MXPA98007249A - Compositions of mix pigment - Google Patents

Abstract

Disclosed is a blending pigment composition for coloring high molecular weight materials, particularly coatings or ink systems, comprising from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive comprising a polymer or vinylpyrrolidone copolymer. The mixing pigment composition is in the form of microgranules and can be obtained by spray drying a pigment dispersion and the additive. The new powders of the pigment composition are easily handled, easily moistened and rapidly dispersed to form homogeneous aqueous pigment dispersions, which are particularly free of larger pigment aggregates and can be easily incorporated into aqueous ink and paint systems such as pigments. mixed without a dispersion step in a bowl mill

Description

COMPOSITIONS OF MIXING PIGMENT DESCRIPTION OF THE INVENTION The present invention relates to mixing pigment compositions in the form of microgranules, comprising from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive comprising a polymer or copolymer of vinylpyrrolidone, provided that the copolymer is not a copolymer of an ethylenically unsaturated sulfonic acid and N-vinyl-pyrrolidone. Organic mixing pigments are known and are described, for example, in the patent of E.U.A. No. 5,554,217. These mixing pigments and mixing pigment compositions show excellent mixing properties when applied to paint and ink systems, particularly solvent-based systems. They have the great advantage that they can be incorporated into a paint or ink system by simply ring the pigment powder in the paint system without the time consuming and energy consuming step in a ball mill. It is also known to use certain pigment preparations, also called master batches, which have a pigment concentration of 30 to 60% by weight based on the preparation, as mixing pigments. Such mixing preparations show excellent properties in certain applications. However, they have the disadvantage of using an expensive preparation process, and occasionally show incompatibility in some application means due to the high amount of carrier additives. Many patents describe processes for pigment surface modifications to improve certain pigment properties, such as color strength or rheological properties, for example, through the addition of pigment derivatives such as pigment sulphonic acids, sulfonamide or other derivatives of pigment. pigment. However, said treated pigments need to be dispersed for many hours in a ball mill in order to incorporate the pigment into a paint vehicle. The patent of E. U.A. No. 3, 806,464 describes the encapsulation of pigments with an acrylic interpolymer, and the Japanese published patent application SHO 57-49664A describes a process for the preparation of pigment compositions containing thermopla resins, which can be dissolved in water with a basic substance. Although these pigments contain polar polymers, they are different from the pigment compositions herein, since they contain different types of additives. In addition, they show incompatibility in certain means of application. Therefore, its use as pigment compositions has not been widely disseminated. Other patents, such as the patents of E. U.A. No. 5,274,010 and 5,401, 780, describe a process for the free enveloping pigmentation of polyolefins by coating the surface of the pigment with a polyvinyl alcohol or other polar polymers such as acrylic polymers, cellulose derivatives, copolymers of maleic anhydride-styrene and polyvinylpyrrolidone, alone or in combination with silane films or zirconium acetylacetonate. The coating of the pigment is achieved (A) through the absorption of a soluble polymer, preformed onto the pigment, or (B) through the polymerization of a corresponding monomer in the presence of the pigment. In any case, the resulting coated pigment is recovered through filtration from an aqueous suspension. Said suspensions are difficult to filter and can show a strong penetration of finely divided pigment particles. Therefore, filter aids are usually added to improve filtration rates. However, the presence of these filter aids in the pigment composition can lead to the incompatibility of the resulting coated pigments when applied to substrates other than polyolefins. In addition, said pigment suspensions contain a large amount of non-absorbed polymer, which dissolves in the aqueous medium and thus in the filtrate after filtration. This highly colored filtrate then requires special treatment in order to recover or degrade the soluble polymer and reduce the color of the filtrate to environmentally acceptable levels. The patent of E. U.A. No. 5, 145, 524 discloses surface modification of pigments through treatment with polyvinyl ethers to obtain pigments with improved properties for automotive finishing systems. This surface treatment also improves the pigment flow properties in aqueous systems, leading to aqueous pigment dispersions with a higher solids content for direct application in waterborne paint systems. Said pigment dispersions may have the disadvantage of foaming and sedimentation. In addition, they require the addition of antifouling agents. In addition, in most cases, they continue to need to be dispersed in a ball mill for optimum dispersion. The patent of E. U.A. No. 3,904,562 describes a process for encapsulating finely divided organic pigment particles with a polymeric outer layer through a precipitation process. This process is very expensive and environmentally unfavorable due to the use of a large amount of an inorganic salt to induce precipitation of the polymer from the aqueous medium. In addition, the encapsulated particles according to the teachings of this patent require a higher molecular weight polyvinylpyrrolidone and a larger amount of pigment based polymer to ensure complete encapsulation, which adversely affects the compatibility of the pigment when it is applied. in several different substrates. Japanese Patent Application SHO 58-2035351 discloses pigment compositions comprising a pigment and a water-soluble copolymer of an ethylenically unsaturated sulfonic acid compound and a N-vinylpyrrolidone compound. Said pigment compositions can be incorporated into aqueous vehicles through simple mechanical agitation are a dispersion step. However, due to the presence of the polymeric sulfonic acids, these pigment compositions may not be suitable for many applications, for example, the application in automotive paint systems, since it is well known that strongly polar polysulphonic acids have an effect harmful in the healing of the coating system. In addition, the presence of polysulfonic acids can improve water absorption, which can further damage the weather resistance of the pigmented coating system. Due to environmental issues and new environmental regulations, the paint industry is moving widely from solvent taken to aqueous coating systems. The newly developed, improved aqueous polymer binder systems are helping to accelerate this transformation, but they also force pigment manufacturers to continually modify their pigments to adapt the properties of the pigment to the customer's final needs. The present invention relates to novel blending pigment compositions in the form of microgranules comprising from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive, which comprises a polymer or copolymer of vinylpyrrolidone . These novel microgranule mixing pigment compositions can be obtained by spray drying an aqueous pigment dispersion having a high solids content containing the pigment and the additive. These exhibit improved pigment properties when applied to aqueous ink and paint systems, particularly those used in industrial coatings, retail sales and the automotive industry. Unexpectedly, it has been discovered that said mixing pigment compositions can be smoothly incorporated into aqueous ink and paint systems, such as a mixing pigment without performing a dispersion step in a ball mill. Compared with conventionally dried and micropulverized pigments, the new pigment compositions are generally less dusty and can be more easily handled. They are also easily moistened and rapidly dispersed to form homogeneous aqueous pigment dispersions, which are virtually free of larger pigment aggregates. It is known that many pigments of small particle size are added during the drying process. However, with pigments exhibiting this tendency to aggregation, surprisingly, the microgranulated mixing pigment compositions of the invention are readily dispersible in aqueous paint systems. In addition, said mixing pigment compositions have the great advantage that they are compatible with a variety of aqueous paint and ink systems, including the automotive paint systems in greatest demand. Additionally, the new blending pigment compositions can be obtained by a very simple, economical and environmentally acceptable method in conventional equipment. This invention relates to mixing pigment compositions, which are in the form of microgranules and comprise from 85 to 99.5 parts, preferably from 90 to 99 parts and most preferably from 94 to 99 parts by weight of a pigment and from 0.5 to 15 parts, preferably 1 to 10 parts and most preferably 1 to 6 parts by weight of an additive comprising a vinylpyrrolidone polymer or copolymer, provided that the copolymer is not a copolymer of an ethylenically unsaturated sulfonic acid and N- vinylpyrrolidone. These new microgranulated mixing pigment compositions can preferably be obtained by spray drying an aqueous pigment dispersion, comprising from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive comprising a polymer or copolymer of vinylpyrrolidone. , provided that the copolymer is not a copolymer of an ethylenically unsaturated sulfonic acid and N-vinylpyrrolidone. Particularly preferred is a spray drying of an aqueous pigment dispersion with a high solids content. They are useful for coloring high molecular weight materials. A wide variety of vinylpyrrolidone homo- or copolymers are suitable as additives for preparing the pigment blending compositions of the invention. In general, the vinylpyrrolidone homopolymer is a polyvinylpyrrolidone obtained through the polymerization of 1-vinyl-2-pyrrolidone (also known as vinylpyrrolidone, N-vinylpyrrolidone and NVP) by methods known per se. Such polymers are well known and many are commercially acceptable. Preferably, the weight average molecular weight of the polyvinylpyrrolidone is more than 300,000 g / mole; very preferably it is between 5,000 to 200,000 g / moles.

Suitable vinylpyrrolidone copolymers are, for example, copolymers of vinylpyrrolidone with vinyl ether, vinyl alcohol; acrylic or methacrylic acid or an ester or amide thereof, and particularly with vinyl acetate. Especially suitable with water-soluble copolymers such as water-soluble polyvinylpyrrolidone / viniol acetate copolymers having a ratio of vinylpyrrolidone to vinyl acetate of 70 to 30 to 60 to 40. Depending on the pigment employed in the pigment composition of It is advantageous to use the additive of vinylpyrrolidone homopolymer or copolymer in admixture with the other polymers, copolymers and / or polymer derivatives preferably soluble in water. Therefore, another preferred embodiment of the present invention relates to the pigment composition of the invention, wherein the additive comprises a mixture of vinylpyrrolidone or the copolymer of vinylpyrrolidone with one or more other water-soluble anionic or cationic polymers, neutral, copolymers and / or polymer derivatives, and wherein the total amount of the additive mixture is less than 20 parts by weight of the pigment composition. Such polymers are, for example, polyacrylic acid, polymethacrylic acid, polymaleic anhydride, polyurethane, polyvinyl ether, polyvinyl alcohol, polyalkylene glycol, polyethylene oxide, cellulose derivatives, poly-imine, polyvinyl pyridine or copolymers thereof, or copolymers such as copolymers of acrylic acid with styrene, acrylonitrile, vinyl acetate, vinyl phosphonate, vinyl propionate, vinyl chloride, itaconic acid or maleic anhydride, or a mixture thereof. Suitable polymer derivatives are, for example, ethoxylated or propoxylated fatty amines such as ethoxylated cocoalkyl, oleyl or soy-alkyl amines; ethoxylated or propoxylated fatty quaternary salts such as ethoxylated cocoalkyltrimethyl ammonium chloride; ethoxylated fatty amides such as ethoxylated oleamides; alkyl-, cycloalkyl-, or alkylated l-oxy poly (ethyleneoxy) ethanol, cycloalkyloxypoly (ethyleneoxy) laurate or oleate, polyethylene glycol laurate or oleate 400, alkyl-, cycloalkyl- or alkylaryl-poly (ethyleneoxy) carboxylate or phosphonate. An especially preferred cycloalkyloxy poly (ethyleneoxy) laurate or oleate is, for example, a poly (ethyleneoxy) sorbitan laurate or oleate. These other polymers, copolymers and / or polymer derivatives preferably soluble in water are known per se and are commercially available. The total amount of the homopolymer or copolymer of vinylpyrrolidone and other polymer, copolymers and / or polymer derivatives preferably soluble in water in the pigment compositions of the invention is preferably not more than 20 parts by weight, most preferably 5 to 15 parts by weight. Preferably, said mixture comprises at least 20%, most preferably from 20 to 80% by weight of the vinylpyrrolidone polymer or vinyl pyrrolidone copolymer. If the other polymer, copolymer and / or polymer derivative is an anionic or cationic polymer, the polymer additive mixture is preferably dissolved as salts in an aqueous medium, preferably a basic aqueous or acid medium. Another preferred embodiment refers to the pigment composition of the invention, wherein said cationic polymer is polyvinylpyridine or poly-imine. Advantageously an anionic polymer or copolymer polymer or derivative is dissolved in water as an alkylammonium, sodium, potassium or ammonium salt. A preferred additional embodiment refers to the pigment composition of the invention, wherein said pigment is an organic or inorganic pigment or a mixture thereof. Pigments especially suitable for the pigment blending compositions herein are organic pigments selected from the group consisting of azo, azomethine, methine, anthraquinone, phthalocyanine, perinone, perylene, diketopyrrolopyrrole, thioindigo, iminoidoindoline, dioxazine, iminoisoindolinone, quinacridone pigments, flavantrone, idantrone, anthrapyrimidine and quinophthalone, or a mixture or solid solution thereof; especially an azo pigment, dioxazine, diketopyrrolopyrrole, quinacridone, phthalocyanine, indatrone or iminoisoindolinone, or a mixture or a solid solution thereof. Notable pigments useful in the pigment blending compositions herein are those pigments described in Color Index, including the group consisting of Pigment Red C.l. 202, Pigment Red C.l. 122, Pigment Red C.l. 179, Pigment Red C.l. 170, Pigment Red C.l. 144, Pigment Red C.l. 177, Pigment Red C.l. 254, Pigment Red C.l. 255, Pigment Red C.l. 264, Pigmento Café C.l. 23, Pigment Yellow C.l. 109, Pigment Yellow C.l. 110, Pigment Yellow C.l. 147, Pigment Yellow C.l. 191.1, Pigment Yellow C.l.74, Pigment Yellow C.l. 83, Pigment Yellow C.l. 13, Pigment Orange C.l. 61, Pigment Orange C.l.71, Pigment Orange C.l. 73, Pigmento Naranja C.l. 48, Pigment Orange C.l. 49, Pigment Blue C.l. 15, Pigment Blue C.l. 60, Pigment Violet C.l. 23, Pigmento Violeta C.l. 37, Pigment Violet C.l. 19, Pigment Green C.l.7, Pigment Green C.l. 36, or a mixture or solid solution thereof. Suitable inorganic pigments in the mixed pigment compositions herein are selected from the group consisting of carbon black, metal oxides, mixed metal oxides, antimony yellow, lead chromate, lead chromate-sulfate, molybdate lead, ultramarine blue, cobalt blue, manganese blue, chromium oxide green, hydrated chromium oxide green, cobalt green, metal sulfides, cadmium sulfoselenides, zinc ferrite and bismuth vanadate, and mixtures thereof. Generally, the pigment according to this invention has an average particle size in the range of 0.001 to 30 μm, preferably in the range of 0.005 to 5 μm. Based on these average particle size scales, it is evident that the pigment is preferably used in the form of a crude pigment or a conditioned pigment. Preferably, the pigment is used in its aqueous compressed cake form as obtained, for example, through the isolation of the pigment after synthesis or conditioning. In addition, the pigment may contain customary additives, such as inorganic fillers, light stabilizers and / or anti-flocculating agents. Therefore, another preferred embodiment of the present invention relates to the pigment composition of the invention, wherein said pigment is a mixture of an organic pigment and an inorganic filler. The term "inorganic filler" means a substantially transparent inorganic pigment. For example, mica, kaolin, talc, wollastonite and natural or synthetic silica, for example, glass, are known inorganic fillers that are suitable for use in the pigment compositions of the present invention.

Talc, Muscovite mica, and kaolin, or mixtures thereof, are highly suitable inorganic fillers. Transparent micas are especially suitable for use as an inorganic filler. Of the micas, the most suitable are muscovite, phlogopite, brolite and synthetic micas. The inorganic filler is preferably used in its natural form, but transparent or semi-transparent inorganic filler pigments can also be employed, for example, a mica treated with a metal oxide, or talc treated with an organic aliphatic compound, such as acid aliphatic long chain. In general, the inorganic filler consists of primary filler particles having any geometric shape, but a flake form is preferred. Preferably, the inorganic filler has an average particle size on the scale of 0.5 to 10 μm and a maximum particle size below 20 μm. Typically, the inorganic filler is used in a concentration of 1 to 30% based on the weight of the pigment. Thus, another preferred embodiment refers to the pigment composition of the invention, wherein said pigment is a mixture of 70 to 99 parts by weight of an organic pigment and 1 to 30 parts by weight of an inorganic filler. Light stabilizers, such as U.V. absorbers, are known in the art. and hindered amine light stabilizers. These can be used in any suitable effective amount in the pigment compositions herein provided they do not damage the properties of the mixing pigment of the composition. Antiflocculating agents, also described as rheology enhancing agents or particle growth inhibitors, are well known in the pigment industry and are suitable as additives for the pigment compositions herein. Generally, anti-flocculating agents are, for example, pigment derivatives such as sulfonic acid, sulfonic acid salts or sulfonamide derivatives of organic pigments. Typically, rheology enhancing agents are used at a concentration of 0.5 to 8% based on the weight of the organic pigment. The inorganic filler, the light stabilizer and / or the anti-flocculating agent is incorporated into the composition before, during or after the spray drying step. Preferably, these customary additives are added before the spray drying step. Depending on the customary additive, it is preferably added at the end of the synthesis or conditioning step, before the pigment is isolated, or is added to a compressed aqueous pigment cake dispersion with a high solids content of additional slurry. The pigment compositions of the invention can be prepared preferably through a process, in which it comprises: (A) preparing an aqueous solution of the additive; (B) forming a slurry of a pigment in the solution to obtain a homogeneous liquid dispersion comprising from 85 to 99.5 parts by weight of the pigment and from 0.5 to 15 parts by weight of the additive, (C) by spray drying the resulting liquid dispersion , and (D) collecting the dried microgranules of the pigment composition. A preferred embodiment thereof relates to the process of the invention, wherein an aqueous compressed pigment cake is formed as a slurry in the solution. In a preferred method, a highly concentrated compressed pigment cake is formed in a slurry in any suitable device, at temperatures between 5 and 90 ° C, preferably 20 to 60 ° C, such as, for example, a Cowles disperser. ®, in the presence of the aqueous additive solution, as illustrated in the examples below, to obtain a homogeneous aqueous dispersion. The suitable conditions for the spray drying of the homogeneous aqueous dispersions can then be easily determined by a person skilled in the art. Due to the pronounced pronounced fluidization effect of the additives employed in accordance with this invention, low viscosity aqueous pigment dispersions with a solids content above 20% can be easily generated or, depending on the pigment and the polymer additive or the additive mixture, solids content of 25% and above this. Despite the high concentration of pigment, these pigment dispersions have the advantage that they are liquid, easily flowable and ideally suited for spray drying. Spray drying is a drying technology well known in the chemical industry. Any equipment that is conventional for spray drying can be used to spray-dry the pigment compositions of the invention. A suitable commercially available equipment includes the BOWEN BLS spray dryer from Bowen or N I RO ATOMIZER from N I RO Company. Due to their high solids content, the pigment dispersions of the invention are dried quickly and economically through spray drying, producing single pigment composition powders composed of microgranules. The additive according to this invention are homogeneously distributed in the mixing pigment compositions and also serve as the binder for the microgranules. Typically, the microgranules have a size on the scale of 1 to 1000 μm, preferably 3 to 300 μm when suspended in a solvent immiscible with water, such as xylene and observed under a light microscope. These can have any form. The shape and size of the microgranules are influenced by various parameters such as the type and size of the pigment particle, the type and concentration of the additive or mixture of additives, respectively, as well as the spray drying conditions and the equipment of the spray dryer. Due to the large particle size of the microgranules, they are generally less dusty and can be handled more easily than conventionally dried and micropulverized pigments. The pigment compositions of the invention are easily moistened in aqueous ink or paint systems. Surprisingly, they are rapidly dispersed by simply stirring the pigment in an aqueous ink or paint system without a dispersion step in a ball mill or other high shear inducing equipment. In this way, the pigment compositions of the invention are ideal for use as pigments in mixing in aqueous systems, where they eliminate the time consuming and energy consuming step of ball milling, as well as the expense of cleaning the ball mills. In general, an effective amount of pigmentation of the mixing pigment composition is incorporated into the high molecular weight organic material that will be pigmented. An effective amount of pigmentation is any amount suitable to provide the desired color in the high molecular weight organic material. In particular, the mixing pigments are used in an amount of 0.01 to 30% by weight, preferably 0.1 to 10% by weight, based on the weight of the high molecular weight organic material that will be pigmented. Organic, pigmented, high molecular weight materials, which are colored according to the process herein are useful in a variety of applications. For example, high molecular weight organic material can be used for pigmentation, lacquers, inks and enamel coating compositions. The high molecular weight pigmented organic materials prepared in accordance with the present invention are particularly useful for preparing automotive coating paints. The high molecular weight organic materials, which are colored according to the process herein, are preferably if the high molecular weight organic material is a coating or an ink system, for example, cellulose ethers, cellulose esters , polyurethanes, polyesters, polycarbonates, polyolefins, polystyrene, polysulfones, polyamides, polycycloamides, poly-imides, polyethers, polyether ketones, polyvinyl halides, polytetrafluoroethylene, acrylic and methacrylic polymers, rubber, silicone polymers, phenol / formaldehyde resins, melamine, resins formaldehyde, urea / formaldehyde resins, epoxy resins and diene rubbers or their copolymers. High molecular weight organic materials, which are useful for heat curable or interlaced coatings, for example, chemically reactive coatings, are also colored according to the process herein. The pigmented, high molecular weight organic materials prepared according to the present process are especially useful in stove finishes, which contain customary binders and which are reactive at high temperature. Examples of high molecular weight organic materials, which are used in such coatings, include acrylic, alkyd, epoxy, phenolic, melamine, urea, polyester, polyurethane, blocked isocyanate, benzoguanamine or cellulose ester resins, or combinations thereof . The high molecular weight, pigmented organic materials prepared according to the present process are also useful in air drying or physical drying coatings. The pigment blending compositions herein are particularly suitable for preparing pigmented coatings of the types conventionally employed in industrial paints, particularly in the automotive industry, especially acrylic / melamine aqueous resins, alkyd / melamine resin, thermoplastic acrylic resin or resin systems of polyurethane. Due to the excellent dispersibility of the mixing pigment compositions of this invention, a uniform distribution of pigment particles throughout the application means is easily obtained. The compositions containing the mixing pigments of the present show an excellent rheological behavior. The mixed pigment compositions herein are used alone or in the presence of other pigments or dyes. It is especially useful to color a high molecular weight organic material with the mixed pigment compositions herein together with an effect pigment. The effect of color and shade is varied by varying the type of the effect pigment and the concentrations of the effect pigment and the pigment composition of the present invention. Shade effect shadows are particularly generated using the mixing pigments with mica pigments or aluminum pigments coated with known transparent titanium dioxide. Due to their unique pigment properties, the new blending pigment compositions are also suitable for coloring high molecular weight organic materials, which are plastics that are calendered, cast, molded or processed into fibers and the like. The pigment compositions impart excellent physical properties to colored plastic articles, such as polypropylene or polyamide fibers, plastic films, bottle cases, etc. Thus, the present invention also encompasses processes wherein the high molecular weight organic compound is a plastic that is calendered, cast, molded or processed into fibers and plastic articles that are calendered, cast, molded or processed into fibers. Mixing pigment compositions are readily dispersible when incorporated into high performance plastics, such as, for example, polyethylene, polypropylene, ABS or polylamide. Surprisingly, the resulting colored molded products show virtually no flow line, proving that the pigment compositions are very homogeneously distributed in the polymer. As one skilled in the art will appreciate, the presence of flow lines is not desirable.

The pigment compositions of the invention are also suitable for the preparation of liquid colors, since they can provide liquid colors with a high solids content in the pigment. Liquid colors are well known in the pigment industry and are mainly used to color plastic materials. In addition, the pigment compositions of the invention are suitable for use in inkjet formulations. The following examples illustrate various embodiments of the invention, but the scope of the invention is not limited thereto. In the examples, all parts are by weight unless otherwise indicated.

EXAMPLES EXAMPLE 1 A stainless steel vessel of 151 .36 liters was loaded with 18. 2 kg of an aqueous compressed cake containing 7.7 kg dry weight of a pigment of 3,6-di (4-chlorophenyl) -1,4-diketopyrrolopyrrole (Pigment Red 254 C. I.), I RGAZINFDPP Red BO, from CIBA Specialty Chemicals Corp., Newport (DE). In a separate container, 600 grams of a 50% aqueous solution of polyvinyl acetate / vinylpyrrolidone (LUVISKOL VA 73W from BASF) and 173.7 grams of a poly (ethyleneoxy) sorbitan laurate were dissolved in a separate container in 5 liters of water. WITCONOL 2720 from Witco Corp.). Then, 1550 grams of ULTRA Tale 609 from Barretts Minerals Inc. was added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed diketopyrrolopyrrole pigment cake. The mixture was stirred with a Cowles® dissolver, generating an easily flowable liquid red pigment dispersion with a solids content of 37.8%. The highly concentrated pigment dispersion was spray-dried in a pilot plant spray dryer (BOWEN BLS from Bowen) with 2,812 kg / cm2 of heated air at an inlet temperature of 400 ± 5 ° C (outlet temperature of 125 ± 3 ° C), yielding 9.5 kg of the red or mixed color pigment composition, which could be easily incorporated into an aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce coatings of Strong opaque red color with excellent durability.

EXAMPLE 2 A stainless steel vessel of 151.36 liters was loaded with 19. 5 kg of an aqueous compressed cake containing 8.2 kg dry weight of a pigment of 3,6-di (4-chlorophenyl) -1,4-diketopyrrolopyrrole IRGAZI N DPP Red BO, from CI BA Specialty Chemicals Corp. In a container by Separated, 683 grams of an aqueous solution of polyvinylpyrrolidone (LUVISKOL K30 from BASF Corp.) were dissolved in 5 liters of water. Then, 2050 grams of U LTRA Tale 609 from Barretts Minerals Inc. was added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed diketopyrrolopyrrole pigment cake. The mixture was stirred with a Cowles® dissolver, generating an easily flowable liquid red pigment dispersion with a solids content of about 38%. The highly concentrated pigment dispersion was spray-dried in a pilot plant spray dryer (BOWEN BLS from Bowen) producing 10.2 kg of the red or mixed color pigment composition, which could be easily incorporated into an aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce strong opaque red coatings of excellent durability.

EXAMPLE 3 A 4-liter WARING mixer from the Cole-Parmer Instrument Company was charged with 2286 grams of an aqueous compressed cake containing 802 grams by dry weight of the isoindolinone pigment IRGAZI N YELLOW 3 RLTN (Pigment Yellow C. l 1 10 of CIBA Specialty Chemicals Corp., Newport DE). In a 1-liter beaker, 59.6 grams of an aqueous solution of polyvinylpyrrolidone (LUVISKOL K30 from BASF Corp.) was dissolved in 200 ml of water. After, 80.2 grams of ULTRA Tale 609 from Barretts Minerals Inc., were added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed yellow isoindolinone pigment cake in the WARI NG mixer. The mixture was combined medium to high speed generating an easily flowable liquid yellow pigment dispersion. Two batches of the above aqueous yellow pigment dispersion were combined, followed by spray drying in a pilot plant spray dryer (BOWEN BLS from Bowen) yielding 1.78 kg of the yellow pigment mixing composition. , which was easily incorporated into an aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce opaque yellow coatings of excellent durability. When dispersed in xylene and observed under a light microscope, the spherical microgranules with a size of 20 to 100 μm, could be observed together with many smaller granules having a size of 5 to 15 μm.

EXAMPLE 4 A 4 liter WARING mixer was charged with 1692 grams of an aqueous compressed cake containing 687 grams by dry weight of the magenta 2,9-dichloroquinacridone pigment (MONASTRAL® Magenta B from CI BA Specialty Chemicals Corp., Newport DE). In a one-liter beaker, 83.8 grams of an aqueous solution of polyvinylpyrrolidone (LUVISKOL K30 from BASF Corp.) were dissolved in 250 ml of water. Then, 125.6 grams of ULTRA Tale 609 from Barretts Minerals Inc., were added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed magenta pigment cake in the WARING mixer. The mixture was combined at a medium to high speed generating a paste dispersion. Then 62.7 g of LUVISKOL K-30 was added together with 750 ml of water, producing in one more mixture a compressed fluid cake. Two batches of the aqueous magenta pigment dispersion were combined, followed by spray drying in a pilot plant spray dryer (Bowen's BOWEN BLS) producing a magenta-colored mixing pigment composition, which was easily incorporated into a aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce magenta coatings of excellent durability.

EXAMPLE 5 A 4 liter WARI NG mixer was charged with 3093 grams of an aqueous compressed cake containing 866 grams by dry weight of the quinacridone pigment Violet Pigment C. l. 19 (MONASTRAL®Red and RT from C IBA Specialty Chemicals Corp., Newport DE). In a one-liter beaker, 86.7 grams of an aqueous solution of polyvisilpyrrolidone LUVISKOL K30 from BASF Corp. was dissolved in 350 ml of water. Then, 86.6 grams of ULTRA Tale 609 from Barretts Minerals Inc. was added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed quinacridone pigment cake in the WARING mixer. The mixture was combined at a medium to high speed generating a dispersion of fluid pigment. The pigment dispersion was spray-dried in a pilot plant spray dryer (BOWEN BLS from Bowen) producing a red pigment mixing composition, which was easily incorporated into an aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce red coatings of excellent durability.

EXAMPLE 6 A 4 liter WARING mixer was charged with 2206 grams of an aqueous compressed cake containing 953 grams by dry weight of azo pigment Yellow Pigment C. l. 191 .1 (CROMOPHTAL®Yellow H RP from CIBA Specialty Chemicals Corp., Newport DE). In a one-liter beaker, 63.5 grams of an aqueous solution of polyvinyl pyrrolidone LUVISKOL K30 from BASF Corp. were dissolved in 400 ml of water. Then 95.3 grams of U LTRA Tale 609 from Barretts Minerals Inc. were added to the aqueous resin solution and stirred until completely wetted. The talc / aqueous resin mixture was added to the compressed yellow azo pigment cake in the WARING mixer. The mixture was combined at a medium to high speed generating a dispersion of pasty pigment. An additional 11 grams of LUVISKOL K30 was diluted with 400 ml of water and added to the pigment paste. The mixture was further combined in a medium at high speed resulting in a yellow pigment dispersion of fluid. Two batches of the above aqueous yellow pigment dispersion were combined and spray-dried in a pilot plant spray dryer (BOWEN BLS from Bowen) producing a yellow pigment mixing composition, which was easily incorporated into the an aqueous paint system without a dispersion step in a ball mill as a mixing pigment to produce yellow coatings of excellent durability. When dispersed in xylene and observed under a light microscope, the spherical microgranules with a size of 20 to 100 μm, could be observed together with many smaller granules having a size of 5 to 15 μm.

EXAMPLE 7 The procedure of Example 6 was repeated; however, using as organic pigment a pigment mixture of 1 103 grams of the aqueous compressed cake containing 476 grams of Pigment Yellow C. l. 191 .1 and 1600 grams of the compressed aqueous cake containing the clear diketopyrrolopyrrole pigment, Pigmento Rojo C. l. 254, both from CI BA Specialty Chemicals Corp., providing a mixture of scarlet pigment, which could be applied in ink, aqueous paint and coatings for sale producing finishes with a strong scarlet color with excellent durability.

EXAMPLE 8 This example demonstrates the incorporation of a pigment-mixing composition containing the pigment 3,6-di (4-chlorophenyl) -1,4-diketopyrrolopyrrole (Pigment Red C. 1.254) in an automotive aqueous paint system, they are a Dispersion step, directly as a mixing pigment.

"Mixing Pigment Dispersion" A 226.8 gram container was loaded with 38.8 grams of a polymeric aqueous dispersant and 121.2 grams of deionized water. The mixture was stirred for 5 to 10 minutes. Then, 40 grams of the pigment composition, prepared according to Example 1, were added to the aqueous resin dispersion by stirring at medium speed to produce a pigment dispersion. The red pigment dispersion was stirred at medium to high speed with a propeller stirrer for 15 minutes, producing a homogeneous "mixing pigment dispersion", containing 20.0% of the pigment composition with a total solids content of 30% and having a pigment / binder ratio of 2: 1.

"Paint Dispersion" The following was mixed: 25.0 grams of the "mixed pigment dispersion", 8.2 grams of light-colored clearing resin solution and 66.0 grams of balanced light-colored resin solution. The viscosity of the resulting paint dispersion was adjusted from 1500 to 2000 cps with deionized water and through the addition of sufficient 2-amino-2-methyl-1-propanol to obtain a pH of about 7.6, and then sprayed on a panel twice at 1 .5 minute intervals as base coat. After 2 minutes, a clear solvent-based coating was sprayed twice at 1.5 minute intervals on the base coat. The sprayed panel was then vaporized with air in a vaporization cabinet for 10 minutes and then "baked" in an oven at 130 ° C for 30 minutes, producing a high-chroma red honeycomb with excellent weather resistance. A microscopic evaluation showed a homogeneous distribution of the pigment particles in the coating system.

EXAMPLE 9 This example demonstrates the incorporation of a mixing pigment composition containing the isoindolinone pigment (Pigment Yellow C. l.10) in an aqueous automotive paint system, without a dispersion step, directly as a mixing pigment.

"Mixing Pigment Dispersion" A 226.8 gram container was loaded with 38.8 grams of a polymeric aqueous dispersant and 121.2 grams of deionized water. The mixture was stirred for 5 to 10 minutes. Then, 40 grams of the pigment composition, prepared according to Example 3, were added to the aqueous resin dispersion by stirring at medium speed to produce a pigment dispersion. The yellow pigment dispersion was stirred at a medium to throttle speed with a propeller agitator for 15 minutes, producing a homogeneous "mixing pigment dispersion", containing 20.0% of the pigment composition with a total solids content of 30% and having a pigment / binder ratio of 2: 1.

"Paint Dispersion" The following was mixed: 25.0 grams of the "mixed pigment dispersion", 8.2 grams of light-colored clearing resin solution and 66.0 grams of balanced light-colored resin solution. The resulting yellow paint dispersion was sprayed onto a panel according to the procedure described in Example 8, producing highly saturated yellow coated panels, which exhibited excellent weather resistance. A microscopic evaluation showed a homogeneous appearance of the coating.

EXAMPLE 10 This example demonstrates the incorporation of a mixing pigment composition containing the azo pigment, Pigment Yellow C. l. 191 .1 in H DPE. Five grams of the pigment composition prepared according to Example 6, 2.5 grams of hindered amine light stabilizer, 1.0 grams of the benzotriazole UV absorber, 1.0 grams of hindered phenol antioxidant and 1.0 grams of the stabilizer of phosphate process, all of Additives Divison of CI BA Specialty Chemicals Corporation, were mixed together with 1000 grams of high density polyethylene (HDPE) from US I. QUANTUM Chemicals at a speed of 175-200 rpm for 30 seconds after reflux. The reflux pigment resin crumbled while hot and malleable, and then fed to a granulator. The resulting granules were molded in a molder by injection with 5 minutes of drying time and a cycle time of 30 seconds at temperatures of 204 and 260 ° C. Wafers of homogeneous color were obtained, which showed a bright yellow color with shades of color similar to each of the temperatures and with excellent stability to light. The yellow molded wafers showed no flow lines when placed in front of a light source and were observed. Similar results were obtained starting from 12.5 grams of a liquid color suspension comprising the liquid carrier and the pigment composition obtained according to Example 6 at a concentration of 40%. The liquid color suspension was prepared by simply stirring the pigment composition in the liquid vehicle without a dispersing step in a high shear mixer.

EXAMPLE 11 This example demonstrates the incorporation of a blending pigment composition into a universally sold paint system. A glass beaker was charged with 63.5 grams of polyethylene glycol, 37.8 grams of deionized water, 10.8 grams of Alcolec S from American Lecithin Company, Danbury CT and 23 grams of IGEPAL CO-530 from GAF Chemicals, Wayne NJ. The mixture was stirred for 10 minutes and the pH was adjusted to 8.0-8.5 with diluted ammonia. Then, 15 grams of the scarlet mixing pigment composition prepared according to Example 7 was added. The resulting suspension was further stirred at a medium to high speed with a stirrer for 20 minutes, resulting in a pigment dispersion. homogeneous, which could be easily incorporated into dispersions of aqueous latex producing very strong scarlet paints with excellent durability.

Claims (2)

1 - . 1 - A composition of pigment for mixing in the form of microgranules, which comprises from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive comprising a polymer or copolymer of vinylpyrrolidone, provided that the The copolymer is not a copolymer of an ethylenically unsaturated sulfonic acid and N-vinyl pyrrolidone.

2 - A pigment composition, which can be obtained by spray drying an aqueous pigment dispersion, which comprises from 85 to 99.5 parts by weight of a pigment and from 0.5 to 15 parts by weight of an additive comprising a polymer or vinylpyrrolidone copolymer. 3. A pigment composition according to claim 1 or 2, wherein the additive comprises a mixture of the vinylpyrrolidone or copolymer of vinylpyrrolidone with one or more other polymer, copolymers and / or neutral, anionic or cationic polymer derivatives. , and wherein the total amount of the additive mixture is less than 20 parts by weight of the pigment composition. 4. A pigment composition according to claims 1 to 3, wherein said pigment is a mixture of an organic pigment and an inorganic filler. 5 - A process for the preparation of the pigment composition of claims 1 to 4, »which comprises: (A) preparing an aqueous solution of the additive; (B) forming a slurry of a pigment in the solution to obtain a homogeneous liquid dispersion comprising from 85 to 99.5 parts by weight of the pigment and from 0.5 to 15 parts by weight of the additive, (C) by spray drying the resulting liquid dispersion , and (D) collecting the dried microgranules of the pigment composition. 6 - An organic material of high molecular weight pigmented, which comprises an effective amount of pigmentation of a pigment composition according to claims 1 to 4 and a high molecular weight organic material. 7 - A process for the preparation of an organic material of high pigmented molecular weight, which comprises incorporating a pigment composition according to claims 1 to 4 to the high molecular weight organic material as a mixing pigment. 8 - A high molecular weight organic material pigmented according to claim 6, wherein the high molecular weight organic material is a reactive coating system heat curable or interlaced. 9 - A high molecular weight organic material pigmented according to claim 8, wherein the high molecular weight organic material is a plastic that is calendered, cast, molded or processed to fibers and plastic articles that are calendered, cast, molded or processor to fibers. 10 - The use of the pigment compositions according to claims 1 to 4, characterized in that it is for the preparation of organic material of high pigmented molecular weight.