were carried out on the printed medium. Rub resistance (rub) refers to the ability of a printed image to resist appearance degradation during image scraping (rubbing). A good resistance to friction, during scraping, will tend not to transfer ink from a printed image to the surrounding areas where the ink has not been printed, that is, on another printed color or on paper or another substrate. Three different abrasion tests are carried out: 2 dry rubbing with rubber (2R Eras), steel tip # 3 (2R Steel) and 1 wet rubbing (IR Wet). The differences in these tests are due to the type of abrasion used, the added weight and the size of the shock (inch strokes) on the printing.
    In the 2 dry rubber rub test (2R Eras), the dry rubber test uses a hard rubber (sand paper) to rub the printed surface with two scrapes on the same section of the print. The weight used was 350g of pressure (simulating manual pressure). In steel tip test # 3 (2R Steel), the steel tip was made of 0.25 inch diameter hard / blunt steel. The hard tip is rounded and has an extremely smooth finish, so that the damage to the image simulates the polishing / buffing effect that a nail can do on the impression. In test 1 polishing / wet friction (IR Wet), wet friction uses a weight of 350g, but only one shock is used through printing. The tip used for wet friction is a hard plastic tip covered with a cleaning cloth (tex-wipe). The tissue is soaked in water just before the test.
    The results are illustrated in Figure 1 and Figure 2. Figure 1 illustrates the black optical density (KOD) compared to the inkjet printing medium printed with different pretreatment compositions. Figure 2 illustrates and reflects the change in the brightness of the inkjet media with different pre-treatment compositions. According to this result, it is clear that the more resin is added, the better result is obtained, that is, no change in brightness and less change in KOD.
    The foregoing description has been presented only to illustrate and describes exemplary embodiments of the present invention. Although certain examples of method, compositions and articles of manufacture have been described here, the scope of protection covered by this patent is not limited to them. On the contrary, this patent application covers all methods, compositions and articles manufactured precisely within the scope of protection of the claims both literally and under the doctrine of equivalents.
    权利要求:
    Claims (14)
    [1]
    1. Pre-treatment composition for pre-treatment of a recording medium for receiving inkjet ink, said composition comprising:
    (a) an aqueous liquid vehicle;
    (b) a polyvalent metal salt as a fixing agent; and (c) a latex resin, characterized by the fact that the latex resin:
    has an acid number less than 20;
    it is present in an amount of 10 to 60% by weight of the pre-treatment composition; and is selected from: acrylic polymers and copolymers, vinyl acetate polymers or copolymers, polyester polymers or copolymers, vinylidene chloride polymers or copolymers, butadiene polymers or copolymers, styrenobutylene polymers or copolymers, polymers or polymers.
    [2]
    2. Pretreatment composition according to claim 1, characterized in that the fixing agent is a polyvalent metal salt selected from the group consisting of calcium chloride, calcium nitrate, magnesium nitrate, magnesium acetate or acetate of zinc.
    [3]
    3. Pretreatment composition, according to claim 1, characterized by the fact that the fixing agent is calcium chloride or calcium nitrate.
    [4]
    4. Pretreatment composition, according to claim 1, characterized in that the fixing agent is present in an amount of 1 to 20% by weight of the total weight of the pretreatment composition.
    Petition 870190095978, of 25/09/2019, p. 12/10
    2/3
    [5]
    5. Pretreatment composition according to claim 1, characterized in that the latex resin has an acid number less than 18.
    [6]
    6. Pretreatment composition according to claim 1, characterized in that the latex resin is a polymer or copolymer selected from the group consisting of acrylic polymers, vinyl-acrylic copolymers and acrylic polyurethane copolymers.
    [7]
    7. Pretreatment composition, according to claim 1, characterized in that the latex resin has an average molecular weight ranging from 150,000 to 300,000.
    [8]
    Pre-treatment composition according to claim 1, characterized in that it has a viscosity within the range of 1 to 2000 cps as measured at 25 ° C.
    [9]
    Pre-treatment composition according to claim 1, characterized in that it additionally comprises up to 1.5% by weight of surfactants.
    [10]
    10. Method for printing durable inkjet images on a recording medium, comprising:
    (a) applying a pretreatment composition to said recording medium, said pretreatment composition comprising an aqueous liquid carrier, a polyvalent metal salt as a fixing agent, and a latex resin; and (b) applying an ink composition on said recording medium, said ink composition comprising an aqueous liquid carrier and a colorant, with ink overprint, of said pretreatment composition, said method characterized by the fact that the latex resin of the pre-treatment composition:
    Petition 870190095978, of 25/09/2019, p. 12/11
    3/3 has an acid number less than 20;
    it is present in an amount of 10 to 60% by weight of the pre-treatment composition;
    is selected from: acrylic polymers and copolymers, vinyl acetate polymers or copolymers, polyester polymers or copolymers, vinylidene chloride polymers or copolymers, butadiene polymers or copolymers, styrenobutylene polymers or copolymers, polymers or copolymers.
    [11]
    11. Method for printing, according to claim 10, characterized in that the pre-treatment composition is applied on the said registration medium using a coating device and the ink composition is blasted on said registration medium via inkjet printer nozzles.
    [12]
    12. Method for printing, according to claim 10, characterized by the fact that the time interval between the end point of the application of the pre-treatment composition on the recording medium and between the initial point of application of the ink composition is between 0.0001 seconds and 80 seconds.
    [13]
    13. Method for printing, according to claim 10, characterized in that the pretreatment composition is rolled onto said recording medium using commercial roller coating equipment.
    [14]
    14. Printing method, according to claim 10, characterized in that the recording medium is a slow-absorbing non-porous recording medium.
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    同族专利:
    公开号 | 公开日
    BR112012028734A2|2016-07-19|
    EP2580293A4|2013-09-04|
    WO2011159371A9|2012-02-16|
    US20130076842A1|2013-03-28|
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    US8851652B2|2014-10-07|
    CN102933396A|2013-02-13|
    EP2580293A1|2013-04-17|
    WO2011159371A1|2011-12-22|
    BR112012028738A2|2016-07-19|
    JP2013530071A|2013-07-25|
    CN102884145B|2016-04-13|
    WO2011159274A1|2011-12-22|
    CN102884145A|2013-01-16|
    JP5688138B2|2015-03-25|
    EP2580293B1|2017-11-08|
    WO2011159370A1|2011-12-22|
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    法律状态:
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-01-29| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-07-02| B07A| Technical examination (opinion): publication of technical examination (opinion) [chapter 7.1 patent gazette]|
    2019-12-17| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-01-07| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 14/06/2010, OBSERVADAS AS CONDICOES LEGAIS. |
    2021-04-20| B21F| Lapse acc. art. 78, item iv - on non-payment of the annual fees in time|Free format text: REFERENTE A 11A ANUIDADE. |
    2021-08-10| B24J| Lapse because of non-payment of annual fees (definitively: art 78 iv lpi, resolution 113/2013 art. 12)|Free format text: EM VIRTUDE DA EXTINCAO PUBLICADA NA RPI 2624 DE 20-04-2021 E CONSIDERANDO AUSENCIA DE MANIFESTACAO DENTRO DOS PRAZOS LEGAIS, INFORMO QUE CABE SER MANTIDA A EXTINCAO DA PATENTE E SEUS CERTIFICADOS, CONFORME O DISPOSTO NO ARTIGO 12, DA RESOLUCAO 113/2013. |
    优先权:
    申请号 | 申请日 | 专利标题
    PCT/US2010/038562|WO2011159274A1|2010-06-14|2010-06-14|Pre-treatment composition|
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