CN114316686A

CN114316686A - Pigment preparation, preparation method and application thereof

Info

Publication number: CN114316686A
Application number: CN202011047970.9A
Authority: CN
Inventors: 郑国民; 刘凯; 杨杰; 潘昌艺; 崔亭
Original assignee: Nippon Paint China Co Ltd
Current assignee: Nippon Paint China Co Ltd
Priority date: 2020-09-29
Filing date: 2020-09-29
Publication date: 2022-04-12
Also published as: WO2022068782A1

Abstract

The invention discloses a pigment preparation, which comprises the following raw materials in percentage by mass: 10-80 wt% of pigment; 0-50 wt% of a dispersant; 0-5 wt% of wetting agent; 0-3 wt% of defoaming agent; 0-1 wt% of bactericide; 0-3 wt% of anti-settling agent; and water, wherein the addition amount of the water is 100 wt% of the sum of the total mass percentages of the raw material components. The pigment preparation is a resin-free system, is universally used for pigments with different colors and is universally used for various water-based industrial coatings. The invention also discloses a preparation method and application of the pigment preparation.

Description

Pigment preparation, preparation method and application thereof

Technical Field

The invention relates to the technical field of water-based industrial coatings. More particularly, it relates to a pigment preparation and its preparation method and application.

Background

After long-term development, the paint varieties are various, and various classification methods are formed according to habits of many years. According to the dispersion medium, the paint can be divided into solvent-based paint and water-based paint. There are 17 types of coating materials classified by film-forming materials, such as acrylic resin coatings, polyurethane resin coatings, epoxy resin coatings, amino resin coatings, and alkyd resin coatings. The coating can be divided into the following according to the final application: architectural coatings, industrial coatings and special coatings. Therefore, in general, a coating material for an interior wall, an exterior wall, a ceiling, and a floor of a building is called an architectural coating material. The paint applied in a factory for machine and machine equipment, building accessories, household appliances, daily necessities, and the like is referred to as industrial paint.

Due to different application fields, the requirements on the performance of the coating are different. Generally, the requirements on the physical and chemical properties of industrial coatings are higher than those of architectural coatings, such as gloss, acid and alkali resistance, salt spray resistance and the like. Therefore, the performance requirements of various components in the coating are different particularly in the water-based coating, and the performance requirements such as water resistance of the dispersing agent and the influence of the dispersing agent on the gloss of a coating film in the water-based industrial coating are far higher than those in the water-based architectural coating.

The water-based industrial coating is divided into two-component polyurethane coating, two-component epoxy paint, one-component acrylic acid/polyurethane coating, water-based amino baking paint and the like according to film-forming substances. Since these coating resins differ in polarity, Solubility Parameter (SP) or hydrophilic-lipophilic balance (HLB) value, and curing mechanisms, it is often desirable to have a corresponding pigment preparation for the color matching of these coatings.

Like other coatings, aqueous industrial coatings generally consist of film-forming substances, pigments and fillers, solvents (water), and auxiliaries. The pigment can make the paint show rich color, make the paint have certain hiding power, and have the function of enhancing the mechanical property and durability of the coating film. However, the dispersion state, the particle size and the distribution of the pigment directly affect the application performance. In the supplied state, the pigment particles are bound together in aggregated form and are aggregates of pigments, and the coating must disperse these aggregates as much as possible to their original particle size to produce a stable pigment dispersion. Generally, paints contain pigments of various colors to match the exact color desired by the customer. The following processes are adopted in factory production to uniformly disperse a plurality of pigments in the paint:

the first method, a multiple pigment blend slurry process. All pigments used in the formula of the colored paint are mixed together, ground and dispersed into paint slurry by a sand mill or other grinding and dispersing equipment, and then the paint (resin), the solvent and the auxiliary agent are added to prepare the paint. The paint produced by the method is designed and fed for production only by the proportion of the pigment (often empirical data), and the colored paint with accurate pigment can not be obtained; secondly, since the difference in structural properties of the pigments is sometimes very different, the pigments cannot be sufficiently dispersed in the coating base material due to the difference in adsorption capacity to the base material during grinding and dispersion, and thus the optimum performance of the pigments cannot be exerted and the pigment dispersion efficiency is reduced. Even when a pigment dispersant is used, it cannot be fully utilized. Let alone control of the rheology of the coating. The more outstanding problems are low grinding dispersion efficiency, small production capacity and large workload of cleaning equipment when varieties and designs are changed. When raw materials fluctuate or a production plan is adjusted, the product quality is easily affected. More importantly, the pigment of the colored paint in batches has large fluctuation, great difficulty is brought to color matching, the color difference between products in each batch is large, and customers with high pigment accuracy requirements are very easy to return goods, cause warehouse overstock and fund overstock and influence the normal operation of the whole enterprise. Meanwhile, more paint and raw material waste can be caused in the processes of production, paint preparation, color mixing and the like, the cost is further increased, and the benefit is influenced.

The second method, single pigment milling. The pigment paint containing several pigments is made into single-colour pigment paste by grinding each pigment into slurry, and when the colour is mixed and made into paint, according to the formula, various single-colour pastes are mixed, and then the resin, solvent and various assistants are added so as to obtain the invented pigment paint with required colour. The method can select the optimum grinding equipment and process conditions according to the characteristics of each pigment because each pigment is ground and dispersed independently, and can also adopt different types of wetting agents and dispersing agents respectively, and the auxiliary agents can ensure that various pigments (including organic or inorganic pigments) can be sufficiently and stably dispersed in the same coating base material to exert the optimum performance of various pigments to the maximum extent. Compared with the first method, the accuracy of the colored paint prepared by the method is greatly improved, and the colored paint is accepted by most manufacturers at home and abroad. However, each color paste produced by the method must be ground and dispersed by using the resin used for producing the color paint, so that the color paste is single in use and has no versatility. If there are dozens of hundreds of paint varieties of different resin bases in the same factory. Hundreds of different mill bases are needed (even if there are several resins and several mill bases of the same color are needed for the same pigment). The production complexity is increased, the inventory is increased, and the mobile capital is increased; meanwhile, a large amount of single pigment slurry storage tanks are needed, and the occupied amount of equipment and products is increased. Sometimes, in some factories producing dozens of different pigment colors with only a few different resin base materials, the pigments are quite messy and complicated, and bring much trouble in management. In addition, when the method is used for producing the colored paint, the preparation of each monochromatic color paste is also involved, and then the paint preparation and color mixing are carried out, so that the process is complex, and the waste of paint and other components is easily caused. The single-color paste can only be used for producing colored paint in a factory, and cannot be used for color mixing in a remote factory, such as a retail store or a warehouse, the production time is long, and orders with short time requirements can only be looked at and cannot be regarded as good.

In view of the above problems, there is a need to provide a new pigment preparation.

Disclosure of Invention

A first object of the present invention is to provide a pigment preparation which is resin-free and suitable for use with pigments of various colors and in general with various aqueous industrial coatings.

A second object of the present invention is to provide a process for the preparation of a pigment preparation.

A third object of the present invention is to provide a use of the pigment preparation.

In order to achieve the first purpose, the invention adopts the following technical scheme:

the pigment preparation is characterized by comprising the following raw materials in percentage by mass:

wherein the addition amount of the water is 100 wt% of the total mass percentage of the components of the raw materials.

Optionally, the pigment has an average particle size of 0.1 to 5 μm.

Optionally, the pigment is an organic and/or inorganic pigment.

Optionally, the organic pigment is selected from one or more of a black pigment and a color pigment.

Optionally, the inorganic pigment is selected from one or more of a coloring pigment and a pearlescent pigment.

Optionally, the dispersant is an aqueous dispersant.

Optionally, the aqueous dispersant is selected from the group consisting of styrene/acrylic acid copolymers, acrylic acid/maleic acid copolymers, acrylic acid/methacrylic acid copolymers, butadiene/acrylic acid copolymers, isobutylene/maleic acid copolymers, diisobutylene/maleic acid copolymers, styrene/maleic acid copolymers, polyethylene glycol monovinyl ether/maleic acid copolymers, and block polymers of monomers of the foregoing copolymers, respectively, with at least one of an acrylate, a maleate, and/or a 1-alkene, such as 1-hexadecene, 1-octadecene, or 1-eicosene, as an additional monomer component.

Optionally, the wetting agent is selected from one or more of modified alkoxylates, polyether modified siloxanes, ethoxy acetylenic diol, and siloxane dual-purpose surfactants.

Optionally, the defoaming agent is selected from one or more of modified polysiloxane and polymer-based defoaming agent.

Optionally, the bactericide is selected from fungicides.

Optionally, the bactericide is a complex of 2-methyl-4-isothiazolin-3-one and 1, 2-benzisothiazolin-3-one.

Optionally, the anti-settling agent is selected from one or more of hectorite clay, fumed silica and polyamide wax.

To achieve the second object, the present invention provides a method for preparing a pigment preparation, comprising the steps of:

adding an optional dispersing agent, a wetting agent, a defoaming agent and an anti-settling agent into part of water, and stirring and mixing uniformly to obtain a mixture A, wherein the addition amount of the water is based on uniformly dispersing all components in the mixture A;

adding pigment into the mixture A, stirring and mixing uniformly, and grinding the mixture until the fineness is less than 10 mu m to obtain a mixture B;

and adding an optional bactericide and the rest of water into the mixture B, and uniformly mixing to obtain the pigment preparation.

To achieve the third objective, the present invention provides a pigment preparation for use in aqueous industrial coatings.

Optionally, the water-based industrial coating is selected from one or more of a water-based two-component polyurethane coating, a two-component epoxy paint, a one-component acrylic coating and a water-based amino baking paint.

The invention has the following beneficial effects:

in the pigment preparation provided by the invention, various pigments can be dispersed and stabilized by limiting the raw material components and the addition amount, and the pigment preparation is universally used in aqueous industrial coating systems such as aqueous two-component polyurethane coating, two-component epoxy coating, single-component acrylic acid, aqueous amino baking paint and the like. The pigment preparation has the advantages of good stability, weather resistance, acid and alkali resistance, high coloring strength and good color development. The paint has good compatibility with various aqueous industrial paint systems, does not influence the physical and chemical properties of the paint such as luster, water resistance, salt mist resistance and the like, has excellent environmental protection performance, and has no detection of various environmental protection limit substances such as Volatile Organic Compounds (VOC), free formaldehyde, benzene, toluene, ethylbenzene, xylene, glycol ether and ether esters, heavy metals, plasticizers and the like by third-party detection.

Detailed Description

In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.

According to one embodiment of the present invention, the present invention provides a pigment preparation, which comprises the following raw materials by mass:

Unless otherwise specified, the mass percentages in the present invention are relative to the total mass of the raw materials.

In the present embodiment, the pigment is a substance that provides color, and any colorable substance that can be used in the aqueous industrial coating material is within the aforementioned selection range of pigments. The pigments are generally in finely divided form, the average particle size preferably being controlled within the range from 0.1 to 5 μm. Optionally the pigment is an organic and/or inorganic pigment.

In some preferred examples, the organic pigment may be one or more of a black pigment and a color pigment. Specifically, organic pigments include, but are not limited to, those selected from the following classes: disazo pigments, disazo condensation pigments, dibenzpyrene dione pigments, anthraquinone pigments, anthrapyrimidine pigments, benzimidazolone pigments, quinacridone pigments, quinophthalone pigments, diketopyrrolopyrrole pigments, diazine pigments, indanthrone pigments, isoindoline pigments, isoindolinone pigments, perylene pigments, phthalocyanine pigments, pyrazole quinazolinone pigments, and combinations thereof.

Examples of suitable organic colored pigments include, but are not limited to: disazo pigments: c.i. pigment yellow 12, 13, 14, 16, 17, 81, 83, 106, 113, 126, 127, 155, 170, 174, 176 and 188; c.i. pigment orange 16, 34 and 44; disazo condensation pigment: c.i. pigment yellow 93, 95 and 128; c.i. pigment red 144, 166, 214, 220, 221, 242 and 262; c.i. pigment brown 23 and 41; dibenzopyrenedione pigment: c.i. pigment red 168; anthraquinone pigment: c.i. pigment yellow 147 and 199; c.i. pigment red 177; anthrapyrimidine pigments: c.i. pigment yellow 108; benzimidazolone pigments: c.i. pigment yellow 120, 151, 154, 180, 181; c.i. pigment orange 36 and 72; c.i. pigment red 175, 185, 208; c.i. pigment brown 25; c.i. pigment violet 32; quinacridone pigment: c.i. pigment orange 48 and 49; c.i. pigment red 122, 202, 206 and 209; c.i. pigment violet 19; quinophthalone pigments: c.i. pigment yellow 138; diketopyrrolopyrrole pigments: c.i. pigment orange 71, 73 and 81; c.i. pigment red 254, 255, 264, 270 and 272; a dioxazine pigment: c.i. pigment violet 23; indanthrone pigment: c.i. pigment blue 60 and 64; isoindoline pigment: c.i. pigment yellow 139 and 185; c.i. pigment orange 61 and 69; c.i. pigment red 260; isoindolinone pigments: c.i. pigment yellow 109, 110 and 173; perylene pigments: c.i. pigment red 123, 149, 178, 179 and 224; c.i. pigment violet 29; c.i. pigment black 31 and 32; phthalocyanine pigment: c.i. pigment blue 15, 15:1, 15:2, 15:3, 15:4, 15:6, 16; c.i. pigment green 7, 36; pyrazole quinazolinone pigments: c.i. pigment orange 67 and c.i. pigment red 216.

The inorganic pigment is preferably one or more of a coloring pigment and a pearlescent pigment. The coloring pigment can be black, white or colored. Examples of suitable inorganic pigments include, but are not limited to: white pigment: titanium dioxide (c.i. pigment white 6); black pigment: black iron oxide (c.i. pigment black 11), iron manganese black, spinel black (c.i. pigment black 27); carbon black (c.i. pigment black 7); graphite (c.i. pigment black 10); black iron chromium oxide (p. brown 29); red iron oxide (c.i. pigment red 101); brown iron oxide (c.i. pigment brown 6 and 7); yellow iron oxide (c.i. pigment yellow 42); nickel titanium yellow (c.i. pigment yellow 53; c.i. pigment yellow 157, 158, 159, 160, 161, 162, 163, 164, and 189); a spinel phase (c.i. pigment yellow 119); bismuth vanadate (c.i. pigment yellow 184). Examples of suitable fillers are inorganic pigments, such as transparent silica, alumina, aluminium hydroxide, natural and synthetic mica, talc, kaolin, calcium carbonates such as natural and precipitated chalk, and barium sulphate.

In this embodiment, exemplary pigments may be added to the raw materials of the pigment preparation in an amount including, but not limited to, 20 to 80 wt%, 25 to 75 wt%, 25 to 60 wt%, 30 to 60 wt%, 35 to 40 wt%, etc., preferably 25 to 75 wt%, in terms of mass percent content.

In the present embodiment, the dispersant is an aqueous dispersant, and in some preferred examples, it is a copolymer comprising two or more monomers. The copolymers may be in the form of random copolymers, alternating copolymers, block copolymers, comb polymers, and graft copolymers. The copolymers may be prepared by conventional polymerization methods, for example by free radical polymerization or by controlled free radical polymerization. Specifically, exemplary copolymers include, but are not limited to: styrene/acrylic acid copolymers, acrylic acid/maleic acid copolymers, acrylic acid/methacrylic acid copolymers, butadiene/acrylic acid copolymers, isobutylene/maleic acid copolymers, diisobutylene/maleic acid copolymers, styrene/maleic acid copolymers, polyethylene glycol monovinyl ether/maleic acid copolymers, and block polymers of monomers of the foregoing copolymers, respectively, with at least one of an acrylate, a maleate, and/or a 1-alkene, such as 1-hexadecene, 1-octadecene, or 1-eicosene, as an additional monomer component. For example, the dispersant may be a TEGO Dispers series product from Evonik corporation, such as TEGO Dispers 755W. BYK-DISPERSANT series styrene/maleic acid copolymers from BYK company block polymer products with acrylates, such as BYK-DISPERSANT 2012, BYK-DISPERSANT 2013; acrylic block copolymers of BASF corporation for controlled radical polymerization

Series products Ultra PX 4575, 4585 and the like.

In this embodiment, the amount of the dispersant added to the raw material includes, but is not limited to, 0, 1-50 wt%, 1-45 wt%, 5-40 wt%, 5-8 wt%, 15-40 wt%, 15-35 wt%, 15-30 wt%, 15-25 wt%, etc., preferably 5-40 wt%, based on the mass percentage. The addition amount of the dispersing agent can be obtained through experiments according to parameters such as specific varieties, particle size, specific surface area or oil absorption of the pigment. The method of testing is as follows:

1. preliminary estimation of dispersant dosage

Table 1 shows the properties and amounts of the different pigments.

TABLE 1 Properties and amounts of the different pigments

2. Determination of the amount of dispersant

Using the preliminarily estimated dosage as a starting point, gradually increasing the dosage according to a certain gradient interval (such as 20 wt% of the initial dosage), wherein the total number of the gradients is 10-20, grinding the sample of each gradient to the fineness of less than 10 micrometers, putting the sample into a freezing box together, keeping the temperature of the freezing box at (-18 +/-2) DEG C, taking out the sample after the sample is placed in the freezing box for 18 hours, storing the sample at (23 +/-2) DEG C for 6 hours, uniformly stirring, and then measuring the fineness again, wherein the dosage of the dispersing agent is generally low, the fineness returns to be coarse after freeze thawing, the fineness gets smaller and smaller with the increase of the dispersing agent, and when the fineness can keep less than 10 micrometers, the dosage of the dispersing agent of the sample is more preferable.

In this embodiment, the wetting agent includes, but is not limited to, a surfactant selected from, for example, modified alkoxylates, polyether modified siloxanes, ethoxylated acetylenic diols, and silicone dual surfactants. The products are from BASF modified alkoxylate Hydropalat WE 3650, BYK polyether modified siloxane BYK 349, Etonik company ethoxy acetylenediol Surfynol 104. The wetting agent is preferably an ethoxylated acetylenediol product

Exemplary amounts of wetting agents added to the raw materials of the pigment preparation include, but are not limited to, 0, 0.1-5 wt%, 0.1-4 wt%, 0.1-3 wt%, 0.1-2 wt%, 0.2-0.8 wt%, 0.2-0.6 wt%, 0.2-1.8 wt%, etc., preferably 0.2-0.6 wt%, by mass percent.

In the present embodiment, the defoaming agent may preferably be one or more of a modified polysiloxane and a polymer-based defoaming agent. The antifoam agent may be from BASF, Tego, BYK. More preferably Tego Foamex 830 defoamer from Tego. The amount of the defoaming agent added to the raw materials of the pigment preparation by mass percentage includes, but is not limited to, 0, 0.1 to 2 wt%, 0.1 to 1 wt%, 0.3 to 1 wt%, 0.2 to 0.6 wt%, etc., preferably 0.2 to 0.6 wt%.

In this embodiment, the germicide is a long-acting, broad-spectrum germicide, and may specifically include a fungicide, such as that from Thor

The bactericide selected by the invention is preferably a compound product of 2-methyl-4-isothiazolin-3-one (MIT) and 1, 2-benzisothiazolin-3-one (BIT), and has very broad-spectrum bactericidal activity on bacteria, mold and yeast causing water-based product pollution and degradation. The amount of the bactericide added to the raw materials of the pigment preparation by mass percentage includes, but is not limited to, 0, 0.2-0.8 wt%, 0.2-0.6 wt%, 0.2-0.5 wt%, 0.2-0.4 wt%, etc., preferably 0.2-0.4 wt%.

In this embodiment, when the pigment is an inorganic pigment in the raw materials of the pigment preparation, an anti-settling agent may be added to prevent settling and agglomeration because the pigment has a high density. The anti-settling agent is preferably a readily dispersible hectorite clay rheological aid (e.g., from Haimax corporation)

LT series products), fumed silica, polyamide wax, and the like. The addition amount of the anti-settling agent can be adjusted according to actual conditions. Exemplary, the anti-settling agent may be added in an amount including, but not limited to, 0, 0.5-2 wt%, 0.5-1.5 wt%, etc.

In the present embodiment, the sum of the total mass percentages of the raw material components is 100 wt%. The amount of water added is preferably 70 wt% or less.

In the pigment preparation, the composition and the dosage of each raw material have influence on the final coating performance of the product, such as gloss, water resistance, salt spray resistance and the like.

In a further embodiment of the present invention, there is provided a process for preparing a pigment preparation as above, comprising the steps of:

In the present embodiment, "optionally present" means that it may be present or absent, and when this component is not present in the raw material, it is added in an amount of 0; when this component is present in the raw materials, the amount added is not 0.

The mechanical equipment used in the preparation method is general equipment in a paint production factory, does not have complex procedures, can be used for industrial mass production, and has better practicability. In addition, the method is more suitable for the grinding process, and can prepare products with higher concentration and finer fineness.

In a further embodiment of the present invention, there is provided the use of a pigment preparation as described above in an aqueous industrial coating.

When the pigment preparation is used in one or more of aqueous industrial coatings including but not limited to aqueous two-component polyurethane coatings, two-component epoxy paints, one-component acrylic coatings and aqueous amino baking paints, the pigment preparation has good compatibility with other components in the coatings, the obtained coatings have various physicochemical properties such as luster, water resistance and salt mist resistance, and are excellent in environmental protection performance, and environmental protection limiters such as formaldehyde, VOC, APEO, benzene chemicals, glycol ethers and esters, heavy metals and plasticizers are not detected by a third party.

The technical solution of the present invention is described below with reference to some specific examples, and all parts and percentages are by mass unless otherwise specified. Unless otherwise indicated, all starting materials used are commercially available:

examples of preparation of pigment preparations:

example 1 white color

The formula of the pigment preparation is shown in table 2 below:

TABLE 2 formulation of pigment preparations

The preparation steps of the pigment preparation comprise: according to the size of the production batch, selecting a proper mixing cylinder, sequentially putting deionized water G-1, an anti-settling agent F, a dispersing agent B, a wetting agent C and a defoaming agent D into the mixing cylinder, stirring for 10-20 minutes at 200-500 rpm of a matched stirrer, then slowly adding titanium dioxide A, and gradually increasing the rotating speed of the stirrer to ensure that the slurry has a vortex of about 45 degrees in the mixing cylinder so as to ensure that various raw materials are uniformly mixed. And (3) after all the raw materials are put into the container, stirring the mixture for about 30 minutes, sanding the mixture by using a sand mill until the fineness of the mixture is less than 10 micrometers, adding a bactericide E, and adjusting the viscosity by using the residual deionized water G-2 to obtain the pigment preparation.

Example 2 Black color

The formula of the pigment preparation is shown in table 3 below:

TABLE 3 formulation of pigment preparations

The preparation steps of the pigment preparation comprise: according to the size of production batch, selecting a proper mixing cylinder, sequentially adding deionized water, a dispersing agent, a wetting agent and a defoaming agent in the formula into the mixing cylinder, stirring for 10-20 minutes at 200-500 rpm of a matched stirrer, then slowly adding carbon black, and gradually increasing the rotating speed of the stirrer to ensure that the slurry has a vortex of about 45 degrees in the mixing cylinder so as to ensure that all raw materials are uniformly mixed. And (3) after all the raw materials are put into the container, stirring the mixture for about 30 minutes, sanding the mixture by using a sand mill until the fineness of the mixture is less than 10 micrometers, adding a bactericide into the mixture, and adjusting the viscosity by using the residual deionized water to obtain a pigment preparation.

Example 3 iron Red

The formula of the pigment preparation is shown in table 4 below:

TABLE 4 formulation of pigment preparations

The preparation steps are the same as example 1, wherein deionized water accounting for 30.35 wt% of the raw material formula is used for mixing with an anti-settling agent, a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 1.75 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 4 iron yellow

The formula of the pigment preparation is shown in table 5 below:

TABLE 5 formulation of pigment preparations

The preparation steps are the same as example 1, wherein deionized water accounting for 35.60 wt% of the raw material formula is used for mixing with an anti-settling agent, a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 1.50 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 5 organic Red

The formula of the pigment preparation is shown in table 6 below:

TABLE 6 formulation of pigment preparations

The preparation steps are the same as example 2, wherein deionized water accounting for 20.00 wt% of the raw material formula is used for mixing with a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 3.60 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 6 organic yellow

The formula of the pigment preparation is shown in table 7 below:

TABLE 7 formulation of pigment preparations

The preparation steps are the same as example 2, wherein deionized water accounting for 35.00 wt% of the raw material formula is used for mixing with a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 3.50 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 7 phthalocyanine blue

The formula of the pigment preparation is shown in table 8 below:

TABLE 8 formulation of pigment preparations

The preparation steps are the same as example 2, wherein deionized water accounting for 33.70 wt% of the raw material formula is used for mixing with a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 4.70 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 8 phthalocyanine Green

The formula of the pigment preparation is shown in table 9 below:

TABLE 9 formulation of pigment preparations

The preparation steps are the same as example 2, wherein deionized water accounting for 16.90 wt% of the raw material formula is used for mixing with a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 2.40 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 9 purple

The formula of the pigment preparation is shown in table 10 below:

TABLE 10 formulation of pigment preparations

The preparation steps are the same as example 2, wherein deionized water accounting for 25.00 wt% of the raw material formula is used for mixing with a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 2.60 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Example 10 inorganic yellow

The formula of the pigment preparation is shown in table 11 below:

TABLE 11 formulation of pigment preparations

The preparation steps are the same as example 1, wherein deionized water accounting for 22.50 wt% of the raw material formula is used for mixing with an anti-settling agent, a dispersing agent, a wetting agent and a defoaming agent; deionized water in an amount of 2.50 wt% of the raw material formulation was used to adjust the viscosity to prepare a pigment preparation.

Comparative example 1

The pigment preparation was prepared according to the starting materials and methods disclosed in publication No. CN 108610747A.

Comparative example 2

Pigment preparations were prepared identical to the formulation of example 1, except that the C SURFYNOL wetting agent was changed to "ethylene glycol" and the remaining conditions were unchanged.

Comparative example 3

The formulation of example 1 was followed except that B BYK-DISPERSANT dispersant was usedIs changed into a model

Pigment preparations were prepared from the dispersant supplied by Uniqema, with the remainder of the conditions unchanged.

Comparative example 4

Pigment preparation-Black

The formula is as follows:

a pigment preparation was prepared by the method of reference example 1.

Comparative example 5

Pigment preparation-yellow

The formula is as follows:

yellow pigment (based on yellow iron oxide; pigment yellow 42): 75 wt%;

atmer 116 (dispersant): 4 wt%;

sodium carbonate (accelerator): 21 wt%.

A pigment preparation was prepared by the method of reference example 1.

Comparative example 6

Pigment preparation-blue

The formula is as follows:

a pigment preparation was prepared by the method of reference example 1.

Examples 1-10 examples of the use of the pigment preparations prepared in the preparation of aqueous industrial coatings

Example 11

The pigment preparations prepared in example 1, comparative example 2 and comparative example 3 were added to the aqueous baking varnish, aqueous two-component polyurethane varnish and aqueous two-component epoxy varnish, respectively, in the amounts and in the amounts shown in table 12 below, wherein the formulations of the aqueous baking varnish, aqueous two-component polyurethane varnish and aqueous two-component epoxy varnish are shown in tables 13 to 15 below, respectively.

Wherein, the related test method comprises the following steps:

the contrast ratio was determined according to GB/T23981.

Gloss (20 ℃ C., 60 ℃ C.) was measured according to GB/T9754.

The salt spray resistance test is carried out in accordance with the neutral salt spray test (NSS test) of GB/T10125.

The water resistance was carried out as specified in GB/T1733-1993 under the regulation A.

TABLE 12 formulation and Effect of the pigment preparations of example 1 and comparative examples 1 to 3 in aqueous stoving varnish, aqueous two-component polyurethane varnish and aqueous two-component epoxy varnish, respectively

TABLE 13 compositional formulation of the aqueous baking varnish in example 11

Composition of	Content (in)
		DPM	5.1
Diethylene glycol monobutyl ether (BDG)	2
		10% DMEA solution	3.1
Surfynol	0.8
		Antkote 2043 emulsion	65
Luwipal 072	12
		Deionized water	10
Texanol	1
		Tego wet 280	0.8
BYK 024	0.2
		Total of	100

TABLE 14 compositional formulation of the water-borne two-component polyurethane varnish in example 11

TABLE 15 compositional formulation of the aqueous two-component epoxy varnish in example 11

As can be seen from Table 12 above, the contrast ratio, gloss, salt spray resistance, and water resistance of example 1 are significantly better in the 3 coating systems than the comparative examples 1-3, especially in the aqueous baking varnish and aqueous epoxy systems, the gloss of comparative example 1 is very low, indicating poor compatibility.

Similar results were obtained by replacing the pigment preparation of example 1 with the pigment preparations of examples 3, 5-6 and 8-10 in the above-described manner.

Example 12

The pigment preparations prepared in example 2 and comparative example 4 were added to a water-borne stoving varnish white paint, a water-borne two-component polyurethane white paint and a water-borne two-component epoxy white paint, respectively, in the amounts and with the resulting effects shown in table 16 below, wherein the formulations of the water-borne stoving varnish white paint, the water-borne two-component polyurethane white paint and the water-borne two-component epoxy white paint are shown in tables 17 to 19 below, respectively.

TABLE 16 formulation and Effect of the pigment preparations of example 2 and comparative example 4 in aqueous stoving varnish white paint, aqueous two-component polyurethane white paint and aqueous two-component epoxy white paint, respectively

TABLE 17 composition recipe for water based baking varnish white paint in example 12

Composition of	Content (in)
		DPM	3.7
Diethylene glycol monobutyl ether (BDG)	1.4
		10% DMEA solution	2.2
Surfynol	0.6
		Antkote 2043 emulsion	46.8
Luwipal 072	8.6
		DIW	7.2
Texanol	0.7
		Tego wet 280	0.6
BYK 024	0.2
		Example 1	28.0
Total of	100

TABLE 18 compositional formulation of the water-borne two-component polyurethane white paint of example 12

TABLE 19 formulation of the aqueous two-component epoxy white paint of example 12

As can be seen from Table 16 above, the pigment preparations prepared in example 2 were added to the white paints of the above 3 coating systems, respectively, to give high gloss, low color grinding, good compatibility, and good salt spray resistance.

Example 13

The pigment preparations prepared in example 4 and comparative example 5 were added to a water-borne stoving varnish white paint, a water-borne two-component polyurethane white paint and a water-borne two-component epoxy white paint, respectively, in the amounts added and the effects obtained are shown in table 20 below.

The formulas of the water-based baking varnish white paint, the water-based double-component polyurethane white paint and the water-based double-component epoxy white paint are respectively shown in the above tables 17-19.

TABLE 20 formulation and Effect of the pigment preparations of example 4 and comparative example 5, respectively, in aqueous stoving varnish white paint, aqueous two-component polyurethane white paint and aqueous two-component epoxy white paint

As can be seen from Table 20 above, the pigment preparation of example 4 added to the white paints of the 3 coating systems showed high gloss, low color difference, good compatibility, and good salt spray resistance.

Examples 1-8 were tested by Nippon paint, Inc. (China) in accordance with GB18582-2008 for the total volatile organic compound content (VOC), free formaldehyde, benzene, toluene, ethylbenzene, xylene, and the total glycol ethers and ether esters in accordance with GB24408-2009, all of which were not detected (no indication: Volatile Organic Compound (VOC) <2 g/L; free formaldehyde < 5 mg/kg; total benzene, toluene, ethylbenzene, xylene, < 50 mg/kg; total glycol ether and ether ester content < 0.001%). The detection is carried out by the national building engineering material quality supervision and inspection center according to the GB24613-2009 determination of harmful substances in the paint for toys, GB/T26125-2011 determination of six limited substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyl and polybrominated diphenyl ether) in the electronic and electric products, GB/T30647-2014 determination of the total content of harmful elements in the paint, GB/T31414-2015 determination of alkylphenol polyoxyethylene ether of water-based paint surfactant, and related items are not detected (undetected description: 1, GB24613-2009, dibutyl phthalate, butyl benzyl phthalate, di-n-octyl phthalate, diisooctyl phthalate < 0.002%, diisononyl phthalate, diisodecyl phthalate < 0.01%. 2, GB/T26125-2011, hexavalent chromium <1 mg/kg.3, hexavalent chromium < 1.3, According to GB/T30647-2014, lead is less than 4mg/kg, cadmium is less than 2mg/kg, cobalt is less than 2mg/kg, mercury is less than 2mg/kg, antimony is less than 3mg/kg, barium is less than 10mg/kg, arsenic is less than 2mg/kg, and selenium is less than 2 mg/kg. 4. According to GB/T31414-2015, the alkylphenol polyoxyethylene ether is less than 10 mg/kg. ). In addition, the products of examples 9-10 also had similar properties to those of examples 1-8.

In conclusion, the environment-friendly universal water-based resin-free pigment preparation can be universally used in various water-based industrial coating systems such as water-based two-component polyurethane coating, two-component epoxy paint, one-component acrylic acid, water-based amino baking paint and the like, has good compatibility with various coating systems, does not influence various physical and chemical properties such as the gloss of the coating and the like, and has excellent environment-friendly performance. Through third-party detection, environmental-friendly limiters such as formaldehyde, VOC, APEO, benzene chemicals, glycol ether and esters, heavy metals, plasticizers and the like are not detected, and the environmental-friendly performance is excellent. The production and preparation method is simple, does not need special equipment and has strong practicability. And therefore have been mass produced and used in companies' various coating systems.

It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.

Claims

1. The pigment preparation is characterized by comprising the following raw materials in percentage by mass:

2. The pigment preparation according to claim 1, wherein the pigment has an average particle size of 0.1-5 μm; preferably, the pigment is an organic and/or inorganic pigment; preferably, the organic pigment is selected from one or more of black pigment and color pigment; the inorganic pigment is selected from one or more of coloring pigment and pearlescent pigment.

3. The pigment preparation of claim 1, wherein the dispersant is an aqueous dispersant; the aqueous dispersant is selected from styrene/acrylic acid copolymer, acrylic acid/maleic acid copolymer, acrylic acid/methacrylic acid copolymer, butadiene/acrylic acid copolymer, isobutylene/maleic acid copolymer, diisobutylene/maleic acid copolymer, styrene/maleic acid copolymer, polyethylene glycol monovinyl ether/maleic acid copolymer and block polymers formed by respectively reacting monomers of the foregoing copolymers with at least one of acrylate, maleate and/or 1-alkene, such as 1-hexadecene, 1-octadecene or 1-eicosene, as an additional monomer component.

4. The pigment preparation according to claim 1, wherein the wetting agent is selected from one or more of modified alkoxylates, polyether modified silicones, ethoxylated acetylenic diols, and silicone dual surfactants.

5. The pigment preparation according to claim 1, wherein the defoamer is selected from one or more of modified polysiloxanes and polymer-based defoamers.

6. Pigment preparation according to claim 1, wherein the fungicide is selected from fungicides; preferably, the bactericide is a complex of 2-methyl-4-isothiazolin-3-one and 1, 2-benzisothiazolin-3-one.

7. Pigment preparation according to claim 1, wherein the anti-settling agent is selected from one or more of hectorite clay, fumed silica, polyamide wax.

8. A process for the preparation of a pigment preparation according to any one of claims 1 to 7, comprising the steps of:

9. Use of the pigment preparation according to any of claims 1 to 7 in aqueous industrial coatings.

10. The use according to claim 9, wherein the aqueous industrial coating is selected from one or more of aqueous two-component polyurethane coating, two-component epoxy coating, one-component acrylic coating, aqueous amino baking finish.