CN114539808A - High-dispersity pearlescent pigment and preparation method thereof - Google Patents
High-dispersity pearlescent pigment and preparation method thereof Download PDFInfo
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- CN114539808A CN114539808A CN202210201436.1A CN202210201436A CN114539808A CN 114539808 A CN114539808 A CN 114539808A CN 202210201436 A CN202210201436 A CN 202210201436A CN 114539808 A CN114539808 A CN 114539808A
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- pearlescent pigment
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- slurry
- coupling agent
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- 239000000049 pigment Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 30
- 238000000576 coating method Methods 0.000 claims abstract description 23
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 239000007822 coupling agent Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000007599 discharging Methods 0.000 claims abstract description 10
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000011787 zinc oxide Substances 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229920003217 poly(methylsilsesquioxane) Polymers 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 4
- 229910003074 TiCl4 Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/401—Inorganic protective coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/402—Organic protective coating
- C09C2200/403—Low molecular weight materials, e.g. fatty acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/402—Organic protective coating
- C09C2200/407—Organosilicon materials, e.g. silanes, silicones
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/10—Wet methods, e.g. co-precipitation
Abstract
The invention discloses a high-dispersity pearlescent pigment and a preparation method thereof; firstly, carrying out oxide coating treatment on a flaky pearlescent pigment, adding a siloxane modifier, stirring and mixing, adding an organic coupling agent into slurry, stirring, discharging, and drying a filter cake to obtain a high-dispersibility pearlescent pigment; through 1 or 2 times of coating treatment on the pearlescent pigment, the surface wettability of the pearlescent pigment powder is fully, compactly and uniformly improved by adopting modification of organic siloxane and an organic coupling agent, and the dispersibility of the powder in a solvent is further improved.
Description
Technical Field
The invention relates to the technical field of pigment preparation, in particular to a high-dispersity pearlescent pigment and a preparation method thereof.
Background
Pearlescent pigments are widely used in the fields of paints, plastics, inks, and the like because of their special pearlescent color; when the pearlescent pigment is applied to printing ink, the pearlescent pigment can not only generate a pearlescent effect when the original color tone is kept, but also bring various gloss colors, and is often used for printing various articles such as advertisements, packaging paper, textiles and the like;
the pearlescent pigment is generally in a flake structure, can be mixed into printing ink with low viscosity by slight stirring, and can be quickly wetted and dispersed in a system, but the compatibility of the pearlescent pigment and an organic solvent is poor, namely the pigment has low affinity to an ink medium, is easy to deposit after being placed for a long time with ink or paint and the like, and is difficult to disperse in the system; in order to increase pearlescence in printing, the content of the pearlescent pigment is generally increased, the poor dispersibility of the pearlescent pigment can cause printing nonuniformity, and the pearlescent pigment is even separated from a medium and stuck on a printing device;
one of the existing solutions is to prevent pigment aggregation by providing a good wetting and dispersion system; another approach is to have the pigment well suspended in the vehicle; the prior Chinese patent CN 110272641A firstly carries out inorganic coating treatment on a pearlescent pigment (A), and then at least one silane surface modifier and at least one coupling agent are added into an aqueous suspension of the pigment obtained by treatment to modify the pigment to obtain the pearlescent pigment; the pigment has the defects of insufficient, incompact and uneven coating, thereby causing poor dispersibility.
Disclosure of Invention
The invention provides a high-dispersity pearlescent pigment and a preparation method thereof, and aims to solve the technical problems in the prior art.
The technical scheme of the invention is realized as follows: a preparation method of high-dispersity pearlescent pigment; the method is characterized in that: the method comprises the following steps:
step one, adding water into flake pearlescent pigment to carry out oxide coating treatment to prepare slurry,
and step two, adding the siloxane modifier when the temperature of the slurry is raised to 60-80 ℃, and stirring.
Adding an organic coupling agent into the slurry, stirring, discharging, and drying a filter cake to obtain the high-dispersibility pearlescent pigment;
wherein the addition amount of the siloxane modifier is 0.15 to 0.45 weight percent of the flaky pearlescent pigment; the siloxane modifier comprises one or two of polymethylsilsesquioxane and polypropylsilsesquioxane;
the addition amount of the organic coupling agent is 0.1-0.5% by weight of the flaky pearlescent pigment, and the organic coupling agent comprises one or two of isopropyl trititanate, KR-38S, KR-138S, KR-TTS and KR-238S, KR-7.
Adding zinc oxide or ferric oxide into a mixed solution of flake pearlescent pigment and water to carry out coating treatment to prepare slurry; stirring, filtering, washing, drying and calcining to obtain the pearlescent pigment.
The first step also comprises the steps of adding zinc oxide or ferric oxide into the mixed solution of the flake pearlescent pigment and water for coating, and dripping water-soluble TiCl at the temperature of 70-80 DEG C4Coating the solution, stirring, heating to 82-89 deg.C, and adding TiCl at uniform speed4A solution, during which the pH is maintained between 3 and 6;
the TiCl4The addition amount of (B) is 0.8-1.5% by weight based on the mixed liquid of flake pearlescent pigment and water.
The addition amount of the oxide is 0.3-2% by weight of the mixed solution of the flaky pearlescent pigment and water.
The oxide coating method and the titanate coating method adopted by the invention have the advantages that the flaky pearlescent pigment is coated more fully, compactly and uniformly by 1 or 2 times of coating treatment, and the dispersibility of the pearlescent pigment is further improved.
The invention has the beneficial effects that the high-dispersity pearlescent pigment and the preparation method thereof are provided, the surface wettability of pearlescent pigment powder is fully, compactly and uniformly improved by coating the pearlescent pigment for 1 or 2 times and modifying organic siloxane and an organic coupling agent, and the dispersity of the powder in a solvent is further improved.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
[ example 1 ] A method for producing a polycarbonate
Selecting 150 parts by weight of flake pearlescent pigment and water, mixing the flake pearlescent pigment and the water according to a solid-to-liquid ratio of 1:8 to prepare slurry, adding 0.3% by weight of zinc oxide solution calculated by the slurry to mix and coat, then heating the slurry to 60 ℃, adding 0.15% by weight of polymethylsilsesquioxane solution calculated by the flake pearlescent pigment, stirring for 30 minutes, adding 0.1% by weight of organic coupling agent isopropyl trititanate calculated by the flake pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and obtaining the high-dispersity pearlescent pigment through filter cakes.
[ example 2 ]
Similar to example 1, except;
adding 0.3 weight percent of zinc oxide or ferric oxide solution calculated by the slurry to mix and coat, then heating the slurry to 80 ℃, adding 0.45 weight percent of polymethylsilsesquioxane solution calculated by the flaky pearlescent pigment, stirring for 30 minutes, adding 0.5 weight percent of organic coupling agent isopropyl trititanate calculated by the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and obtaining the high-dispersity pearlescent pigment from filter cakes.
[ example 3 ]
Similar to example 1, except; adding zinc oxide solution accounting for 0.3 weight percent of the slurry to mix and coat, then heating the slurry to 80 ℃, dropwise adding water-soluble TiCl4 solution accounting for 0.8 weight percent of the mixture of flaky pearlescent pigment and water at a constant speed to carry out secondary coating, stirring, heating to 82 ℃, and keeping the pH value at 6; adding 0.15 weight percent of polymethylsilsesquioxane solution based on the flaky pearlescent pigment, stirring for 30 minutes, adding 0.1 weight percent of organic coupling agent isopropyl trititanate based on the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and filtering a filter cake to obtain the high-dispersibility pearlescent pigment.
[ example 4 ]
Similar to example 1, except; adding zinc oxide or ferric oxide solution with the weight portion of 2 percent of the slurry for mixing and coating, then heating the slurry to 70 ℃, and dropwise adding water-soluble TiCl with the weight portion of 1.5 percent of the mixed solution of flake pearlescent pigment and water at a constant speed4Carrying out secondary coating on the solution, stirring, heating to 89 ℃, and keeping the pH value at 3 during the period; adding 0.45 weight percent of polymethylsilsesquioxane solution based on the flaky pearlescent pigment, stirring for 30 minutes, adding 0.5 weight percent of organic coupling agent isopropyl trititanate based on the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and filtering a filter cake to obtain the high-dispersibility pearlescent pigment.
[ example 5 ]
Similar to example 1, except; adding 2 weight percent of ferric oxide solution based on the slurry to mix and coat, and then lifting the slurryThe temperature is raised to 70 ℃, 0.8 weight percent of water-soluble TiCl calculated by the mixed solution of the flake pearlescent pigment and the water is dripped at a constant speed4Carrying out secondary coating on the solution, stirring, heating to 89 ℃, and keeping the pH value at 5 during the period; adding 0.15 weight percent of polymethylsilsesquioxane solution based on the flaky pearlescent pigment, stirring for 30 minutes, adding 0.5 weight percent of organic coupling agent isopropyl trititanate based on the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and obtaining the high-dispersibility pearlescent pigment from a filter cake.
[ example 6 ]
Similar to example 1, except; adding zinc oxide or ferric oxide solution with the weight part of 0.3 percent of the slurry to mix and coat, then heating the slurry to 60 ℃, dripping water-soluble TiCl with the weight part of 1.5 percent of the mixture of flake pearlescent pigment and water with uniform speed4Carrying out secondary coating on the solution, stirring, heating to 89 ℃, and keeping the pH value at 5 during the period; adding 0.45 weight percent of polypropylsilsesquioxane solution calculated by the flaky pearlescent pigment, stirring for 30 minutes, adding 0.1 weight percent of organic coupling agent isopropyl trititanate calculated by the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and obtaining the high-dispersibility pearlescent pigment from the filter cake.
[ example 7 ]
Similar to example 6, except; adding zinc oxide or ferric oxide solution with the weight portion of 2 percent of the slurry to mix and coat, then heating the slurry to 60 ℃, and dripping 0.8 percent of water-soluble TiCl with the weight portion of the mixture of flake pearlescent pigment and water with uniform speed4Carrying out secondary coating on the solution, stirring, heating to 82 ℃, and keeping the pH value at 3 during the period; adding 0.15 weight percent of polymethylsilsesquioxane based on the flaky pearlescent pigment and a polypropylsilsesquioxane solution, stirring for 30 minutes, adding 0.5 weight percent of organic coupling agent isopropyl trititanate based on the flaky pearlescent pigment into the slurry, stirring for 30 minutes, discharging, drying at 150 ℃, and obtaining the pearlescent pigment with high dispersibility from a filter cake.
The products obtained in examples 1 to 7 above and the flaky pearlescent pigment were subjected to a sedimentation test. The procedure for the sedimentation experiment was: putting 3g of the prepared pearlescent pigment product into a 100mL measuring cylinder, adding 97g of distilled water, uniformly stirring, and detecting the viscosity; standing for 30min, 6h and 24h, and measuring the thickness of the pearl powder settled at the bottom of the measuring cylinder.
The results of the settling experiments are shown in table 1.
Table 1 results of sedimentation experiments
As can be seen from table 1, the pearlescent pigments prepared in the examples of the present invention, after being mixed with water, have deposited precipitates with a thickness greater than that of the flake pearlescent pigments, and the precipitates are loose and easily re-dispersed; has better redispersibility and can meet the use requirement.
The pearlescent pigment modified and prepared by the method has golden or red hue, and the surface wettability of the pearlescent pigment powder is fully, compactly and uniformly improved by coating the pearlescent pigment for 1 or 2 times and modifying by adopting organic siloxane and an organic coupling agent, so that the dispersibility of the powder in a solvent is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A preparation method of high-dispersity pearlescent pigment; the method is characterized in that: the method comprises the following steps:
step one, adding water into flake pearlescent pigment to perform oxide coating treatment to prepare slurry;
step two, when the temperature of the slurry is raised to 60-80 ℃, adding a siloxane modifier and stirring;
adding an organic coupling agent into the slurry, stirring, discharging, and drying a filter cake to obtain the high-dispersibility pearlescent pigment;
wherein the addition amount of the siloxane modifier is 0.15 to 0.45 weight percent of the flaky pearlescent pigment; the siloxane modifier comprises one or two of polymethylsilsesquioxane and polypropylsilsesquioxane;
the addition amount of the organic coupling agent is 0.1-0.5% by weight of the flaky pearlescent pigment, and the organic coupling agent comprises one or two of isopropyl trititanate, KR-38S, KR-138S, KR-TTS and KR-238S, KR-7.
2. The method for preparing a highly dispersible pearlescent pigment according to claim 1, characterized in that:
adding zinc oxide or ferric oxide into a mixed solution of flake pearlescent pigment and water to carry out coating treatment to prepare slurry; stirring, filtering, washing, drying and calcining to obtain the pearlescent pigment.
3. The method for preparing a highly dispersible pearlescent pigment according to claim 1, characterized in that:
the first step also comprises the steps of adding zinc oxide or ferric oxide into the mixed solution of the flake pearlescent pigment and water for coating, and dripping water-soluble TiCl at the temperature of 70-80 DEG C4Coating the solution, stirring, heating to 82-89 deg.C, and adding TiCl at uniform speed4A solution, during which the pH is maintained between 3 and 6;
the TiCl4The addition amount of (B) is 0.8-1.5% by weight based on the mixed liquid of flake pearlescent pigment and water.
4. The method for preparing a highly dispersible pearlescent pigment according to claim 1, characterized in that: the addition amount of the oxide is 0.3-2% by weight of the mixed solution of the flaky pearlescent pigment and water.
5. The highly dispersible pearlescent pigment produced by the method for producing highly dispersible pearlescent pigment according to any one of claims 1 to 4.
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CN202210201436.1A CN114539808A (en) | 2022-03-03 | 2022-03-03 | High-dispersity pearlescent pigment and preparation method thereof |
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CN105860593A (en) * | 2016-04-08 | 2016-08-17 | 广东工业大学 | Composition capable of enhancing pearlescent effect of pearlescent pigment, and preparation method and application thereof |
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CN111303664A (en) * | 2020-03-23 | 2020-06-19 | 福建坤彩材料科技股份有限公司 | Silver pearlescent pigment and preparation method and application thereof |
CN113248944A (en) * | 2020-06-24 | 2021-08-13 | 广西七色珠光材料股份有限公司 | Pearlescent pigment for powder coating, preparation method and reaction device thereof |
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US4318844A (en) * | 1979-06-20 | 1982-03-09 | Bayer Aktiengesellschaft | Inorganic pigments with improved gloss and distribution in lacquer binders |
CN1342731A (en) * | 2000-09-01 | 2002-04-03 | 户田工业株式会社 | Compound particle, its preparation method and pigment, paint and resin composition using the compound particle |
CN1353145A (en) * | 2000-11-06 | 2002-06-12 | 默克专利股份有限公司 | Stabilization of pearl light luster pigment |
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