CN116445013A - Preparation method of nonferrous metal pigment - Google Patents
Preparation method of nonferrous metal pigment Download PDFInfo
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- CN116445013A CN116445013A CN202310261677.XA CN202310261677A CN116445013A CN 116445013 A CN116445013 A CN 116445013A CN 202310261677 A CN202310261677 A CN 202310261677A CN 116445013 A CN116445013 A CN 116445013A
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- nonferrous metal
- metal powder
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 78
- 239000002184 metal Substances 0.000 title claims abstract description 78
- 239000000049 pigment Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 21
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 21
- 239000003086 colorant Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- 239000011241 protective layer Substances 0.000 claims abstract description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000007524 organic acids Chemical class 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 7
- GGAUUQHSCNMCAU-ZXZARUISSA-N (2s,3r)-butane-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C[C@H](C(O)=O)[C@H](C(O)=O)CC(O)=O GGAUUQHSCNMCAU-ZXZARUISSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- BWKIBIZZLRPKFY-UHFFFAOYSA-N 1,2,3-benzothiadiazole-5-carbaldehyde Chemical compound O=CC1=CC=C2SN=NC2=C1 BWKIBIZZLRPKFY-UHFFFAOYSA-N 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- MYONAGGJKCJOBT-UHFFFAOYSA-N benzimidazol-2-one Chemical compound C1=CC=CC2=NC(=O)N=C21 MYONAGGJKCJOBT-UHFFFAOYSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 150000001875 compounds Chemical group 0.000 claims description 3
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- PXZQEOJJUGGUIB-UHFFFAOYSA-N isoindolin-1-one Chemical compound C1=CC=C2C(=O)NCC2=C1 PXZQEOJJUGGUIB-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 3
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 claims 2
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 claims 1
- 239000008096 xylene Substances 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 9
- 239000002932 luster Substances 0.000 abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 7
- 239000010410 layer Substances 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003795 desorption Methods 0.000 abstract 1
- 230000006872 improvement Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- QNUOBYLNEXVUMC-UHFFFAOYSA-N 2h-pyren-1-one Chemical compound C1=C2C(=O)CC=C(C=C3)C2=C2C3=CC=CC2=C1 QNUOBYLNEXVUMC-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- VPWFPZBFBFHIIL-UHFFFAOYSA-L disodium 4-[(4-methyl-2-sulfophenyl)diazenyl]-3-oxidonaphthalene-2-carboxylate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=CC(C)=CC=C1N=NC1=C(O)C(C([O-])=O)=CC2=CC=CC=C12 VPWFPZBFBFHIIL-UHFFFAOYSA-L 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- C09C1/62—Metallic pigments or fillers
-
- 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
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
- C09C1/642—Aluminium treated with inorganic compounds
-
- 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
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
- C09C1/644—Aluminium treated with organic compounds, e.g. polymers
-
- 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
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
- C09C1/648—Aluminium treated with inorganic and organic, e.g. polymeric, compounds
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The preparation method of the nonferrous metal pigment comprises the following preparation steps: dispersing metal powder in a hydrophilic solvent, adding a silane coupling agent, and adjusting the pH value; adding hydrophilic solvent, polyacrylic acid and organic acid to obtain metal powder coated with polyacrylic acid; adding a colorant into solvent oil to react with amine, and adding metal powder coated with polyacrylic acid to obtain nonferrous metal powder; and (3) coating the nonferrous metal powder on the protective layer, and treating to obtain the nonferrous metal pigment. The coated high polymer is colorless and transparent, polyacrylic acid is adopted as a raw material, a certain amount of acid is added, polymerization reaction does not occur in the process, only condensation dehydration reaction occurs, the surface film layer is thin, about 120nm is achieved, and the luster of the metal powder is not affected; the coated high polymer does not need to carry out polymerization reaction, and is simple and easy to control; the carboxyl is introduced into the metal powder, and the amino is introduced into the organic colorant, so that the colorant can be tightly coated on the surface of the metal powder; the ethyl orthosilicate is hydrolyzed to form a protective layer on the surface to prevent the coloring agent from desorption.
Description
Technical Field
The invention relates to the technical field of pigment preparation methods, in particular to a preparation method of nonferrous metal pigment.
Background
Metallic luster pigments have bright metallic luster and color, and are therefore used as decorative pigments in the fields of automobiles, inks, textiles, color cosmetics, plastics, ceramics, and the like. The existing lustrous pigments mainly adopt mica materials, but the glossiness is general.
Coating a coloring pigment on a metal can obtain a pigment having metallic luster and vivid color. The flaky aluminum powder, zinc powder or alloy thereof is adopted as a base material, so that the color is bright, and the metal luster is good. The components are simple and controllable, and no toxic or side effect is caused. However, the metal powder is difficult to color, the condition of the coating reaction of the metal powder by using the polymer polymerization reaction is complex, the operation is complex, the combination of the polymer and the metal is difficult to ensure, and the color and luster and the glossiness of the coated pigment are difficult to ensure.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a nonferrous metal pigment.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of the nonferrous metal pigment comprises the following preparation steps:
1) Dispersing metal powder in a hydrophilic solvent, adding a silane coupling agent, regulating the pH value by using triethanolamine, stirring for 1-8 hours at the temperature of 40-80 ℃, filtering, and cleaning for 1-2 times by using the hydrophilic solvent;
2) Adding hydrophilic solvent, polyacrylic acid and organic acid, and stirring at 40-80 ℃ for 1-8 h to obtain metal powder coated with polyacrylic acid;
3) Adding a colorant into solvent oil to react with amine, adding metal powder coated with polyacrylic acid, heating and stirring for 1-8 h at 40-80 ℃ to obtain nonferrous metal powder;
4) The nonferrous metal powder is coated on the protective layer for treatment, and is washed by hydrophilic solvent for 1 to 2 times, and is subjected to heat treatment for 1 to 4 hours at 160 to 200 ℃ to obtain the nonferrous metal pigment.
As a further improvement of the invention: the metal powder in the step 1) adopts aluminum powder or zinc powder or alloy powder thereof.
As a further improvement of the invention: the silane coupling agent in the step 1) is one or more of vinyl, amino, epoxy, sulfhydryl silane coupling agent or titanane coupling agent.
As a further improvement of the invention: and 3) regulating the pH value of the triethanolamine in the step 1) to 8-10.
As a further improvement of the invention: the organic acid in the step 2) is one or more of oxalic acid, citric acid, tartaric acid and butane tetracarboxylic acid.
As a further improvement of the invention: the colorant in the step 3) is at least one of azo pigments, phthalocyanine pigments, AS color phenolic pigments, benzimidazolone pigments, perylene series and pyrenone pigments, isoindolinone pigments and quinophthalone pigments.
As a further improvement of the invention: the solvent oil in the step 3) is one of dimethylbenzene or ethyl acetate.
As a further improvement of the invention: the amine in the step 3) is one or two of monoethanolamine, diethanolamine, triethanolamine, ammonia water, ethylenediamine, tert-butylamine and n-butylamine.
As a further improvement of the invention: the step 4) of coating and protecting layer treatment comprises the following steps: adding nonferrous metal powder into ethanol, slowly adding the prepared A, B solution, heating at 40-60deg.C, stirring for 8-16 hr, and filtering; the solution A is ethanol solution of tetraethoxysilane, and the solution B is a compound solution of water, organic amine and ethanol. As a further improvement of the invention: the preparation method comprises the following preparation steps:
(1) Adding 30g of Al powder into a three-necked flask, weighing 200g of isopropanol, regulating the pH value to 8-10 with triethanolamine, slowly adding 12g of vinyltriethoxysilane, heating and stirring at 50 ℃ for 5 hours, filtering after the reaction is finished, and washing with alcohol for 1-2 times to obtain a first-step product;
(2) The product of the first step was added to a three-necked flask containing 200g of isopropanol and the mixed solution was slowly added: 18.0g polyacrylic acid, 2.0g butane tetracarboxylic acid and proper amount of isopropanol; heating and stirring at 80 ℃ for 6 hours, evaporating the solvent by adopting a rotary evaporator to obtain aluminum powder coated with polyacrylic acid, and heating at 160 ℃ for 30 minutes to obtain a second-step product;
(3) Adding 12g of phthalocyanine blue into a three-neck flask containing 200g of solvent oil, slowly adding 2g of ethylenediamine and 6g of n-butylamine, stirring at 80 ℃ for 4 hours, adding the second-step product, continuously stirring for 12 hours, filtering, and drying the filtered powder at 200 ℃ for 4 hours to obtain a third-step product;
(4) Preparing a solution A: adding 10.0g of tetraethyl orthosilicate into 40.0g of isopropanol, and uniformly stirring; preparing a solution B: adding 3.0g of ethylenediamine monohydrate into 25.0g of isopropanol, adding 75.0g of water, and uniformly stirring;
(5) Adding the product of the third step into a three-neck flask containing 200g of isopropanol, heating to 40 ℃, simultaneously dropwise adding the solution A and the solution B under stirring, continuously stirring at 40 ℃ for 12 hours after the solution A, B is dropwise added, filtering, and drying at 200 ℃ for 1.5 hours to obtain the nonferrous metal pigment.
Compared with the prior art, the invention has the beneficial effects that:
1) The coated high molecular polymer is colorless and transparent, polyacrylic acid is used as a raw material, a certain amount of acid is added, the polymerization reaction does not occur in the process, and only condensation dehydration reaction occurs. The surface film layer is thin, and the luster of the metal powder is not affected;
2) The coated high polymer does not need to carry out polymerization reaction, and is simple and easy to control;
3) The carboxyl is introduced into the metal powder, and the amino is introduced into the organic colorant, so that the colorant can be tightly coated on the surface of the metal powder;
4) Hydrolysis of Ethyl orthosilicate to form SiO on the surface 2 And a protective layer for preventing the colorant from being desorbed.
Drawings
For a clearer description of the technical solutions, the drawings that are required to be used in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the preparation of the nonferrous metal pigment of the present invention;
FIG. 2 is a schematic view of a comparative example and a nonferrous metal pigment prepared according to the present invention under a microscope;
FIG. 3 is a schematic structural view of the nonferrous metal pigment of the present invention
FIG. 4 is an SEM image of a comparative example pigment;
FIG. 5 is an SEM image of the nonferrous metal pigment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention and corresponding drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention will now be further described with reference to the accompanying drawings and examples:
the preparation method of the nonferrous metal pigment comprises the following preparation steps:
1) Dispersing metal powder in a hydrophilic solvent, adding a silane coupling agent, regulating the pH value by using triethanolamine, stirring for 1-8 hours at the temperature of 40-80 ℃, filtering, and cleaning for 1-2 times by using the hydrophilic solvent;
2) Adding hydrophilic solvent, polyacrylic acid and organic acid, and stirring at 40-80 ℃ for 1-8 h to obtain metal powder coated with polyacrylic acid;
3) Adding a colorant into solvent oil to react with amine, adding metal powder coated with polyacrylic acid, heating and stirring for 1-8 h at 40-80 ℃ to obtain nonferrous metal powder;
4) The nonferrous metal powder is coated on the protective layer for treatment, and is washed by hydrophilic solvent for 1 to 2 times, and is subjected to heat treatment for 1 to 4 hours at 160 to 200 ℃ to obtain the nonferrous metal pigment.
As an embodiment of the present invention, the metal powder in the step 1) is a flake aluminum powder or zinc powder or an alloy powder thereof; the silane coupling agent is one or more of vinyl, amino, epoxy, mercapto silane coupling agent or titanane coupling agent; the pH value of the ethanol is regulated to 8-10.
As an embodiment of the present invention, the organic acid in the step 2) is one or more of oxalic acid, citric acid, tartaric acid and butane tetracarboxylic acid.
AS an embodiment of the present invention, the colorant in the step 3) is at least one of azo pigments, phthalocyanine pigments, AS color phenol pigments, benzimidazolone pigments, perylene series and pyrenone pigments, isoindolinone pigments, quinophthalone pigments; the solvent oil is one of dimethylbenzene or ethyl acetate; the amine is one or two of monoethanolamine, diethanolamine, triethanolamine, ammonia water, ethylenediamine, tert-butylamine and n-butylamine.
As an embodiment of the present invention, the step 4) of coating the protective layer includes the steps of: adding nonferrous metal powder into ethanol, slowly adding the prepared A, B solution, heating at 40-60deg.C, stirring for 8-16 hr, and filtering; the solution A is ethanol solution of tetraethoxysilane, and the solution B is a compound solution of water, organic amine and ethanol.
As shown in fig. 3, the structure of the nonferrous metal pigment of the present invention includes a protective layer 1, a colored layer 2, a polymer layer 3, and a metal layer 4.
Embodiment case one:
the preparation method of the nonferrous metal pigment comprises the following preparation steps:
1) Weighing 30g of Al powder and adding the Al powder into a three-necked flask;
2) 200g of isopropanol and dispersed aluminum powder are weighed, the pH value is regulated to 8-10 by triethanolamine, and 12g of vinyltriethoxysilane is slowly added;
3) Heating and stirring for 5h at 50 ℃, filtering after the reaction is finished, and washing with alcohol for 1-2 times to obtain a product of the first step;
4) The product of the first step was added to a three-necked flask containing 200g of isopropanol and the mixed solution was slowly added: 18.0g polyacrylic acid, 2.0g butane tetracarboxylic acid and proper amount of isopropanol;
5) Heating and stirring for 6h at 80 ℃, and evaporating the solvent by adopting a rotary evaporator to obtain the aluminum powder coated with polyacrylic acid;
6) And (3) heat treatment: heating at 160deg.C for 30min;
7) 12g of phthalocyanine blue is added into a three-neck flask containing 200g of solvent oil, and 2g of ethylenediamine and 6g of n-butylamine are slowly added;
8) Stirring at 80deg.C for 4 hr, adding the above second step product, and stirring for 12 hr;
9) Filtering, and baking the filtered powder at 200 ℃ for 4 hours to obtain blue powder;
10 Configuration a solution: adding 10.0g of tetraethyl orthosilicate into 40.0g of isopropanol, and uniformly stirring;
11 Configuration B solution: adding 3.0g of ethylenediamine monohydrate into 25.0g of isopropanol, adding 75.0g of water, and uniformly stirring;
12 Adding the product obtained in the third step into a three-neck flask containing 200g of isopropanol, heating to 40 ℃, and simultaneously dropwise adding the solution A and the solution B under stirring;
13 After the A, B solution is added dropwise, stirring is continued for 12 hours at 40 ℃, filtering is carried out, and drying is carried out for 1.5 hours at 200 ℃ to obtain the blue metal pigment.
Wherein the Al powder in the step 1) is 60 mu flake aluminum powder.
As shown in figure 1, the preparation principle diagram of the nonferrous metal pigment is that a coating layer containing carboxyl is formed on the surface of aluminum, a silane coupling agent is used as a bridge, one end of the coating layer is combined with aluminum powder, the other end of the coating layer is combined with carboxyl-containing polymer resin, carboxyl is introduced at the same time, the surface activity of the powder is improved, a colorant and amine are reacted, amine groups are introduced, the two are reacted, the carboxyl and amine groups have high reactivity, the colorant is coated on the surface of the aluminum powder, and finally, a protective layer is coated to prevent the colorant from being desorbed.
Implementation case two:
the preparation method of the nonferrous metal pigment comprises the following preparation steps:
step 7) adding 12g of pigment red 202 into a three-neck flask containing 200g of solvent oil, and slowly adding 2g of ethylenediamine and 6g of n-butylamine;
the rest of the operation steps are as in example one;
obtaining the red metal pigment.
Implementation case three:
the preparation method of the nonferrous metal pigment comprises the following preparation steps:
1) 15g of 45 mu flaky zinc powder is weighed into a three-necked flask;
the rest of the operation steps are as in example one;
to obtain the blue metal pigment.
As shown in FIG. 2, polypropylene is not used in the comparative example, the coloring condition of the pigment coated by the colorant and the metal powder is shown in the upper left corner of the figure, the nonferrous metal pigment prepared by the invention is shown in the lower right corner of the figure, FIG. 2 is a schematic diagram of the comparative example and the nonferrous metal pigment prepared by the invention under a microscope, the pigment of the comparative example is not colored, and the coloring effect of the nonferrous metal pigment prepared by the invention is good after the polypropylene is used.
The main functions of the invention are as follows: the coated high polymer is colorless and transparent, polyacrylic acid is adopted as a raw material, a certain amount of acid is added, polymerization reaction does not occur in the process, only condensation dehydration reaction occurs, the surface film layer is thin, about 120nm is achieved, and the luster of the metal powder is not affected; the coated high polymer does not need to carry out polymerization reaction, and is simple and easy to control; the carboxyl is introduced into the metal powder, and the amino is introduced into the organic colorant, so that the colorant can be tightly coated on the surface of the metal powder; and the tetraethoxysilane is hydrolyzed to form a SiO2 protective layer on the surface to prevent the coloring agent from being desorbed.
In view of the above, after reading the present document, those skilled in the art should make various other corresponding changes without creative mental effort according to the technical scheme and the technical conception of the present invention, which are all within the scope of the present invention.
Claims (10)
1. The preparation method of the nonferrous metal pigment is characterized by comprising the following preparation steps:
1) Dispersing metal powder in a hydrophilic solvent, adding a silane coupling agent, regulating the pH value by using triethanolamine, stirring for 1-8 hours at the temperature of 40-80 ℃, filtering, and cleaning for 1-2 times by using the hydrophilic solvent;
2) Adding hydrophilic solvent, polyacrylic acid and organic acid, and stirring at 40-80 ℃ for 1-8 h to obtain metal powder coated with polyacrylic acid;
3) Adding a colorant into solvent oil to react with amine, adding metal powder coated with polyacrylic acid, heating and stirring for 1-8 h at 40-80 ℃ to obtain nonferrous metal powder;
4) The nonferrous metal powder is coated on the protective layer for treatment, and is washed by hydrophilic solvent for 1 to 2 times, and is subjected to heat treatment for 1 to 4 hours at 160 to 200 ℃ to obtain the nonferrous metal pigment.
2. The method for preparing a nonferrous metal pigment according to claim 1, wherein the metal powder in the step 1) is aluminum powder or zinc powder or an alloy thereof.
3. The method for preparing a nonferrous metal pigment according to claim 1, wherein the silane coupling agent in the step 1) is one or more selected from vinyl, amino, epoxy, mercapto silane coupling agents and titanane coupling agents.
4. A method for preparing a non-ferrous pigment according to claim 3, wherein the pH is adjusted to 8-10 with the triethanol of step 1).
5. The method for preparing a nonferrous metal pigment according to claim 1, wherein the organic acid in the step 2) is one or more of oxalic acid, citric acid, tartaric acid and butane tetracarboxylic acid.
6. The method according to claim 1, wherein the colorant in the step 3) is at least one of azo pigments, phthalocyanine pigments, AS-colored phenol pigments, benzimidazolone pigments, perylene series and pyrene pigments, isoindolinone pigments, quinophthalone pigments.
7. The method for preparing a nonferrous metal pigment according to claim 6, wherein the solvent oil in the step 3) is one of xylene or ethyl acetate.
8. The method for preparing a non-ferrous metal pigment according to claim 7, wherein the amine in the step 3) is one or two of monoethanolamine, diethanolamine, triethanolamine, ammonia water, ethylenediamine, tert-butylamine, and n-butylamine.
9. The method for preparing a nonferrous metal pigment according to claim 1, wherein the coating and protecting treatment in the step 4) comprises the steps of: adding nonferrous metal powder into ethanol, slowly adding the prepared A, B solution, heating at 40-60deg.C, stirring for 8-16 hr, and filtering; the solution A is ethanol solution of tetraethoxysilane, and the solution B is a compound solution of water, organic amine and ethanol.
10. The method for preparing the nonferrous metal pigment according to claim 1, comprising the following steps:
(1) Adding 30g of aluminum powder into a three-necked flask, weighing 200g of isopropanol, regulating the pH value to 8-10 with triethanolamine, slowly adding 12g of vinyltriethoxysilane, heating and stirring at 50 ℃ for 5 hours, filtering after the reaction is finished, and washing with alcohol for 1-2 times to obtain a product of the first step;
(2) The product of the first step was added to a three-necked flask containing 200g of isopropanol and the mixed solution was slowly added: 18.0g polyacrylic acid, 2.0g butane tetracarboxylic acid and proper amount of isopropanol; heating and stirring at 80 ℃ for 6 hours, evaporating the solvent by adopting a rotary evaporator to obtain aluminum powder coated with polyacrylic acid, and heating at 160 ℃ for 30 minutes to obtain a second-step product;
(3) Adding 12g of phthalocyanine blue into a three-neck flask containing 200g of solvent oil, slowly adding 2g of ethylenediamine and 6g of n-butylamine, stirring at 80 ℃ for 4 hours, adding the second-step product, continuously stirring for 12 hours, filtering, and drying the filtered powder at 200 ℃ for 4 hours to obtain a third-step product;
(4) Preparing a solution A: adding 10.0g of tetraethyl orthosilicate into 40.0g of isopropanol, and uniformly stirring; preparing a solution B: adding 3.0g of ethylenediamine monohydrate into 25.0g of isopropanol, adding 75.0g of water, and uniformly stirring;
(5) Adding the product of the third step into a three-neck flask containing 200g of isopropanol, heating to 40 ℃, simultaneously dropwise adding the solution A and the solution B under stirring, continuously stirring at 40 ℃ for 12 hours after the solution A, B is dropwise added, filtering, and drying at 200 ℃ for 1.5 hours to obtain the nonferrous metal pigment.
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