CN109666313A - A kind of preparation method of corrosion resistant hydrate colour aluminium pigment - Google Patents
A kind of preparation method of corrosion resistant hydrate colour aluminium pigment Download PDFInfo
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- CN109666313A CN109666313A CN201910041151.4A CN201910041151A CN109666313A CN 109666313 A CN109666313 A CN 109666313A CN 201910041151 A CN201910041151 A CN 201910041151A CN 109666313 A CN109666313 A CN 109666313A
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- preparation
- flake aluminum
- aluminum
- flake
- pigment
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 112
- 239000000049 pigment Substances 0.000 title claims abstract description 46
- 239000004411 aluminium Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000007797 corrosion Effects 0.000 title claims abstract description 21
- 238000005260 corrosion Methods 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 12
- 238000005253 cladding Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 235000019441 ethanol Nutrition 0.000 claims description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000012065 filter cake Substances 0.000 claims description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- 239000000908 ammonium hydroxide Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000004210 ether based solvent Substances 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 150000002505 iron Chemical class 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003223 protective agent Substances 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007792 addition Methods 0.000 claims description 3
- 150000001722 carbon compounds Chemical class 0.000 claims description 3
- 229940125904 compound 1 Drugs 0.000 claims description 3
- 239000006185 dispersion Substances 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
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical group [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- -1 γ-aminoethylaminopropyl Chemical group 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 3
- 239000011521 glass Substances 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000008439 repair process Effects 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- TWKUSWXMHAMZCC-UHFFFAOYSA-N 5-[aminomethoxy(dimethoxy)silyl]pentan-1-amine Chemical compound NCO[Si](OC)(OC)CCCCCN TWKUSWXMHAMZCC-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 241000532370 Atla Species 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- IAFHSTAZIDDZST-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound C(C)O[Si](O)(O)O.[Si](OCC)(O)(O)O IAFHSTAZIDDZST-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- ZYXNLUSQOKGKDT-UHFFFAOYSA-N iron(2+) oxygen(2-) silane Chemical group [SiH4].[O-2].[Fe+2] ZYXNLUSQOKGKDT-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007740 vapor deposition 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
- 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
- C09C3/06—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
- C09C3/12—Treatment with organosilicon compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of preparation method of corrosion resistant hydrate colour aluminium pigment, step has: the cleaning of flake aluminum and surface active；Flake aluminum coated with silica；It is coated with the flake aluminum surface deposition of iron oxide of silica；The flake aluminum of the deposition of iron oxide is surface-treated, the flake aluminum without microcrack structure cladding of glass-ceramic structures shape layer, as corrosion resistant hydrate colour aluminium pigment is made.The hydrate colour aluminium pigment is the pigment of the more covered composite yarn structures of Al-Si-Fe- polymer, the glass phase compound being made of carbon repairs clad, close glass-ceramic composite construction is constituted, so the colored aluminum pigment being prepared has excellent waterproof, corrosion resistance.The partial size of hydrate colour aluminium pigment has obtained good control, and coating film is complete, and aluminum flake surface is smooth, and clad is close.
Description
Technical field
The present invention relates to a kind of preparation methods of pigment, more particularly to one kind to be used for various superior automobile coating or decoration
The preparation method of the hydrate colour aluminium pigment of the big thickness waterproof heat resistant type of property ink plastics.
Background technique
Colored aluminum pigment is usually that various colored organic or inorganic pigments are deposited on aluminium powder surface and are made.With sheet
Aluminium powder is substrate, deposits certain thickness oxide coating film, opens up aluminium pigment in applicating medium using optical interference phenomena
Existing various colors.Colored aluminum pigment is mainly used for various superior automobile coating or decorative ink plastics etc..
There are two types of the common preparation methods of colored aluminum pigment: one is what is carried out in high-temperature fluidized bed device, patent
It is the depositing metal oxide on flake aluminum by chemical vapor deposition in EP0668329B1, by controlling coating thickness
Etc. parameters, realize color control.This production method, higher cost, yield is small, and there are certain danger.Another is
It carries out in the liquid phase, the method mentioned in patent CN200810163113 is that metal ion is sunk by precipitating reagent sodium hydroxide
Product makes aluminium powder show different colours on passivation flake aluminum using optical interference phenomena.The Aluminium of this method preparation
Pigment is easy to occur to corrode, is broken since aluminium flake coats for a long time in acid condition, causes aluminium pigment rough surface, brightness
Decline, the problem of corrosion resistance difference.
Therefore, how to overcome the colored aluminum pigment of existing liquid phase method preparation, easily corrode, is easily broken and cause aluminium pigment surface
Coarse, brightness decline, corrosion resistance difference defect be industry urgent problem to be solved.
Summary of the invention
The present invention easily corrodes to solve existing colored aluminum pigment, easily broken and cause under aluminium pigment rough surface, brightness
Drop, the problem of corrosion resistance difference propose a kind of system of the hydrate colour aluminium pigment of heat-and corrosion-resistant at low cost, granularity is controllable
Preparation Method.
A kind of preparation method of corrosion resistant hydrate colour aluminium pigment proposed by the present invention, includes the following steps:
Step 1: the cleaning of flake aluminum and surface active；
Step 2: flake aluminum coated with silica；
Step 3: being coated with the flake aluminum surface deposition of iron oxide of silica；
Step 4: the flake aluminum of the deposition of iron oxide is surface-treated, be made glass-ceramic structures shape layer without micro-
Split the flake aluminum of structure cladding, as corrosion resistant hydrate colour aluminium pigment.
Wherein, in the step 1, sheet aluminum paste is dispersed in alcohol ether solvents, ammonium hydroxide is added, is dispersed with stirring, removes
The oil solvent and impurity in aluminium powder are removed, after the completion washing filtering.
Preferably, in the step 2, the flake aluminum handled by step 1 is dispersed in alcohol ether solvents, stirring is simultaneously
Heating, sequentially add deionized water, catalyst, ethyl orthosilicate alcohol ether mixed liquor, heat preservation make its reaction, wash again after the completion
And filter, obtain the flake aluminum of coated with silica.
Preferably, in the step 3, the flake aluminum filter cake obtained by step 2 processing is dispersed in deionized water
In, protective agent, dispersing agent is added, heats up and stirs, trivalent iron salt is added dropwise, and control pH, wash after the completion and filter.
Preferably, in the step 4, the flake aluminum filter cake obtained by step 3 processing is dispersed in alcohol ether solvents
In, ammonium hydroxide, deionized water is added, long chain silane coupling agent processing is added, washing filters after the completion, obtains the glass-pottery
The flake aluminum without microcrack structure cladding of porcelain structure shape layer.
Wherein, the flake aluminum is silver dollar shape, and particle size range is 10 ~ 60 μm；The corrosion resistant hydrate colour aluminium
Pigment, component therein and ratio are as follows: flake aluminum 52 ~ 73%, silica 4 ~ 18%, ferriferous oxide 8 ~ 42%, carbon compound
1~2%。
Preferably, the temperature range in the step 2 is 35 ~ 50 DEG C；In the alcohol ether mixed liquor of the ethyl orthosilicate
Ethyl orthosilicate and the mass ratio of deionized water are 1:1 ~ 1:3, and catalyst and total system volume ratio are 1:40 ~ 1:60, described
Total system volume is the volume of the raw material of all additions and total liquid of solvent composition.The catalyst is ammonium hydroxide, ethylenediamine, two
One of ethylene triamine or triethylene tetramine.
Preferably, the trivalent iron salt is iron chloride or ferric nitrate, described to be warming up to 70 ~ 90 DEG C, control pH value is 3 ~
4.5。
Preferably, the long chain silane are as follows: γ-aminoethyl amino propyl trimethoxy silane, γ-chloropropyl triethoxy
In silane, vinyltriethoxysilane, methyltriethoxysilane, tetraethoxysilane or dimethyl diethoxysilane
It is a kind of.
Preferably, the alcohol ether solvents are one in ethyl alcohol, propyl alcohol, isopropanol, propylene glycol monomethyl ether or butyl glycol ether
Kind.
The present invention coats one layer of fine and close silicon dioxide layer of protection to flake aluminum in advance, improves aluminium powder corrosion resistance,
Then the iron oxide layer of deposition of iron oxide-silane hybrid layer under buffer and protectant double action, high refractive index rises
Arrived colour developing and high heat resistance, organosilan belong to glass phase, as convered structure, to aluminium powder surface it is uncoated on sky
Repairing filling is played the role of in position, formed glass-ceramic structures shape layer without microcrack structure, realize the side cladding on aluminium powder surface
The process that side is repaired.The uniform cladding for being conducive to iron oxide simultaneously further increases aluminium powder surface cladding consistency, improves packet
Cover the corrosion resistance of aluminium powder.It is accumulated followed by subsequent multiple layer metal oxide, passes through metal oxide covering amount
Increase can obtain and obtain different colors.It finally can get the bright Aluminium of waterproof heat resistant at low cost, that granularity is controllable
Pigment.The present invention is carried out in liquid phase environment, highly-safe, and cost is significantly lower than gas-phase deposition process for preparing.Cladding the
Layer of silicon dioxide layer is that reticular structure can effectively take blocking effect to water；Subsequent clad is iron oxide layer and organosilan
Hybrid layer forms fine and close glass-ceramic structures layer, it can be achieved that the big thickness waterproof heat resistant of aluminium powder coats.
Detailed description of the invention
Fig. 1 is the schematic diagram of sheet aluminium flake clad structure；
Fig. 2, Fig. 3, Fig. 4 are the scanning electron microscope (SEM) photograph of the colored aluminum pigment prepared by embodiment 1,2,3 respectively.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention will be further described.
As shown in Figure 1, the flake aluminum clad structure for corrosion resistant hydrate colour aluminium pigment prepared by the present invention is illustrated
Figure: innermost layer is silver dollar shape aluminium flake substrate, and middle layer is silicon dioxide layer, and outermost layer is glass-ceramic structures coloring layer.This hair
Bright hydrate colour aluminium pigment obtained, component therein and ratio are as follows: flake aluminum 52 ~ 73%, silica 4 ~ 18%, iron oxidation
Object 8 ~ 42%, carbon compound 1 ~ 2%.
A kind of preparation method of corrosion resistant hydrate colour aluminium pigment proposed by the present invention, steps are as follows:
Step 1: the cleaning of flake aluminum and surface active
Sheet aluminum paste is dispersed in alcohol ether solvents, ammonium hydroxide is added, is dispersed with stirring, removes the oil solvent and impurity in aluminium powder,
Washing filtering after the completion.The flake aluminum is silver dollar shape, and particle size range is 10 ~ 60 μm.
Step 2: flake aluminum coated with silica
Flake aluminum through over cleaning and surface activation process is dispersed in alcohol ether solvents, stir and is heated up, temperature range is
It 35 ~ 50 DEG C, sequentially adds deionized water, catalyst, the alcohol ether mixed liquor for generating the ethyl orthosilicate of silica can be reacted, protect
Temperature makes its reaction, washs and filters again after the completion, obtains the flake aluminum of coated with silica.The alcohol ether of ethyl orthosilicate mixes
The mass ratio of ethyl orthosilicate and deionized water in liquid is 1:1 ~ 1:3, and catalyst and total system volume ratio are 1:40 ~ 1:
60, which is the volume of the raw material of all additions and total liquid of solvent composition.The catalyst is ammonium hydroxide, second two
One of amine, diethylenetriamine or triethylene tetramine.
Step 3: by flake aluminum surface deposition of iron oxide
The flake aluminum filter cake dispersion for being coated with silica in deionized water, is added protective agent, dispersing agent, is warming up to 70
It ~ 90 DEG C and stirs, the trivalent iron salt for generating ferriferous oxide can be reacted by being added dropwise, and controlling pH value is 3 ~ 4.5, washs and takes out after the completion
Filter.The trivalent iron salt is iron chloride or ferric nitrate.
Step 4: the flake aluminum of the deposition of iron oxide being surface-treated, glass-ceramic structures shape layer is made
The flake aluminum of no microcrack structure cladding, as corrosion resistant hydrate colour aluminium pigment.
The flake aluminum filter cake of surface deposition of iron oxide is dispersed in alcohol ether solvents, ammonium hydroxide, deionized water is added, is added
Long chain silane coupling agent processing, washing filters after the completion, obtains coating without microcrack structure for the glass-ceramic structures shape layer
Flake aluminum.And long chain silane is typical silane coupling agent, be can be selected: γ-aminoethyl amino propyl trimethoxy silane,
γ-chloropropyl triethoxysilane, vinyltriethoxysilane, methyltriethoxysilane, tetraethoxysilane or diformazan
One of base diethoxy silane.The glass-ceramic structures shape layer without microcrack structure by the long chain silane that is added and
Ferriferous oxide reaction generates.
The alcohol ether solvents that the present invention uses be can be in ethyl alcohol, propyl alcohol, isopropanol, propylene glycol monomethyl ether or butyl glycol ether
It is a kind of.
In following embodiment, the solid content of the sheet aluminum paste used is 70%, and average grain diameter is 32 μm, remaining chemistry examination
Agent is that analysis is pure.
Embodiment 1
Step 1: being that the commercially available sheet aluminum paste of 30g is dispersed in 200ml propylene glycol monomethyl ether by solid content, 28% ammonia of 6ml is added
Water after agitator treating is clean, filters；
Step 2: filter cake is dispersed in 240ml propylene glycol monomethyl ether, 45 DEG C of heating is simultaneously stirred, sequentially add 25ml deionized water,
28% ammonium hydroxide of 6ml is then slowly added to the alcohol ether mixed liquor of ethyl orthosilicate, after the reaction was completed, washs and filters to obtain filter cake.
Wherein, the alcohol ether mixed liquor of ethyl orthosilicate is mixed with by 12ml ethyl orthosilicate and 40ml propylene glycol monomethyl ether；
Step 3: the filter cake in second step is added in reaction kettle, 300ml deionized water and protective agent, dispersing agent is added, stirs
It mixes and is warming up to 85 DEG C.The FeCl of the 0.5mol/l of 135ml is slowly added dropwise3Solution, maintaining pH on the way is 4, after being added dropwise to complete, and is used
Deionized water is washed and is filtered；
Step 4: filter cake in third step is dispersed in 180ml propylene glycol monomethyl ether, stir, 28% ammonium hydroxide of 3ml is added and 15g is gone
3ml γ-aminoethyl amino propyl trimethoxy silane is then added in ionized water, and after the reaction was completed, washing filters.
Embodiment 2
Step 1: being that the commercially available sheet aluminum paste of 30g is dispersed in 200ml propylene glycol monomethyl ether by solid content, 28% ammonia of 6ml is added
Water after agitator treating is clean, filters；
Step 2: filter cake is dispersed in 240ml propylene glycol monomethyl ether, 40 DEG C of heating is simultaneously stirred, sequentially add 25ml deionized water,
28% ammonium hydroxide of 6ml is then slowly added to the alcohol ether mixed liquor of ethyl orthosilicate, after the reaction was completed, washs and filters to obtain filter cake；
Wherein, the alcohol ether mixed liquor of ethyl orthosilicate is mixed with by 12ml ethyl orthosilicate and 40ml propylene glycol monomethyl ether；
Step 3: the filter cake in second step is added in reaction kettle, 300ml deionized water and protective agent, dispersing agent is added, stirs
It mixes and is warming up to 85 DEG C.The FeCl of the 0.5mol/l of 270ml is slowly added dropwise3Solution, maintaining pH on the way is 4, after being added dropwise to complete, and is used
Deionized water is washed and is filtered；
Step 4: filter cake in third step is dispersed in 180ml propylene glycol monomethyl ether, stir, 28% ammonium hydroxide of 3ml is added and 15g is gone
3ml γ-chloropropyl triethoxysilane is then added in ionized water, and after the reaction was completed, washing filters.
Embodiment 3
Step 1: being that the commercially available sheet aluminum paste of 30g is dispersed in 200ml propylene glycol monomethyl ether by solid content, 28% ammonia of 6ml is added
Water after agitator treating is clean, filters；
Step 2: filter cake is dispersed in 240ml propylene glycol monomethyl ether, 50 DEG C of heating is simultaneously stirred, sequentially add 25ml deionized water,
28% ammonium hydroxide of 6ml is then slowly added to the alcohol ether mixed liquor of ethyl orthosilicate, after the reaction was completed, washs and filters to obtain filter cake；
Wherein, the alcohol ether mixed liquor of ethyl orthosilicate is mixed with by 12ml ethyl orthosilicate and 40ml propylene glycol monomethyl ether；
Step 3: the filter cake in second step is added in reaction kettle, 300ml deionized water and protective agent, dispersing agent is added, stirs
It mixes and is warming up to 85 DEG C.The Fe (N0) of the 1mol/l of 215ml is slowly added dropwise3Solution, maintaining pH on the way is 4, after being added dropwise to complete, and is used
Deionized water is washed and is filtered；
Step 4: filter cake in third step is dispersed in 180ml propylene glycol monomethyl ether, stir, 28% ammonium hydroxide of 3ml is added and 15g is gone
3ml γ-aminoethyl amino propyl trimethoxy silane is then added in ionized water, and after the reaction was completed, washing filters, after obtaining cladding
Colored aluminum pigment.
The colored aluminum pigment that embodiment obtains is coated on colour atla with lacquering, with multi-angle spectrophotometer data measured
It is as follows:
Metal dynamic value (FI) known to upper table data through colored aluminum pigment prepared by the present invention is high, has strong metal.
The brightness (L15, L45) in 15 °, 45 ° directions is larger, and the colored aluminum pigment of a/b value difference display preparation shows not
Same color.Wherein, L15, L45 respectively represent 15 °, the brightness on 45 ° of directions；FI indicates metal dynamic value；A value indicates red -- it is green
Transition, b value indicates blue -- yellow transition.
Elemental analysis is carried out to the colored aluminum pigment prepared in embodiment 1.It is as follows:
| Element | Element term | Mass percent |
| Al | Aluminium | 60.82 |
| Si | Silicon | 16.08 |
| C | Carbon | 9.48 |
| O | Oxygen | 9.27 |
| Fe | Iron | 4.34 |
| It is other | It is other | Surplus |
By knowing in table, the colored aluminum pigment that the present invention prepares is the pigment of the more covered composite yarn structures of Al-Si-Fe- polymer, by
The glass phase compound of carbon composition repairs clad, constitutes close glass-ceramic composite construction, so system
Standby obtained colored aluminum pigment has excellent waterproof, corrosion resistance.As shown in Fig. 2 ~ Fig. 4, to be coated under SEM observation
The pattern on aluminium powder surface afterwards.By scanning electron microscope (SEM) photograph, it can be seen that, colored aluminum pigment prepared by the present invention, partial size has been obtained well
Control, coating film is complete, and aluminum flake surface is smooth, and clad is close.
By above-mentioned picture and comparative illustration it is found that colored aluminum pigment prepared by the present invention is that Al-Si-Fe- polymer wraps more
The pigment for covering composite construction, the good dispersion in water phase, soilless sticking phenomenon, aluminium powder are not etched, and ferric oxide particles material is in sheet
Deposition compact on aluminium powder and uniformly；Display is coated on colour atla, the colored aluminum pigment of this patent published method preparation is in tone
The upper colored aluminum pigment effect with vapor deposition preparation differs smaller, is greatly improved in brightness.
Embodiment described above is primarily to illustrate creating conception of the invention, it is noted that for this field
Those of ordinary skill for, without departing from the inventive concept of the premise, various modifications and improvements can be made, these are all
It belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of corrosion resistant hydrate colour aluminium pigment, includes the following steps:
Step 1: the cleaning of flake aluminum and surface active；
Step 2: flake aluminum coated with silica；
Step 3: being coated with the flake aluminum surface deposition of iron oxide of silica；
Step 4: the flake aluminum of the deposition of iron oxide is surface-treated, be made glass-ceramic structures shape layer without micro-
Split the flake aluminum of structure cladding, as corrosion resistant hydrate colour aluminium pigment.
2. preparation method as described in claim 1, which is characterized in that in the step 1, sheet aluminum paste is dispersed in alcohol
In ether solvents, ammonium hydroxide is added, is dispersed with stirring, remove the oil solvent and impurity in aluminium powder, after the completion washing filtering.
3. preparation method as described in claim 1, which is characterized in that in the step 2, the piece that step 1 is handled will be passed through
Shape aluminium powder is dispersed in alcohol ether solvents, is stirred and is warming up to, sequentially add deionized water, catalyst, ethyl orthosilicate alcohol ether
Mixed liquor, heat preservation make its reaction, wash and filter again after the completion, obtain the flake aluminum of coated with silica.
4. preparation method as described in claim 1, which is characterized in that in the step 3, will be obtained by step 2 processing
The dispersion of flake aluminum filter cake in deionized water, protective agent, dispersing agent is added, heats up and stirs, trivalent iron salt is added dropwise, and controls
PH processed, washs after the completion and filters.
5. preparation method as described in claim 1, which is characterized in that in the step 4, will be obtained by step 3 processing
Flake aluminum filter cake be dispersed in alcohol ether solvents, be added ammonium hydroxide, deionized water, be added long chain silane coupling agent processing, complete
Washing filters afterwards, obtains the flake aluminum without microcrack structure cladding of the glass-ceramic structures shape layer.
6. preparation method as described in claim 1, which is characterized in that the flake aluminum is silver dollar shape, and particle size range is
10~60μm；The corrosion resistant hydrate colour aluminium pigment, component therein and ratio are as follows: flake aluminum 52 ~ 73%, silica
4 ~ 18%, ferriferous oxide 8 ~ 42%, carbon compound 1 ~ 2%.
7. preparation method as claimed in claim 3, which is characterized in that the temperature range in the step 2 is 35 ~ 50 DEG C；Just
Silester and the mass ratio of deionized water are 1:1 ~ 1:3, and catalyst and total system volume ratio are 1:40 ~ 1:60, described total
System volume is the volume of the raw material of all additions and total liquid of solvent composition；The catalyst is ammonium hydroxide, ethylenediamine, diethyl
One of alkene triamine or triethylene tetramine.
8. preparation method as claimed in claim 4, which is characterized in that the trivalent iron salt is iron chloride or ferric nitrate, institute
It states and is warming up to 70 ~ 90 DEG C, control pH value is 3 ~ 4.5.
9. preparation method as claimed in claim 5, which is characterized in that the long chain silane are as follows: γ-aminoethylaminopropyl three
Methoxy silane, γ-chloropropyl triethoxysilane, vinyltriethoxysilane, methyltriethoxysilane, tetraethoxy
One of silane or dimethyl diethoxysilane.
10. such as claim 2,3 and 5 described in any item preparation methods, which is characterized in that the alcohol ether solvents be ethyl alcohol,
One of propyl alcohol, isopropanol, propylene glycol monomethyl ether or butyl glycol ether.
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| CN111100484A (en) * | 2019-12-27 | 2020-05-05 | 河南兴安新型建筑材料有限公司 | Nano SiO2Preparation method of coated flaky pigment Al powder |
| CN113789070A (en) * | 2021-09-16 | 2021-12-14 | 山东银箭金属颜料有限公司 | Wet production process of aluminum powder pigment |
| CN115011237A (en) * | 2022-06-30 | 2022-09-06 | 上海三银涂料科技股份有限公司 | Color and storage stable effect pigment building coating and preparation method thereof |
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| CN115011237A (en) * | 2022-06-30 | 2022-09-06 | 上海三银涂料科技股份有限公司 | Color and storage stable effect pigment building coating and preparation method thereof |
| CN115011237B (en) * | 2022-06-30 | 2023-03-10 | 上海三银涂料科技股份有限公司 | Color and storage stable effect pigment building coating and preparation method thereof |
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Application publication date: 20190423 |