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    • 专利摘要:
    COLORFUL SOLAR REFLECTIVE SYSTEM, METHODS FOR PREPARING A COLORFUL SOLAR REFLECTIVE SYSTEM, AND TO REDUCE THE ENERGY CONSUMPTION OF A STRUCTURE, COLORFUL COMPOSITION, USE OF COLORFUL COMPOSITION, COLORFUL SOLAR REFLECTIVE COATING, STRUCTURE, AND, ITEM. The present invention provides a colored solar reflective system comprising (1) a particulate material substantially in the crystalline habit of rutile and with an average particle size between about 0.5 (Mi) m and about 2.0 (Mi) m (2) ) an organic pigment with a maximum absorption coefficient of about 5,000 mm1 or more in the visible light region, a maximum dispersion coefficient of about 500 mmi or less in the visible light region and an average absorption coefficient of 500 mmi or least in the infrared region. The solar reflective system, which can be used in a coating composition or as a composition from which articles can be formed, has an intense dark color yet also providing better total solar reflectance.
    公开号:BR112012020387B1
    申请号:R112012020387-8
    申请日:2011-02-11
    公开日:2021-01-19
    发明作者:Karl Lowry；Emily Ruth Parnham；Sean Reid；John Robb；Rebecca Louise Tonkin；John L. Edwards
    申请人:Tioxide Europe Limited；
    IPC主号:
    专利说明:

    FIELD OF THE INVENTION
    [0001] This invention, in general, concerns improved colored solar reflective systems, colored compositions containing colored solar reflective systems, and various uses of such colored compositions. BACKGROUND OF THE INVENTION
    [0002] New technologies are being continuously developed to improve energy efficiency. One such technology is the use of reflective infrared pigments in coatings positioned outside buildings (or another object). As you know, the sun emits about 50% of its energy as radiation near infrared. When this near-infrared radiation is absorbed, it is physically converted to heat. Coatings containing infrared reflective pigments work by reflecting sunlight and blocking heat transfer, thereby reducing the thermal load on the building. For example, white pigments, such as titanium oxide, have been used in coatings to reflect most of the sun's energy. It is often desirable to provide a colored coating instead of white for aesthetic reasons. However, the selection of non-white pigments that are available for use is limited, as they tend to absorb more energy from the sun than is desired, leading to a marked reduction in the aforementioned effect. Thus, several systems have been and continue to be developed to provide colored coatings with better solar reflectance.
    [0003] For example, US patent number 5,540,998 describes a system in which two or more non-white pigments with particle diameters of 50 μm or less are combined to produce a low luminosity color, and in particular achromatic black. US patent number 5,962,143 additionally describes a black colored coating that contains one or more black pigments, one or more non-white pigments and silicic acid.
    [0004] In US patent number 6,174,360, it is prescribed that the use of complex inorganic colored pigments (CICP's) in coatings presents dark brown colors in the visible portion together with reflexivity in the near infrared portion of the electromagnetic spectrum.
    [0005] US patent number 6,336,397 describes an infrared reflective system containing two or more layers, with one layer containing a resin and pigment that provide the desired color and another layer containing a pigment that provides infrared reflectance. US patent publication number 2009/0268278 also discloses a two-layer infrared reflective system with a top layer consisting of a synthetic resin and an organic pigment and a bottom layer consisting of a synthetic resin and a white oxide-based pigment of titanium.
    [0006] Furthermore, US patent number 6,521,038 provides for a mixed pigment that reflects near the infrared containing a non-absorbent dye near the infrared and a white pigment that is coated with a dye like this. The mixed pigment can then be used as a coloring agent in coatings.
    [0007] Finally, WO 2009/136141 describes the use of particulate material of near-infrared dispersion that provides high reflection of near-infrared radiation and low reflectance of visible light in combination with various non-white dyes.
    [0008] While each provides solar reflectance, some of the disadvantages of using these currently available systems include: they provide relatively faded coloring, since a high level of conventional titanium dioxide is required to give the desired level of solar reflection; the application of two or more layers is both time-consuming and expensive and can result in coatings with a patched or non-uniform appearance that tends to clear over time; and impurities contained in the systems can lead to absorptions in the near infrared part of the spectrum resulting in a reduction in solar reflectance. As such, alternative systems that exhibit better solar reflectivity over a wide range of uniform dark colors or more intense than can be otherwise obtained are still highly desirable. SUMMARY OF THE INVENTION
    [0009] The present invention provides a colored solar reflective system including a particulate material with a large average particle size and an organic pigment that is chosen based on the following properties: (i) it has to absorb strongly in the region of visible light; (ii) it has to absorb negligibly in the region of light close to the infrared; and (iii) it has to disperse light negligibly in the region of visible light. The solar reflective system, which can be used in a coating composition or as a composition from which articles can be formed, has an intense dark color yet also providing better total solar reflectance.
    [00010] In one aspect, the present disclosure provides a colored solar reflective system containing (1) a particulate material substantially in the crystalline habit of rutile and with an average particle size between about 0.5 μm and about 2.0 μm and (2) an organic pigment with a maximum absorption coefficient of about 5,000 mm-1 or more in the visible light region, a maximum dispersion coefficient of about 500 mm-1 or less in the visible light region, and a average absorption coefficient of about 50 mm-1 or less in the near-infrared light region. In some embodiments, the organic pigment with the mentioned properties can be a single organic pigment or it can be a mixture of organic pigments where each pigment has the mentioned properties.
    [00011] In another aspect, the colored solar reflective system can be dispersed in a vehicle to form a colored composition. The colored composition can then be used as a layer coating or as a composition from which articles can be formed. BRIEF DESCRIPTION OF THE FIGURES
    [00012] For a detailed understanding and better appreciation of the present invention, reference should be made to the following detailed description of the invention, considered together with the attached figure.
    [00013] Figure 1 is a graph representing the reflectance for ral 8007 (yellowish brown) at various wavelengths. It shows reflectance as a function of wavelength for ral 8007 (yellowish brown) for a comparative system and an inventive reflective system. DESCRIPTION OF THE PREFERRED EMBODIMENT (S)
    [00014] In this specification and in the following claims, reference will be made to numerous terms that must be understood with the following meanings.
    [00015] The terms "visible light" refer to electromagnetic radiation with a wavelength in the range of 400 nm to 760 nm of the electromagnetic spectrum.
    [00016] The terms "near-infrared light" refer to electromagnetic radiation with a wavelength in the range of 760 nm to about 2500 nm of the electromagnetic spectrum.
    [00017] The terms "total solar reflectance" or "TSR" refer to the fraction of incident solar energy (-360 nm-2500 nm) that is reflected by a surface in question. It is a ratio of energies of the reflected wave to that of the incident wave. For example, a reflectance of 0.8 is equal to a reflectance of 80% of the incident wave. The total solar reflectance can be determined in the manner specified in the standard test method ASTM E903, whose contents in the integrals are incorporated herein by reference.
    [00018] The terms "organic pigment" refer to an organic particle (s) substantially insoluble in the application medium in which it (s) is (are) dispersed (s) and which gives color.
    [00019] The terms "energy consumption" refer to the use or consumption of conventional forms of energy, for example, electricity, gas, etc. Thus, the reduction of energy consumption in a structure is related to the reduction of the use, for example, of electricity in the structure.
    [00020] The term "structure" refers to any object that can be exposed to the sun, for example, a building, an automobile, a train, a container, a vase, piping, a road, floor, a lane. , a parking lot, sidewalk, a swimming pool, a deck, a textile product, an airplane, a ship, a submarine, a window profile, bypass, roof granules, thin tile roof, an agricultural film, or a glass product . The material of the structure is not limited; therefore, it can comprise metal, glass, ceramics, plastic, concrete, asphalt, wood, tile, natural or artificial fibers, rubber, etc.
    [00021] The present disclosure relates in general to colored solar reflective systems. It has surprisingly been observed that the colored solar reflective systems of the present invention allow color to be decoupled from reflection properties close to the infrared, that is, reflectance and photocatalytic properties close to the infrared of the colored systems can be varied regardless of color. Thus, once a desired color has been achieved with certain organic pigments, the desired solar reflectance properties, which depend on the concentration of particulate, can then be achieved independently.
    [00022] Colored solar reflective systems also provide better infrared reflectivity in structures made with or covered by these systems, while also providing previously inaccessible colors and tones, including, but not limited to, the blue part of the color spectrum. For example, applying the present colored solar reflective system to an exterior surface of a structure, such as a wall or ceiling, allows the structure to exhibit greater total solar reflectance. This, in turn, results in a lower surface temperature and heat transfer through the coated structure. Therefore, the interior temperature of the structure is lower and therefore less energy is needed to cool the interior of the structure. In addition, the potential evaporative loss of any volatile component contained in the structure is reduced. In addition, structural integrity is improved, as heat damage, such as cracks and thermal warping, is significantly reduced. Finally, the colored solar reflective system can be applied in a single layer coating, reducing cost time while still providing consistent color in the applied coating.
    [00023] According to one embodiment, the colored solar reflective system includes (1) a particulate material substantially in the crystalline habit of rutile and with an average particle size between about 0.5 μm and about 2.0 μm, preferably between about 0.6 μm and about 1.7 μm, and even more preferably between about 0.7 μm and about 1.4 μm and (2) an organic pigment with a maximum absorption coefficient of about 5,000 mm-1 or more, preferably about 10,000 mm-1 or more, and more preferably about 15,000 mm-1 or more in the visible light region, a maximum dispersion coefficient of about 500 mm-1 or less, preferably about 250 mm-1 or less, and more preferably about 100 mm-1 or less in the visible light region, and an average absorption coefficient of about 50 mm-1 or less, preferably about 30 mm-1 or less , and more preferably about 10 mm -1 or less in the near-infrared light region.
    [00024] In one embodiment, the particulate material is selected from titanium dioxide, doped titanium dioxide, and a mixture of these.
    [00025] The titanium dioxide suitable in the present invention is one capable of dispersing near-infrared light while also providing low dispersion and low absorbance of visible light. Such properties can be obtained when titanium dioxide has an average particle size between about 0.5 μm and about 2.0 μm. In yet another embodiment, titanium dioxide has an average particle size between about 0.6 μm and about 1.7 μm, and more preferably between about 0.7 μm and about 1.4 μm. It was surprisingly observed that such titanium dioxide reflects near-infrared light at an unusually high level, also showing remarkably low visible light reflectance when compared to conventional titanium dioxide pigment. In addition, unlike conventional titanium dioxide, which is very reflective of visible light making conventional color systems in which it is used faded, the titanium dioxide of the present invention mixes with the organic pigment without affecting the color of the system too much. to provide a more widely available palette of dark, or more intensely colored systems.
    [00026] As skilled in the art, the crystal size is different from the particle size. Crystal size is related to the size of the fundamental crystals that make up the particulate material. These crystals can then aggregate to a certain degree to form larger particles. For example, conventional titanium dioxide in the rutile crystalline habit has a crystal size of about 0.17 μm - 0.29 μm and a particle size of about 0.25 μm - 0.40 μm, while Conventional titanium in the form of anatase crystal has a crystal size of about 0.10 μm - 0.25 μm and a particle size of about 0.20 μm - 0.40 μm. The particle size is thus affected by factors such as the crystal size as well as lamination techniques used during production, such as dry, single or incorporative lamination. Thus, in some embodiments, the particle size of titanium dioxide is larger than the crystal size. In still other embodiments, the particle size of titanium dioxide is approximately equal to the crystal size.
    [00027] The crystal size and particle size of titanium dioxide can be determined by methods well known to those skilled in the art. For example, the crystal size can be determined by transmission electron microscopy on a polished sample with image analysis of the resulting photograph. The result of the crystal size can additionally be validated by reference using NANOSHPHERE ™ latex size standards (available from Thermo Scientific). One method that can be used to determine the particle size of titanium dioxide includes X-ray sedimentation.
    [00028] Because of the higher refractive index, the particulate material contains titanium dioxide in a crystalline habit of substantially rutile. Thus, according to another embodiment, more than 90% by weight of titanium dioxide, preferably more than 95% by weight of titanium dioxide, and even more preferably more than 99% by weight of titanium dioxide, based on total weight of the particulate material, are in the crystalline habit of rutile. In yet another embodiment, the particulate material may additionally contain titanium dioxide which is in the form of an anatase crystal.
    [00029] Known processes that can be used to prepare titanium dioxide include, but are not limited to, the sulfate process, chloride process, fluoride process, hydrothermal process, aerosol process and leaching process; however, each such known process is modified by one or more of the following conditions: (a) treatment at a higher temperature, for example, 900 ° C or more; (b) treatment for a longer period of time, for example, 5 hours or more; (c) increase or decrease in typical levels of growth moderators present during the process; and (d) reduction of the typical level of rutile seeds.
    [00030] Thus, for example, titanium dioxide can be prepared by the sulfate process, which generally includes: (i) reacting a titaniferous feed stock with sulfuric acid to form a water-soluble solid reaction cake; (ii) dissolving the reaction cake in water and / or weak acid to produce a solution of titanium sulfate; (iii) hydrolyze the titanium sulfate solution to convert titanium sulfate to titanium dioxide hydrate; and (iv) separating the precipitated titanium dioxide hydrate from the solution and calcining to obtain titanium dioxide, in which the process is modified by one or more of the conditions (a) - (d) described above. In one embodiment, the process is modified by condition (a); in another, the process is modified by condition (b); in another, the process is modified by condition (c); and in another, the process is modified by condition (d).
    [00031] The titanium dioxide of the present disclosure may be white or translucent or may be colored. Preferably, titanium dioxide is white. Thus, in one embodiment, titanium dioxide has a luminosity value L * (CIE color space L * a * b *) greater than 95, an a * value less than 5 and a b * value less than 5.
    [00032] Preferably, the particulate material contains more than 70% by weight of titanium dioxide, based on the total weight of the particulate material. In another embodiment, the particulate material contains more than 80% by weight, preferably more than 90% by weight, more preferably more than 95% by weight and even more preferably more than 99.5% by weight of titanium dioxide, with based on the total weight of the particulate material.
    [00033] In another embodiment, the particulate material is doped titanium dioxide. In the form used herein, "doped titanium dioxide" refers to the titanium dioxide of the present disclosure but additionally including one or more dopants that have been incorporated during the preparation of titanium dioxide. Doping agents, which can be incorporated by known methods, may include, but are not limited to, calcium, magnesium, sodium, vanadium, chromium, manganese, iron, nickel, aluminum, antimony, phosphorus, niobium or cesium. The dopant can be incorporated in an amount of not more than 30% by weight, preferably not more than 15% by weight, and more preferably not more than 5% by weight, based on the total weight of titanium dioxide. For example, the dopant can be incorporated in an amount of 0.1 to 30% by weight, or 0.5 to 15% by weight, or 1 to 5% by weight, based on the total weight of titanium dioxide. Due to its higher refractive index, such doped titanium dioxide can be recognized as being in a crystalline habit substantially of rutile. In other embodiments, the particulate material may additionally contain doped titanium dioxide in the form of an anatase crystal.
    [00034] In yet another embodiment, the particulate material can additionally be treated as known in the art with a coating agent to form coated titanium dioxide or coated doped titanium dioxide. For example, the particulate material can be dispersed in water together with the coating agent. The pH of the solution can then be adjusted to precipitate the desired hydrated oxide to form a coating on the surface of the particulate material. After coating, the particulate material can be washed and dried before being crushed, for example, in a fluid energy mill or micronizer, to separate particles stuck to the coating. At this grinding stage, an organic surface treatment can also be applied if desired.
    [00035] Coating agents suitable for use include those normally used to coat an inorganic oxide or aqueous oxide on the particle surface. Typical inorganic oxides and aqueous oxides include one or more oxides and / or aqueous oxides of silicon, aluminum, titanium, zirconium, magnesium, zinc, cerium, phosphorus, or tin, for example, AI2O3, SiO2, ZrO2, CeO2, P2O5, silicate sodium, potassium silicate, sodium aluminate, aluminum chloride, aluminum sulfate, or a mixture of these. The amount of coating coated on the surface of titanium dioxide or doped titanium dioxide can vary from about 0.1% by weight to about 20% by weight of the inorganic oxide and / or aqueous oxide in relation to the total weight of the dioxide titanium or doped titanium dioxide.
    [00036] Organic surface treatments suitable for application in the crushing stage include polyols, amines, alkyl phosphonic acids and silicone derivatives. For example, the organic surface treatment may be trimethylpropane, pentaerythritol, triethanolamine, n-octyl phosphonic acid or trimethylethane.
    [00037] In addition to the aforementioned particulate material, the colored solar reflective system also includes an organic pigment. According to various modalities, the organic pigment can be selected from a black, brown, blue, cyan, green, violet, magenta, red, orange, yellow pigment and a mixture of these. The selection will depend on the necessary organic pigments required to achieve the desired color, for example, blues, reds, browns and strong greens. The organic pigment can be obtained from commercial sources and is chosen based on the following properties: (i) it has to absorb strongly in the region of visible light; (ii) it has to absorb negligibly in the region of light close to the infrared; and (iii) it has to disperse light negligibly in the region of visible light. To “absorb strongly in the visible light region”, the organic pigment must have a maximum absorption coefficient of at least about 5,000 mm-1, preferably at least about 10,000 mm-1, and more preferably at least about 15,000 mm-1 in the visible light region. To “absorb negligibly in the region of light near infrared”, the organic pigment must have an average absorption coefficient of less than about 50 mm-1, preferably less than about 30 mm-1, more preferably less than about 15 mm-1, and even more preferably less than about 10 mm-1 in the near-infrared light region. To "disperse light negligibly in the region of visible light", the organic pigment must have a maximum dispersion coefficient of less than about 500 mm-1, preferably less than about 250 mm-1, and more preferably less than about 100 mm-1 in the visible light region. The absorption and dispersion coefficients can be determined by methods well known to those skilled in the art, for example, such as those described in “Solar Spectral Optical Properties of Pigments - Part I: Model for Deriving Scattering and absorption Coefficients From Transmittance and Reflectance Measurements” , R Levinson et al., Solar Energy Materials and Solar Cells 89 (2005) 319-349, whose contents in full are incorporated herein by reference.
    [00038] In some embodiments, the organic pigment is an organic pigment with the properties described above (i), (ii) and (iii). In other embodiments, the organic pigment is a mixture of more than one organic pigment, each with the above-described properties (i), (ii), and (iii). In other embodiments, the colored solar reflective system is characterized by additionally containing less than about 5% by weight, based on the total weight of the colored solar reflective system, of one or more organic pigments that do not have the above-described properties (i) , (ii) and (iii). In yet another embodiment, the colored solar reflective system is characterized in that it additionally contains less than about 2.5% by weight, preferably less than about 1% by weight, based on the total weight of the colored solar reflective system, of one or more organic pigments that do not have the properties described above (i), (ii) and (iii). In one embodiment, the colored solar reflective system contains from 0 to 2.5% by weight, as well as from 0.1 to 1% by weight, based on the total weight of the colored solar reflective system, of one or more organic pigments that do not have the properties above (i), (ii) and (iii).
    [00039] According to one embodiment, the (or each) organic pigment can be an azo pigment, anthraquinone, phthalocyanine, perinone / perylene, indigo / thioindigo, dioxazin, oxazin, isoindolinone, isoindoline, diketopyrrolepyrole, azomethine or azometin-azozo .
    [00040] The colored solar reflective system can be formed by combining particulate material and organic pigment. Thus, in one embodiment, the colored solar reflective system can be prepared by a method comprising mixing the particulate material with the organic pigment. Mixing can take place by any known means.
    [00041] In yet another embodiment, the present disclosure provides a colored composition containing the colored solar reflective system dispersed in a vehicle. The vehicle can be any component or combination of components in which the colored solar reflective system can be dispersed. The amount of the colored solar reflective system included in the colored composition is an amount sufficient to provide about 0.1 volume% to about 20 volume% of organic pigment, based on the total volume of the color composition, and about 0, 5% by volume to about 40% by volume of particulate material, based on the total volume of the colored composition. Thus, in one embodiment, the colored composition comprises about 0.1% by volume to about 20% by volume of organic pigment and about 0.5% by volume to about 40% by volume of particulate material, based on in the total volume of the colored composition, dispersed in a vehicle.
    [00042] According to one modality, the vehicle is a natural or synthetic resin. The resin may be, but is not limited to, a polyolefin resin, poly (vinyl chloride) resin, ABS resin, polystyrene resin, methacrylic resin, polycarbonate resin, poly (ethylene terephthalate) resin, polyamide resin, alkyd resin, acrylic resin, polyurethane resin, polyester resin, melamine resin, fluoropolymer, or epoxy resin.
    [00043] In another mode, the vehicle is a carrier. The carrier can be, but is not limited to, an aqueous solvent, for example, water. The carrier can also be a non-aqueous solvent, for example, an organic solvent such as a petroleum distillate, alcohol, ketone, ester, glycol ether and the like.
    [00044] In yet another modality, the vehicle is a binder. The binder can be, but is not limited to, a metal silicate binder, for example, an aluminosilicate binder. The binder can also be a polymeric binder, for example, a polymer binder or acrylic copolymer.
    [00045] The colored composition may additionally include one or more usual additives. Suitable additives for use include, but are not limited to, thickeners, stabilizers, emulsifiers, texturizers, adhesion promoters, UV stabilizers, anti-luminosity agents, dispersants, antifoam agents, wetting agents, coalescing agents, and biocides / fungicides.
    [00046] The colored composition may also include one or more spacer particles usable in the spacing and support of the material contained in the composition. The spacer particles can be silica, silicates, aluminates, sulfates, carbonates, clays, or polymeric particles in the form of hollow beads or in the form of microspheres.
    [00047] The colored composition can be used as a coating composition, for example, as a common ink, pen ink, liquid coating, powder coating, etc., or it can be used as a composition, for example, as a plastic or polymer molding composition, of which articles can be formed by molding, extrusion or other known processes.
    [00048] Thus, in one embodiment, the present disclosure provides a colored solar reflective coating of a layer containing the colored solar reflective system dispersed in the vehicle. In another embodiment, the colored solar reflective coating of a layer has a luminance value L * (CIE color space L * a * b *) of 75 or less, preferably 65 or less, more preferably 55 or less, and yet more preferably 45 or less.
    [00049] As mentioned earlier, the colored solar reflective system also provides better near-infrared reflectivity. Thus, in another embodiment, the colored solar reflective coating of a layer has a total solar reflectance greater than 30%. In yet another embodiment, the colored solar reflective coating of a layer has a total solar reflectance greater than 35%, preferably greater than 40%, and even more preferably greater than 45%.
    [00050] Once formulated, the reflective solar colored coating of a layer can be applied to one or more surfaces of a structure. Thus, in another embodiment, the present disclosure provides a structure comprising the solar reflective colored coating of a layer.
    [00051] In another embodiment, the colored reflective solar coating of a layer covers a substrate, where the substrate absorbs a proportion of radiation close to infrared. The thickness of the reflective layer is such that more than 1% of the incident radiation near the infrared reaches the substrate.
    [00052] In yet another embodiment, the present disclosure provides a method for reducing the energy consumption of a structure by applying the solar reflective colored coating of a layer to one or more surfaces of the structure. The reflective colored solar coating of a layer can be applied by any known device, for example, brush application, roller application, sprinkling, immersion, etc. Due to its better reflectivity close to the infrared, the colored solar reflective coating of a layer causes the surface temperature of the resulting coated surface to be reduced in relation to the surface temperature of a surface coated with a non-reflective coating of the same color. Thus, less energy is needed to cool the interior of the structure.
    [00053] The solar reflective colored coating of a layer shown here can also be applied to the surface of a structure after one or more primers have been applied to the structure. For example, the surface of the structure can be coated with a primer prior to the application of a colored coating of a layer.
    [00054] The present disclosure also provides an article comprising the colored composition. In one embodiment, the article has a brightness value L * (CIE color space L * a * b *) of 75 or less, preferably 65 or less, more preferably 55 or less, and even more preferably 45 or less.
    [00055] As mentioned earlier, the colored solar reflective system also provides better near-infrared reflectivity. Thus, in another modality, the article has a total solar reflectance greater than 30%. In yet another embodiment, the article has a total solar reflectance greater than 35%, preferably greater than 40%, and even more preferably greater than 45%. Total solar reflectance can be determined according to the method described in ASTM E903.
    [00056] The present invention will be further illustrated taking into account the following examples, which should be exemplary of the invention. Examples Example 1A. An experimental program was carried out to match the color 8007 (yellowish brown). The target was: L * = 39.56, a * = 12.20, and b * = 18.01. Organic pigments PB60 (Albion Colors Bricofor Blue 3GRP), PY154 (High performance colors PY1540) and PR122 (High performance colors PR1220), where PB60 and PY154 were used in combination with titanium dioxide with an average particle size of 1.4 μm. This system was then compared to a system containing the inventive combination of organic pigments PY128 (Ciba 8GNP), PR122 (High performance colors PR1220) and PV23 (Ciba Cromophtal Violet Gt) with titanium dioxide with an average particle size of 1.4 μm .
    [00057] A dye concentrate was prepared for each of the specified pigments (PB60, PY154, PR122, PY128, PV23) using an acrylic resin, a wetting and dispersing additive, a solvent and the specified dye. The quantities of each component are specified in table 1. This tincture concentrate was ground with steel ballotini.
    Table 1: Components of the tincture concentrate
    [00058] A colored resin solution was then constituted by taking the quantities specified in table 2 of each of the required dye concentrates and mixing vigorously for 2 minutes with the specified amount of additional acrylic resin.
    Table 2: Constitution of the colored resin solution
    [00059] Titanium dioxide (amount specified in table 3) was added to 7.5 g of the colored resin solution to create a base mixture that was then vigorously mixed for 30 seconds. This dyed base mixture was then left with an additional 13 g of colored resin. This base mixture was then ground for a further 2 minutes.
    Table 3: Amount of titanium dioxide added to the colored resin solution.
    [00060] The common test paint was then applied to an opacity card using a number 150 coiled wire applicator; whose caliber determined the nominal wet film thickness. The solvents evaporated naturally and the panel was heated in an oven at 105 ° C for 30 minutes. This process was then repeated to give a second coating.
    [00061] Reflectance spectra were measured using a UV / vis / NIR spectrophotometer with an integrating sphere and a wavelength range of 300 nm - 2500 nm. The total solar reflectance was calculated from these data, according to the method described in ASTM E903. L *, a * & b * in a D65 illuminant, were also calculated from these data.
    [00062] In an attempt to achieve the same% TSR in the comparative system as in the inventive system, TiO2 PVC had to be increased in the comparative system. Despite this increase, it was not yet possible to reach the highest% TSR of the inventive system. The required color was also not obtainable in the comparative system, since the yellow pigment dispersed significant light in the visible light region. The blue pigment showed significant absorption in the region above 760 nm, decreasing the potential reflectance. This can be seen clearly in figure 1 where there is much less reflectance after 760 nm in the comparative system. Despite the additional titanium dioxide in the comparative system, the% TSR is even lower than in this system, compared to the inventive system because of the absorption in the region near the infrared by the blue pigment. The% TSR for each system is provided in table 4 below.
    Table 4:% TSR for ral 8007. Example 1B. A PVC plate was made in color 8007 (yellowish brown) using titanium dioxide with an average particle size of 1.4 μm. Stock solutions of PY128 (Ciba 8GNP), PR122 (High performance colors PR1220) and PV23 (Ciba Cromophtal Violet Gt) were prepared by mixing 40 g of each pigment with 350 g of acetylbutyl citrate.
    Table 5: PVC formulation
    [00063] The PVC plate was prepared as follows: a dry mixture was prepared using a crypto-peerless mixer. A J.R.Dare two-roller laminator (140 ° C front and 135 ° C rear roll) was then used to produce PVC. The resulting PVC was preheated for 3 minutes at 165 ° C then pressed for 2 minutes at 15te / in2.
    [00064] Reflectance spectra were measured using a UV / vis / NIR spectrophotometer with an integrating sphere and a wavelength range of 300 nm - 2500 nm. The total solar reflectance was calculated from these data, according to the method described in ASTM E903 and was determined equal to 50.87%. Example 2. The inventive titanium dioxide system with an average particle size of 1.4 μm and organic pigments PY180 (Clariant Fast Yellow HG), PR122 (HPC PR1220), PV23 (Ciba Cromophtal Violet Gt), PB15: 3 (HPC PB1530 ), PBlack 32 (BASF Paliogen Black L0086), P071 (Ciba Irgazin DPP Cosmoray) were used in an ink system to make colored dyes and the specified ink 6011, 7010, 7022 and 7034.
    [00065] A dye concentrate was prepared for each of the specified pigments (PY180, PR122, PV23, PB15: 3, PBlack 32, P071) using an acrylic resin, a wetting and dispersing additive, a solvent and the specified ink. The amounts of each component are specified in table 6. This dye concentrate was then ground with steel ballotini. PV23, PB 15: 3, PBlack32 PR122, PY180, PO71
    Table 6: Components of the tincture concentrate.
    [00066] A colored resin solution was constituted by taking the amounts specified in table 7 of each of the required dye concentrates and mixing vigorously for 2 minutes with the specified amount of additional acrylic resin.
    Table 7: Constitution of the colored resin solution
    [00067] Titanium dioxide was added, in the quantities specified in table 8, to 7.50 g of the colored resin solution to create a base mixture which was then vigorously mixed for 30 seconds. This dyed base mixture was then left with an additional 13.00 g of colored resin. This base mixture was then ground for a further 2 minutes.
    Table 8: Amount of titanium dioxide added to the colored resin solution
    [00068] The common paint was launched on a black substrate using an applicator wound with number 6 wire to give a dry film thickness of about 28 microns. The solvents evaporated naturally and the panel was then heated in an oven at 105 ° C for 30 minutes. Reflectance spectra were measured using a UV / vis / NIR spectrophotometer with an integrating sphere and a wavelength range of 300 nm - 2500 nm. The total solar reflectance was calculated from these data, according to the method described in ASTM E903.
    [00069] The% TSR was compared with data collected from publications of TSR values available for optimized systems using complex inorganic color pigments. The known TSR values were reported calculated according to ASTM E903 (weighted ordinates for 300-2500 nm), measured on the top coat and primer. The inventive system was not thus optimized since the solar reflectance was measured on a black substrate, but it can be seen from table 9 that there is still a significant increase in% TSR for the inventive system.
    Table 9:% TSR values for various ral numbers. Example 3. Ral 7024 (graphite gray) was made using 4 different average particle sizes of titanium dioxide (0.7 micron, 1.1 micron, 1.4 micron, and 1.7 micron) and organic pigments PY180 (Clariant Fast Yellow HG), PV23 (Ciba Cromophtal Violet Gt), PBlack 32 (BASF Paliogen Black L0086). The organic pigments were made in dye concentrates, detailed in table 6 above. A colored resin solution was then constituted by taking the amounts specified in table 10 of each of the required dye concentrates and mixing vigorously for 2 minutes with the specified amount of additional acrylic resin.
    Table 10: Constitution of the colored resin solution and amount of titanium dioxide added to the colored resin solution.
    [00070] Titanium dioxide was added to 7.50 g of the colored resin solution to create a base mixture that was then vigorously mixed for 30 seconds. This dyed base mixture was then left with an additional 13.00 g of colored resin. This base mixture was then ground for a further 2 minutes. This produced a 10% volume concentration of TiO2 in all four common paints.
    [00071] Ordinary paint was dropped onto a substrate using a number 150 coiled wire applicator to give a dry film thickness of about 77 microns. The solvents evaporated naturally and the panel was heated in an oven at 105 ° C for 30 minutes. Reflectance spectra were measured using a UV / vis / NIR spectrophotometer with an integrating sphere and a wavelength range of 300 nm - 2500 nm. The total solar reflectance was calculated from these data, according to the method described in ASTM E903 and the results are provided in table 11.
    Table 11: TSR result for ral 7024
    [00072] The 0.7 micron particle size TiO2 gives the highest TSR value, but requires that a large amount of organic compounds be added to maintain color because of the TiO2 pastel effect. The 1.1 and 1.4 micron TiO2 still gives a high TSR value, but uses about 2/3 of the amount of organic compounds when compared to the 0.7 μm particle size TiO2.
    [00073] The matter in question is to be considered illustrative, not restrictive, and the appended claims are intended to cover all such modifications, improvements, and other modalities, which fall within the real scope of the present invention. Thus, to the maximum extent permitted by law, the scope of the present invention must be determined by the most comprehensive interpretation possible of the following claims and their equivalents, and must not be restricted or limited by the following detailed description.
    权利要求:
    Claims (14)
    [0001]
    1. Colored solar reflective system, characterized by the fact that it comprises: (1) a particulate material in the crystalline habit of rutile and with an average particle size between 0.6 μm and 1.7 μm, the particulate material selected from the group consisting of titanium dioxide, doped titanium dioxide and a mixture of these; and (2) an organic pigment with a maximum absorption coefficient of 5,000 mm-1 or more, in the visible light region, a maximum dispersion coefficient of 500 mm-1 or less, in the visible light region and an absorption coefficient medium of 50 mm-1 or less, in the infrared region, the organic pigment being one or more organic particles that are insoluble in the application medium in which they are dispersed and that give color.
    [0002]
    2. Colored solar reflective system, according to claim 1, characterized by the fact that the organic pigment has: (a) a maximum absorption coefficient of 10,000 mm-1 or more, preferably 15,000 mm-1 or more, in the visible light region; and / or (b) a maximum dispersion coefficient of 250 mm-1 or less, preferably 100 mm-1 or less, in the region of visible light; and / or (c) an average absorption coefficient of 30 mm-1 or less, preferably 10 mm-1 or less, in the infrared region.
    [0003]
    3. Colored solar reflective system, according to claim 1 or 2, characterized by the fact that the particulate material: (a) contains more than 70% by weight of titanium dioxide, based on the total weight of the particulate material; or (b) is doped titanium dioxide which is nickel titanate and antimony; or (c) is doped titanium dioxide which is chromium titanate and antimony; or (d) is titanium dioxide that has an average particle size between 0.7 μm and 1.4 μm.
    [0004]
    A colored solar reflective system according to any one of claims 1-3, characterized by the fact that the particulate material is coated titanium dioxide and / or coated doped titanium dioxide.
    [0005]
    5. Colored solar reflective system according to any one of claims 1-4, characterized by the fact that the organic pigment is selected from the group consisting of: azo pigments, anthraquinone, phthalocyanine, perinone / perylene, indigo / thioindigo, dioxazin , quinacridone, isoindolinone, isoindoline, diketopyrrolopyrole, azomethine and azomethine azos.
    [0006]
    6. Method for preparing a colored solar reflective system as defined in claim 1, characterized by the fact that it comprises mixing: a particulate material in the crystalline habit of rutile and with an average particle size between 0.6 μm and 1.7 μm, the particulate material selected from the group consisting of titanium dioxide, doped titanium dioxide and a mixture thereof; with an organic pigment with a maximum absorption coefficient of 5,000 mm-1 or more, in the visible light region, a maximum dispersion coefficient of 500 mm-1 or less, in the visible light region and an average absorption coefficient of 50 mm-1 or less, in the infrared region, the organic pigment being one or more organic particles that are insoluble in the application medium in which they are dispersed and that impart color.
    [0007]
    7. Colored composition, characterized by the fact that it comprises a colored solar reflective system as defined in any one of claims 1-5 and a vehicle, in which the particulate material and the organic pigment are dispersed in the vehicle.
    [0008]
    8. Colored composition, according to claim 7, characterized by the fact that: (i) the organic pigment is present in an amount of 0.1% by volume to 20% by volume, based on the total weight of the colored composition , and the particulate material is present in an amount of 0.5% by volume to 40% by volume, based on the total weight of the colored composition; (ii) the vehicle is a natural or synthetic resin comprising a polyolefin resin, poly (vinyl chloride) resin, ABS resin, polystyrene resin, methacrylic resin, polycarbonate resin, poly (ethylene terephthalate) resin, resin polyamide, alkyd resin, acrylic resin, polyurethane resin, polyester resin, melamine resin, fluoropolymer or epoxy resin, or a carrier or binder; (iii) the composition additionally comprises one or more thickeners, stabilizers, emulsifiers, texturizers, adhesion promoters, UV stabilizers, anti-luminosity agents, dispersants, antifoaming agents, wetting agents, coalescing agents, spacer particles or biocides / fungicides.
    [0009]
    9. Use of the colored composition as defined in claim 7 or 8, characterized by the fact that it is like a common ink, pen ink or coating or as a composition from which an article can be formed.
    [0010]
    10. Solar reflective colored coating of a layer, characterized by the fact that it comprises a colored solar reflective system as defined in any one of claims 1-5 and a vehicle, in which the particulate material and the organic pigment are dispersed in the vehicle.
    [0011]
    11. Solar reflective colored coating of a layer, according to claim 10, characterized by the fact that: (i) the coating covers a substrate that absorbs a proportion of radiation close to the infrared and in which the thickness of the layer is so such that more than 1% of the incident radiation near the infrared reaches the substrate; and / or (ii) the coating has an L * brightness value of 75 or less, preferably 65 or less, more preferably 55 or less, and even more preferably 45 or less; and / or (iii) the coating has a total solar reflectance greater than 30%, preferably greater than 35%, even more preferably greater than 40%, and even more preferably greater than 45%.
    [0012]
    12. Structure, characterized by the fact that it comprises: (i) the solar reflective colored coating of a layer as defined in claim 10 or 11; or (ii) one or more surfaces of the structure are coated with the colored solar reflective coating of a layer as defined in claim 10 or 11.
    [0013]
    13. Article comprising the colored composition as defined in claim 7 or 8, characterized by the fact that the article has an L * brightness value of 75 or less.
    [0014]
    14. Article according to claim 13, characterized in that: (a) the article has an L * luminance value of 65 or less, preferably 55 or less, and more preferably 45 or less; and / or (b) the article has a total solar reflectance greater than 30%, preferably greater than 35%, more preferably greater than 40%, and even more preferably greater than 45%.
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    CA2787741C|2018-01-02|Titanium dioxide
    同族专利:
    公开号 | 公开日
    GB201002700D0|2010-04-07|
    AU2011217003B2|2015-04-16|
    PL2536792T3|2017-01-31|
    EP2536792B1|2016-08-24|
    CN102762670A|2012-10-31|
    AU2011217003A1|2012-08-02|
    MX2012009408A|2012-09-12|
    EP2536792A1|2012-12-26|
    CA2787625A1|2011-08-25|
    GB2477930A|2011-08-24|
    SI2536792T1|2016-10-28|
    WO2011101657A1|2011-08-25|
    KR20130008552A|2013-01-22|
    CA2787625C|2019-03-26|
    JP2013519780A|2013-05-30|
    CN102762670B|2015-11-25|
    UA107372C2|2014-12-25|
    KR101867266B1|2018-07-23|
    MY159933A|2017-02-15|
    US20130048925A1|2013-02-28|
    ES2600002T3|2017-02-06|
    SG183245A1|2012-09-27|
    BR112012020387A2|2016-05-10|
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    法律状态:
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2019-02-19| B06T| Formal requirements before examination|
    2019-11-12| B07A| Technical examination (opinion): publication of technical examination (opinion)|
    2020-08-11| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|
    2020-12-08| B09A| Decision: intention to grant|
    2021-01-19| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 11/02/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
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    GB1002700A|GB2477930A|2010-02-17|2010-02-17|Solar reflective system|
    GB1002700.1|2010-02-17|
    PCT/GB2011/050267|WO2011101657A1|2010-02-17|2011-02-11|Titanium dioxide|
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