CN109705621A - A kind of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment and preparation method thereof - Google Patents
A kind of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment and preparation method thereof Download PDFInfo
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- CN109705621A CN109705621A CN201910065384.8A CN201910065384A CN109705621A CN 109705621 A CN109705621 A CN 109705621A CN 201910065384 A CN201910065384 A CN 201910065384A CN 109705621 A CN109705621 A CN 109705621A
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- Prior art keywords
- bismuth vanadate
- yellow pigment
- molybdenum bismuth
- vanadate yellow
- silicon dioxide
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 120
- BYUANIDVEAKBHT-UHFFFAOYSA-N [Mo].[Bi] Chemical compound [Mo].[Bi] BYUANIDVEAKBHT-UHFFFAOYSA-N 0.000 title claims abstract description 83
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000001052 yellow pigment Substances 0.000 title claims abstract description 80
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 71
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000049 pigment Substances 0.000 claims abstract description 25
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 23
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 23
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 23
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 14
- 239000011733 molybdenum Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 6
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 5
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 5
- 230000002572 peristaltic effect Effects 0.000 claims description 5
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical group [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 5
- 241000219307 Atriplex rosea Species 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- IQXJCCZJOIKIAD-UHFFFAOYSA-N 1-(2-methoxyethoxy)hexadecane Chemical compound CCCCCCCCCCCCCCCCOCCOC IQXJCCZJOIKIAD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 claims description 2
- 229950009789 cetomacrogol 1000 Drugs 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 229940085675 polyethylene glycol 800 Drugs 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 208000016261 weight loss Diseases 0.000 claims description 2
- 230000004580 weight loss Effects 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims 1
- 238000010931 ester hydrolysis Methods 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000008187 granular material Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000007704 wet chemistry method Methods 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- WUJISAYEUPRJOG-UHFFFAOYSA-N molybdenum vanadium Chemical compound [V].[Mo] WUJISAYEUPRJOG-UHFFFAOYSA-N 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 229910015667 MoO4 Inorganic materials 0.000 description 2
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 2
- 229910019501 NaVO3 Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 229940040544 bromides Drugs 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229940068984 polyvinyl alcohol Drugs 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a kind of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment, by SiO2Transparent shell wrapping layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted.In addition, also disclosing the preparation method of above-mentioned superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment.Superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present invention, by silica as transparent package shell, Coated molybdenum bismuth vanadate yellow pigment, significantly improves the heat-resisting quantity and acid resistance of molybdenum bismuth vanadate yellow pigment, and can satisfy higher use demand.The present invention uses wet chemistry method ultra-fine molybdenum pucherite particle obtained under liquid-phase condition, Silica-coated is carried out before undried, calcining, avoid the reunion and agglomeration of powder pigment, granules of pigments partial size it is thin and uniformly, good dispersion, and without expensive equipment, simple process is easy to operate, production cost is low, facilitates promotion and application.
Description
Technical field
The present invention relates to inorganic pigment technical field more particularly to a kind of coated molybdenum bismuth vanadate yellow pigment and its preparations
Method.
Background technique
Cadmium yellow (CdS) and chrome yellow (PbCrO4、BaCrO4), have many advantages, such as bright-colored, strong covering power, cheap, is
Instantly the Inorganic yellow pigment generally used on the market, and applicating history is long, use scope is wide.However, due to contained
Cadmium, lead and chromium (VI) poisoning metal element can seriously endanger human health and pollute environment, therefore, develop novel environment-friendly type yellow
Color pigment is not only imperative to replace, more significant.
Molybdenum pucherite (general formula BiVO4·nBi2MoO6, 0.2≤n≤2) and it is a kind of Advanced Inorganic that novel environment friendly is nontoxic
Yellow uitramarine, tone can be regulated and controled by the size of n value, and when n value is gradually increased, tone is yellow by red phase Huang Xiang Lvxiang
Transformation, as n=0.75, the pigment yellow PY184 that the BASF AG as to have appeared on the market registers on pigment index, it is by four directions
The BiVO of crystal form4With the Bi of rhombic form2MoO6The Yellow organic dye of the bright green of composition, strong covering power.
Currently, the manufacturing method of molybdenum bismuth vanadate yellow pigment has calcination and precipitating-calcination method.Calcination is
By corresponding oxide or the salt that corresponding oxide can be generated through thermal decomposition by composition ingredient, after solid-phase ball milling mixes, in height
The lower calcining of temperature.Precipitating-calcination method is first to dissolve corresponding water-soluble each salt ingredient, under the conditions ofs corresponding temperature and pH etc.
Them are made to generate oxides or hydroxide gel precipitating, then in about 600 DEG C of temperature after the precipitating of generation is washed, dried
Lower calcining, ultimately forms the BiVO mutually adjoined4And Bi2MoO6Two-phase crystallization.Above two method finally must wet-milling, suction filtration
To reach corresponding granularity, not only technique is cumbersome, but also gained granules of pigments granularity is still larger, it is difficult to meet higher using need
It asks.
In addition, the above-mentioned pigment of the prior art is intolerant to strong acid, and when being calcined to 600 DEG C or more, pigment can make because of sintering
It darkens, loses glassy yellow, thus cannot be used under strong acid environment, also may not apply to the more demanding neck of temperature tolerance
Domain, such as engineering plastics, high-temperature coatings, glass ink, ceramic paint.It therefore, is the service performance for improving pigment, to molybdenum vanadic acid
Bismuth yellow uitramarine carries out the hot spot that surface modification treatment has become research and development, and the method mainly used at present is in the pigment
Surface deposit colorless inorganic matter protective film, such as zirconium silicate, phosphate and various oxides, but pigment granules and nothing in the prior art
Machine protective film be only mutual mixing and absorption together, protective film is not fine and close enough, therefore the effect is unsatisfactory.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of superfine silicon dioxide coated molybdenum pucherites
Yellow uitramarine, by silica as transparent package shell, Coated molybdenum bismuth vanadate yellow pigment, to significantly improve molybdenum vanadium
The heat-resisting quantity and acid resistance of sour bismuth yellow uitramarine, and meet higher use demand.Another object of the present invention is to provide
The preparation method of above-mentioned superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment, first by being made ultra-fine under liquid-phase condition
Molybdenum bismuth vanadate yellow pigment carries out Silica-coated then without drying and calcination immediately, causes to obtain ultra-fine, package
Close molybdenum bismuth vanadate yellow pigment.
The purpose of the present invention is achieved by the following technical programs:
A kind of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment provided by the invention, by SiO2Transparent shell package
Layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted.The superfine silicon dioxide coated molybdenum vanadic acid
Bismuth yellow uitramarine average particle size is 0.5~1.0 μm, wherein the SiO2The average thickness of transparent shell wrapping layer be 40~
70nm。
In above scheme, its red scale value of yellow uitramarine of the present invention a*≤- 3.0, yellow value degree b* >=65；In air atmosphere
Under in 1150 DEG C calcining after still be in bright-coloured bright yellow, red scale value a*≤0, yellow value degree b* >=63.The yellow uitramarine warp
Concentration is that the salt acid soak 0.5h of 2mol/L is non-discolouring, weight-loss ratio < 20wt%.
Another object of the present invention is achieved by the following technical programs:
The preparation method of above-mentioned superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment provided by the invention, including it is following
Step:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by bismuth nitrate (Bi (NO3)3·5H2O it) is dissolved in nitric acid solution, after dispersing agent stirring and dissolving is added, obtains
To A liquid；
Molybdenum source and vanadium source are dissolved in sodium hydroxide solution by (1-2), according to molar ratio Mo: V: Bi=2.50~2.80:
0.60~0.64: 1, obtain B liquid；
(1-3) at room temperature mixes the A liquid and B liquid, and adjusting solution system pH value is 6.0~6.5, is stirring mixing water
It is reacted under the conditions of bath, is then filtered, washed, obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake；
(2)SiO2Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
The ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in dehydrated alcohol by (2-1), according to molar ratio Si: Bi=
Be added tetraethyl orthosilicate (C at 3~4: 18H20O4Si), and concentrated ammonia liquor is added, is distilled under water bath condition by being added dropwise stirring
Water hydrolyzes tetraethyl orthosilicate, is aged, is filtered after being added dropwise to complete, and SiO is obtained2Primary package molybdenum bismuth vanadate yellow pigment filter
Cake；
(2-2) is by the SiO2The operation that primary package molybdenum bismuth vanadate yellow pigment filter cake repeats step (2-1) it is primary or
It is wrapped up again more than once, obtains SiO2Molybdenum bismuth vanadate yellow pigment filter cake is wrapped up again；
(2-3) is by the SiO2Package molybdenum bismuth vanadate yellow pigment filter cake is dried, is calcined again, is obtained after cooling
Superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment.
Preparation method of the present invention uses wet chemistry method that the ultra-fine molybdenum pucherite of glassy yellow is made under liquid-phase condition first
(Bi0.82V0.45Mo0.55O4), then without drying and calcination, using the hydrolysis of tetraethyl orthosilicate, in molybdenum pucherite table
Bread wraps up in fine and close silica, significantly improves the heat-resisting quantity and acid resistance of pigment, ultra-fine, high temperature resistant is resistance to obtain
Sour molybdenum bismuth vanadate yellow pigment.
Further, dispersing agent described in preparation method of the present invention is polyvinylpyrrolidone, neopelex, ten
Six alkyl trimethyl ammonium bromides, polyvinyl alcohol, polyethylene glycol-800, cetomacrogol 1000, dosage be bismuth nitrate 5~
8wt%.The molybdenum source is ammonium molybdate [(NH4)6Mo7O24·4H2O], molybdic acid disodium (Na2MoO4·2H2O)；The vanadium source is inclined
Sodium vanadate (NaVO3), ammonium metavanadate (NH4VO3)。
Further, in step (1-1), (1-2) described in preparation method of the present invention nitric acid and sodium hydroxide solution concentration
For 1.5~2.5mol/L；Step (1-3) the water-bath condition are as follows: 60~80 DEG C of temperature, 1.5~2.0h of reaction time.Institute
State dehydrated alcohol (C in step (2-1)2H6O dosage) is according to molar ratio O: Bi=150~250: 1；The concentrated ammonia liquor
(NH3·H2O dosage) is according to molar ratio N: Si=2.8~3.3: 1；Distilled water (the H2O dosage) is according to mass ratio
Water: tetraethyl orthosilicate=20~25: 1, be added dropwise using multi-channel peristaltic pump, each channel drip rate be 0.3~
0.4mL/min；0.5~the 1.0h of digestion time.Drying temperature is 80~100 DEG C in the step (2-3), and calcination temperature is
450~550 DEG C.
The invention has the following advantages:
(1) superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present invention, granularity is small, average particle size be 0.5~
1.0 μm, it can satisfy higher use demand；Its inclusion enclave silica, while the corrosion of extraneous strong acid can be completely cut off, a side
Face significantly reduces the volatilization of Bi element at high temperature in pigment, it is ensured that tetragonal phase molybdenum pucherite
(Bi0.82V0.45Mo0.55O4) crystal phase stablize, to greatly improve the high-temperature stability of pigment；On the other hand make pigment in height
Colorant sintering discoloration can be prevented under temperature.Therefore, the resistance to strong acid of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present invention
While, also it can still keep bright-colored after 1150 DEG C of high-temperature calcinations, be greatly expanded its application field.
(2) present invention use wet chemistry method ultra-fine molybdenum pucherite particle obtained under liquid-phase condition, it is undried, forge
Silica-coated is carried out before burning, and avoids powder pigment reunion as caused by drying, calcining；Simultaneously as titanium dioxide
The package of silicon makes pigment not agglomerate after 450~550 DEG C of calcinings, and therefore, granules of pigments is very thin, uniform particle sizes, good dispersion,
It does not need that nanoscale yellow uitramarine powder can be obtained through subsequent wet-milling, suction filtration and stoving process.
(3) preparation method of the present invention is without expensive equipment, and simple process is easy to operate, and influence factor is easy to control, and calcines
Temperature is low, saves energy consumption, and used dehydrated alcohol is reusable, and production cost is low, facilitates promotion and application.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 be ultra-fine molybdenum bismuth vanadate yellow pigment filter cake made from one step of the embodiment of the present invention (1-3) after drying
Transmission electron microscope (TEM) photo；
Fig. 2 is the transmission electron microscope of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one
(TEM) photo；
Fig. 3 is the XRD spectrum of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from various embodiments of the present invention；
Fig. 4 is that the FTIR spectrum (FTIR) of forward and backward pigment is wrapped up in the embodiment of the present invention one (before package: for step
Suddenly ultra-fine molybdenum bismuth vanadate yellow pigment filter cake made from (1-3) is through drying, 500 DEG C of calcined samples；After package: for step
Superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from (2-3)).
Specific embodiment
Embodiment one:
A kind of preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present embodiment, its step are as follows:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by 9.70g Bi (NO3)3·5H2O is dissolved in the nitric acid solution that 100mL concentration is 2.0mol/L, is added
After polyethylene of dispersing agent pyrrolidones 0.60g stirring and dissolving, A liquid is obtained；
(1-2) is by 9.76g ammonium molybdate [(NH4)6Mo7O24·4H2O] and 1.48g sodium metavanadate (NaVO3) it is dissolved in 100mL
Concentration is to obtain B liquid in the sodium hydroxide solution of 2.0mol/L；
(1-3) at room temperature mixes above-mentioned A liquid and B liquid, is 6.0 with sodium hydroxide solution regulation system pH value, is stirring
It mixes and stirs under the conditions of bath temperature is 70 DEG C and reacts 2.0h, after filtering, washed once first with a large amount of distilled water, then with anhydrous second
Alcohol washed once, and obtaining ultra-fine molybdenum bismuth vanadate yellow pigment filter cake, (detection after drying is as shown in Figure 1, its good dispersion, is
Irregular blocky, partial size is 100~200nm)；
(2)SiO2Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
Above-mentioned ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in 200mL dehydrated alcohol by (2-1), and 16.5g is being added just
Tetraethyl orthosilicate and 14mL concentrated ammonia liquor are slowly dripped under the conditions of stirring and bath temperature are 45 ± 2 DEG C using multi-channel peristaltic pump
280mL distilled water is added to hydrolyze tetraethyl orthosilicate, the rate of dripping in each channel is 0.4mL/min, 45 after being added dropwise to complete
It is aged 1.0h under ± 2 DEG C of water-baths, is filtered, SiO is obtained2Primary package molybdenum bismuth vanadate yellow pigment filter cake；
(2-2) is by above-mentioned SiO2The operation that primary package molybdenum bismuth vanadate yellow pigment filter cake repeats step (2-1) is primary, i.e.,
Secondary capsulation is carried out, SiO is obtained2Secondary capsulation molybdenum bismuth vanadate yellow pigment filter cake；
(2-3) is by above-mentioned SiO2After secondary capsulation molybdenum bismuth vanadate yellow pigment filter cake is dried at a temperature of 80 DEG C, at 500 DEG C
Temperature lower calcination, heating rate are 5 DEG C/min, soaking time 1h, obtain superfine silicon dioxide coated molybdenum vanadium after cooling
Sour bismuth (Bi0.82V0.45Mo0.55O4) yellow uitramarine.
Embodiment two:
A kind of preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present embodiment, its step are as follows:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by 7.30g Bi (NO3)3·5H2O is dissolved in the nitric acid solution that 100mL concentration is 1.5mol/L, is added
After polyethylene of dispersing agent alcohol 0.45g stirring and dissolving, A liquid is obtained；
(1-2) is by 10.0g molybdic acid disodium (Na2MoO4·2H2) and 1.06g ammonium metavanadate (NH O4VO3) to be dissolved in 100mL dense
Degree is to obtain B liquid in the sodium hydroxide solution of 1.5mol/L；
(1-3) at room temperature mixes above-mentioned A liquid and B liquid, is 6.5 with sodium hydroxide solution regulation system pH value, is stirring
It mixes and stirs under the conditions of bath temperature is 70 DEG C and reacts 2.0h, after filtering, washed once first with a large amount of distilled water, then with anhydrous second
Alcohol washed once, and obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake；
(2)SiO2Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
Above-mentioned ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in 200mL dehydrated alcohol by (2-1), and the positive silicon of 9.4g is added
Sour tetra-ethyl ester and 10mL concentrated ammonia liquor are slowly added dropwise under the conditions of stirring and bath temperature are 45 ± 2 DEG C using multi-channel peristaltic pump
280mL distilled water hydrolyzes tetraethyl orthosilicate, and the rate of dripping in each channel is 0.3mL/min, 45 ± 2 after being added dropwise to complete
It is aged 1.0h under DEG C water-bath, is filtered, SiO is obtained2Primary package molybdenum bismuth vanadate yellow pigment filter cake；
(2-2) is by above-mentioned SiO2The operation that primary package molybdenum bismuth vanadate yellow pigment filter cake repeats step (2-1) carries out one
Secondary, i.e. secondary capsulation obtains SiO2Secondary capsulation molybdenum bismuth vanadate yellow pigment filter cake；
(2-3) is by above-mentioned SiO2After secondary capsulation molybdenum bismuth vanadate yellow pigment filter cake is dried at a temperature of 90 DEG C, at 450 DEG C
Temperature lower calcination, heating rate are 5 DEG C/min, soaking time 1h, obtain superfine silicon dioxide coated molybdenum vanadium after cooling
Sour bismuth (Bi0.82V0.45Mo0.55O4) yellow uitramarine.
Embodiment three:
A kind of preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present embodiment, not with embodiment one
It is with place:
Vanadium source is ammonium metavanadate (NH in step (1-2)4VO3), dosage 1.42g；
Bath temperature is 65 DEG C in step (1-3)；
The dosage of tetraethyl orthosilicate is 12.4g in step (2-1), and the dosage of concentrated ammonia liquor is 10.5mL, the use of distilled water
Amount is 210mL.
Example IV:
A kind of preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present embodiment, not with embodiment one
It is with place:
Molybdenum source is molybdic acid disodium (Na in step (1-2)2MoO4·2H2O), dosage 13.38g；Vanadium source is ammonium metavanadate
(NH4VO3), dosage 1.42g；
The dosage of tetraethyl orthosilicate is 14.4g in step (2-1), and the dosage of concentrated ammonia liquor is 12.3mL, the use of distilled water
Amount is 250mL, and the rate of dripping in each channel of multi-channel peristaltic pump is 0.35mL/min；
Calcination temperature is 450 DEG C in step (2-3).
Embodiment five:
A kind of preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment of the present embodiment, not with embodiment two
It is with place:
Bi (NO in step (1-1)3)3·5H2The dosage of O is 9.70g；
Molybdic acid disodium (Na in step (1-2)2MoO4·2H2O dosage) is 12.9g；Ammonium metavanadate (NH4VO3) dosage
For 1.45g；
The dosage of tetraethyl orthosilicate is 12.50g in step (2-1), and the dosage of concentrated ammonia liquor is 15mL, the dosage of distilled water
For 280mL.
As shown in Fig. 2, superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one, by
SiO2Transparent shell wrapping layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted, and dispersibility is preferable,
In irregular shape, partial size is 0.5~1.0 μm, wherein SiO2The average thickness of transparent shell wrapping layer is 40~70nm.
From figure 3, it can be seen that superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention is
Tetragonal phase Bi0.82V0.45Mo0.55O4(PDF 85-0631)；In addition, the crystal phase of wrapping layer silica is not observed in figure.
As shown in figure 4, sample surfaces exist after the spectral line of two samples of comparison package front and back can be seen that package by taking embodiment one as an example
A large amount of Si-OH group, the crystal phase of wrapping layer silica is not observed in conjunction with Fig. 3, illustrates transparent shell wrapping layer SiO2
It is unformed.
Performance test:
1, colorimetric parameter test: using Hangzhou Yan Te Science and Technology Ltd. production the full-automatic chromascope of YT-ACM402 into
Row test: simulation D65 working flare illumination, using d/0 illuminating watches geometrical condition, diffusion bulb diameter is 150mm, tests bore dia
For 30mm, test wavelength range is visible light (400~700nm), surveys the colorimetric parameter CIE-L*a*b* of its pigment, wherein L* generation
For table by black (0) to white (100), a* indicates that, by green (-) to red (+), b* is indicated by blue (-) to yellow (+).
2, acid resistance is tested: accurately being weighed 0.1000g colorant and is placed in dry centrifuge tube, 10mL concentration, which is added, is
Clear liquid is carefully toppled over discarding by the salt acid soak half an hour of 2mol/L, centrifugation, twice with alcohol centrifuge washing, drying weighing, meter
Calculate acid etching vector (wt%)=(G0-G1)/G0× 100%, wherein G0、G1The respectively forward and backward pigment weight of salt acid soak.
The colorimetric parameter such as table 1 of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from various embodiments of the present invention
It is shown.
With the yellow uitramarine of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake after drying made from one step of embodiment (1-3)
(the ultra-fine molybdenum bismuth vanadate yellow pigment not wrapped up) as a comparison case.Obtained by the comparative example and various embodiments of the present invention
Yellow uitramarine acid resistance test value it is as shown in table 2, calcined colorimetric parameter is as shown in table 3 in air atmosphere.
The colorimetric parameter of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment made from 1 various embodiments of the present invention of table
The acid resistance test value of 2 various embodiments of the present invention of table and comparative example
3 various embodiments of the present invention of table and the comparative example calcined colorimetric parameter in air atmosphere
Claims (10)
1. a kind of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment, it is characterised in that: by SiO2Transparent shell wrapping layer,
And the molybdenum bismuth vanadate yellow powder pigment particle being coated in it is constituted.
2. superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 1, it is characterised in that: described ultra-fine
Silica-coated type molybdenum bismuth vanadate yellow pigment average particle size is 0.5~1.0 μm, wherein the SiO2Transparent shell package
The average thickness of layer is 40~70nm.
3. superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 1 or claim 2, it is characterised in that: described
Its red scale value of yellow uitramarine a*≤- 3.0, yellow value degree b* >=65；In air atmosphere still in bright-coloured bright after 1150 DEG C of calcinings
Yellow, red scale value a*≤0, yellow value degree b* >=63.
4. superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 1 or claim 2, it is characterised in that: described
Yellow uitramarine is non-discolouring through the salt acid soak 0.5h that concentration is 2mol/L, weight-loss ratio < 20wt%.
5. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment, feature described in one of claim 1-4
Be the following steps are included:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
Bismuth nitrate is dissolved in nitric acid solution by (1-1), after dispersing agent stirring and dissolving is added, obtains A liquid；
Molybdenum source and vanadium source are dissolved in sodium hydroxide solution by (1-2), according to molar ratio Mo: V: Bi=2.50~2.80: 0.60
~0.64: 1, obtain B liquid；
(1-3) at room temperature mixes the A liquid and B liquid, and adjusting solution system pH value is 6.0~6.5, in stirring and water-bath item
It is reacted under part, is then filtered, washed, obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake；
(2)SiO2Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
The ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in dehydrated alcohol by (2-1), according to molar ratio Si: Bi=3~4
: 1 is added tetraethyl orthosilicate, and concentrated ammonia liquor is added, and makes positive silicic acid tetrem by the way that distilled water is added dropwise under water bath condition stirring
Ester hydrolysis is aged after being added dropwise to complete, is filtered, and SiO is obtained2Primary package molybdenum bismuth vanadate yellow pigment filter cake；
(2-2) is by the SiO2The operation that primary package molybdenum bismuth vanadate yellow pigment filter cake repeats step (2-1) carries out primary or one
It is wrapped up again more than secondary, obtains SiO2Molybdenum bismuth vanadate yellow pigment filter cake is wrapped up again；
(2-3) is by the SiO2Package molybdenum bismuth vanadate yellow pigment filter cake is dried, is calcined again, is obtained after cooling ultra-fine
Silica-coated type molybdenum bismuth vanadate yellow pigment.
6. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature
Be: the dispersing agent is polyvinylpyrrolidone, neopelex, cetyl trimethylammonium bromide, polyethylene
Alcohol, polyethylene glycol-800, cetomacrogol 1000, dosage are 5~8wt% of bismuth nitrate.
7. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature
Be: the molybdenum source is ammonium molybdate, molybdic acid disodium；The vanadium source is sodium metavanadate, ammonium metavanadate.
8. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature
Be: the concentration of nitric acid and sodium hydroxide solution is 1.5~2.5mol/L in the step (1-1), (1-2)；Step (the 1-
3) water-bath condition are as follows: 60~80 DEG C of temperature, 1.5~2.0h of reaction time.
9. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature
Be: the dosage of dehydrated alcohol is according to molar ratio O: Bi=150~250: 1 in the step (2-1)；The use of the concentrated ammonia liquor
Amount is according to molar ratio N: Si=2.8~3.3: 1；The dosage of the distilled water is according to quality than water: tetraethyl orthosilicate=
20~25: 1, it is added dropwise using multi-channel peristaltic pump, the rate of dripping in each channel is 0.3~0.4mL/min；The digestion time
For 0.5~1.0h.
10. the preparation method of superfine silicon dioxide coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature
Be: drying temperature is 80~100 DEG C in the step (2-3), and calcination temperature is 450~550 DEG C.
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