CN103523831A - Preparation method of bismuth vanadate - Google Patents
Preparation method of bismuth vanadate Download PDFInfo
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- CN103523831A CN103523831A CN201210228971.2A CN201210228971A CN103523831A CN 103523831 A CN103523831 A CN 103523831A CN 201210228971 A CN201210228971 A CN 201210228971A CN 103523831 A CN103523831 A CN 103523831A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of bismuth vanadate. The preparation method comprises the following steps of: dissolving Bi2O3 into nitric acid to prepare a Bi(NO3)3 solution; preparing a NaVO3 mixed solution from NH4VO3, Na5P3O10, Na2MoO4, pure water and NaOH; adding the Bi(NO3)3 solution into the NaVO3 mixed solution, adjusting the initial pH value of the reaction solution after adding the Bi(NO3)3 solution, and stirring; after reaction, performing aging treatment; washing, separating and drying the BiVO4 precipitate obtained by the reaction to obtain dry BiVO4 powder; calcining the dry BiVO4 powder to obtain sintered BiVO4 powder; performing ball milling on the sintered BiVO4 powder; drying the BiVO4 powder subjected to ball milling to obtain a BiVO4 product. The preparation method of bismuth vanadate is short in preparation cycle and simple in process, and the prepared product is excellent in performance.
Description
Technical field
The present invention relates to a kind of preparation method of mineral dye, relate in particular to a kind of preparation method of pucherite.
Background technology
BiVO
4that yellow ultramarine has is nontoxic, good weatherability, color and luster is bright and environment amenable premium properties, it is a kind of novel pigment that has rosy prospect, thereby can be used to replace the pigment contain the poisonous elements such as lead, cadmium, chromium, be applied to the exigent occasion of properties such as painted of automobile finish, industrial coating, rubber item, plastics and printing-ink.
BiVO
4as a kind of lovely luster, functional, leaded, not nontoxic yellow novel environment friendly pigment, because its excellent stability has a wide range of applications.BiVO
4mainly contain cubic Zircon cut, monocline scheelite type structure and cubic scheelite-type structure, wherein oblique system BiVO
4be suitable as yellow ultramarine.
BiVO
4preparation method mainly contain solid phase method, sol-gel method, chemical coprecipitation, hydrothermal synthesis method, organometallics thermal decomposition method, liquid-phase precipitation method and microemulsion method etc.Above preparation method all can prepare jonquilleous BiVO
4pigment, but or complicated process of preparation; Or the inadequate homogeneous of composition; Or temperature tolerance is poor, can not meet higher requirement.Comparatively speaking, liquid-phase precipitation method is simple to operate because of it, the BiVO that is suitable for low cost
4the production of pigment.
The US Patent No. 5,536,309 that on July 16th, 1996 authorizes has been reported a kind of doping BiVO
4preparation method, by chemical precipitation method, preparing material composition is Bi
xe
vsi
yv
(1-z)p
zo
wpigment, wherein E is the mixture of calcium or calcium zinc-magnesium, doping after BiVO
4the thermostability having had.The US Patent No. 4,937,063 of checking and approving June 17 nineteen ninety has been introduced a kind of solid state reaction and has been prepared BiVO
4method, the compound of bismuth oxide compound and vanadium is by mixing and ball milling, dry.The techniques such as calcining obtain BiVO
4pigment.On August 28th, 1991, disclosed European patent EP 0443981A1 proposed a kind ofly by the mixture that is comprised of bismuth oxide, Vanadium Pentoxide in FLAKES, barium carbonate of calcining, to be made baric or contained the method for glassy yellow pigment of the strong coloring force of zinc.
Above preparation method all can prepare jonquilleous BiVO
4pigment, or complicated process of preparation; Or the inadequate homogeneous of composition; Or tinting strength is poor, or temperature tolerance is poor, can not meet higher requirement.
Therefore develop a kind of technical route simple, the BiVO that product performance are good
4the technology of preparing of pigment is significant.
Summary of the invention
In view of the problem that prior art exists, the object of the present invention is to provide a kind of preparation method of pucherite, it can simplify preparation technology.
Another object of the present invention is to provide a kind of preparation method of pucherite, it can improve the product performance of obtained pucherite.
To achieve these goals, the invention provides a kind of preparation method of pucherite, comprise step: by Bi
2o
3be dissolved in and in nitric acid, prepare Bi (NO
3)
3solution; By NH
4vO
3, Na
5p
3o
10, Na
2moO
4, pure water and NaOH preparation NaVO
3mixing solutions; By Bi (NO
3)
3solution adds NH
4vO
3in mixing solutions, Bi (NO
3)
3after solution adds, regulate the initial pH of reaction soln, and stir; After completion of the reaction, carry out ripening; The BiVO obtaining for reaction
4throw out washing, separated, dry, to obtain dry BiVO
4powder; By dry BiVO
4powder calcination, to obtain the BiVO of sintering
4powder; By the BiVO of sintering
4powder carries out ball milling; By the BiVO after ball milling
4powder drying, to obtain BiVO
4product.
Beneficial effect of the present invention is as follows.
The preparation method of described pucherite provided by the invention, its preparation cycle is short, and preparation technology is simple; And the excellent product performance preparing.
Embodiment
First preparation method according to pucherite of the present invention is described.
According to the preparation method of pucherite of the present invention, comprise step: by Bi
2o
3be dissolved in and in nitric acid, prepare Bi (NO
3)
3solution; By NH
4vO
3, Na
5p
3o
10, Na
2moO
4, pure water and NaOH preparation NaVO
3mixing solutions; By Bi (NO
3)
3solution adds NaVO
3in mixing solutions, Bi (NO
3)
3after solution adds, regulator solution pH, stirs; After reaction finishes, carry out ripening; The BiVO obtaining for reaction
4throw out is through washing, separated, dry, to obtain dry BiVO
4powder; By dry BiVO
4powder calcination, to obtain the BiVO of sintering
4powder; By the BiVO of sintering
4powder carries out ball milling; By the BiVO after ball milling
4vacuum powder is dry, to obtain BiVO
4product.
According in the preparation method of pucherite of the present invention, preferably, Bi (NO
3)
3strength of solution is 0.1 ~ 2mol/L.
According in the preparation method of pucherite of the present invention, preferably, preparing NaVO
3during mixing solutions, vanadium and bismuth mol ratio are V:Bi=(0.6 ~ 1.8): 1; Molybdenum and bismuth mol ratio are Mo:Bi=(0 ~ 1): 1, and sodium hydroxide and bismuth mol ratio are NaOH:Bi=(5 ~ 10): 1, tripoly phosphate sodium STPP and bismuth mol ratio are Na
5p
3o
10: Bi=(0.01 ~ 1): 1.
According in the preparation method of pucherite of the present invention, preferably, described preparation NaVO
3the process of mixing solutions is: by NH
4vO
3, Na
5p
3o
10, Na
2moO
4add pure water to mix, and then add NaOH, continue afterwards to add pure water, preparation NaVO
3mixing solutions.
According in the preparation method of pucherite of the present invention, preferably, by Bi (NO
3)
3solution adds NH
4vO
3in mixing solutions process, by Bi (NO
3)
3solution adds NH
4vO
3the flow velocity of mixing solutions is 1ml/min ~ 500ml/min, when adding, stirs, and reaction 1h ~ 5h, 20 ℃ ~ 90 ℃ of temperature of reaction, the initial pH of reaction soln is 4 ~ 10.More preferably, by Bi (NO
3)
3solution adds NH
4vO
3mixing solutions process is completed by peristaltic pump.
According in the preparation method of pucherite of the present invention, preferably, digestion time 2 ~ 30h;
According in the preparation method of pucherite of the present invention, preferably, dry BiVO
4saltiness in powder is 0.51 ~ 0.75%;
According in the preparation method of pucherite of the present invention, preferably, the BiVO obtaining for reaction
4throw out washing, when separated, dry, described drying temperature is 60 ℃ ~ 120 ℃.
According in the preparation method of pucherite of the present invention, preferably, by dry BiVO
4during powder calcination, the temperature of calcining is 200 ℃ ~ 800 ℃, time 1h ~ 10h; More preferably, calcining adopts retort furnace to complete.
According in the preparation method of pucherite of the present invention, preferably, by the BiVO of sintering
4when powder carries out ball milling, ball-milling medium is zirconium ball, and dispersion agent is Sodium dodecylbenzene sulfonate, and adds pure water, and zirconium ball, pure water, Sodium dodecylbenzene sulfonate, BiVO
4ratio be zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=(8 ~ 15): 3:(0.001 ~ 0.01): 1, Ball-milling Time is 5 ~ 60h.Preferably, BiVO after ball milling
4particle diameter is 204.3nm ~ 926.8nm.
According in the preparation method of pucherite of the present invention, preferably, by the BiVO after ball milling
4during powder drying, dry under 0.05 ~ 0.09MPa vacuum tightness at 50 ℃ ~ 80 ℃.
Secondly the embodiment of the preparation method of pucherite according to the present invention is described.
Embodiment 1
By 10g Bi
2o
3be dissolved in the nitric acid of 18ml65wt.% and add the Bi (NO of pure water preparation 1.2mol/L
3)
3solution;
By 6g NH
4vO
3, 0.158g Na
5p
3o
10, 0.62g Na
2moO
42H
2o adds after pure water mixing, slowly adds the 10g NaOH of weighing, after reaction, continues to add pure water to be mixed with 1mol/LNaVO
3mixing solutions (the mol ratio V:Bi=1.195:1 of calculating; Mo:Bi=0.06:1; NaOH:Bi=5.83:1; Na
5p
3o
10: Bi=0.01:1);
By the Bi (NO of preparation
3)
3solution adds the NaVO of preparation with peristaltic pump
3in mixing solutions, flow velocity is 20ml/min, adds Bi (NO
3)
3solution, regulates reaction solution to make its initial pH=7, mechanical stirring 1h then, and temperature of reaction is 60 ℃, after question response, ageing 2h;
After reaction, mixed solution is through repeated precipitation, washing, separation, then by BiVO
4be placed in loft drier dry at 80 ℃;
By dry BiVO
4powder is placed in retort furnace, at 300 ℃, calcines 3h;
By the BiVO after sintering
4powder is according to zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=8:3:0.005:1 adds ball milling 30h;
Under the vacuum tightness of 0.05MPa, 50 ℃ dry, obtains BiVO
4product.
Embodiment 2
By 10gBi
2o
3be dissolved in the nitric acid of 18ml 65wt.% and add the Bi (NO of pure water preparation 2mol/L
3)
3solution;
By 9.03g NH
4vO
3, 4.89g Na
5p
3o
10, 0g Na
2moO
42H
2o(is Na
2moO
42H
2o does not exist) add pure water mixing, slowly add 17.16g NaOH, after reaction, continue to add pure water to be mixed with 2mol/LNaVO
3mixing solutions (mol ratio V:Bi=1.8:1; Mo:Bi=0:1; NaOH:Bi=10:1; Na
5p
3o
10: Bi=0.31:1);
By the Bi (NO of preparation
3)
3solution adds the NaVO of preparation with peristaltic pump
3in mixing solutions, flow velocity 100ml/min, adds Bi (NO
3)
3solution, regulates reaction soln to make its initial pH=10, mechanical stirring 5h then, and temperature of reaction is 90 ℃, after question response, ageing 24h;
After reaction, mixed solution is through repeated precipitation, washing, separation, then by BiVO
4be placed in loft drier dry at 120 ℃;
By dry BiVO
4powder is placed in retort furnace, at 800 ℃, calcines 1h;
By the BiVO after sintering
4powder is according to zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=10:3:0.001:1 ball milling 60h;
Under the vacuum tightness of 0.06MPa, 60 ℃ of vacuum-dryings, obtain BiVO
4product.
Embodiment 3
By 10g Bi
2o
3be dissolved in the nitric acid of 25ml 65wt.% and add the Bi (NO of pure water preparation 0.1mol/L
3)
3solution;
By 3.01g NH
4vO
3, 15.787g Na
5p
3o
10, 10.38g Na
2moO
42H
2o mixes after adding pure water, slowly adds 8.58g NaOH, after reaction, continues to add pure water to be mixed with 0.1mol/LNaVO
3mixing solutions (mol ratio V:Bi=0.6:1; Mo:Bi=1:1; NaOH:Bi=5:1; Na
5p
3o
10: Bi=1:1);
By the Bi (NO of preparation
3)
3solution adds the NaVO of preparation with peristaltic pump
3in mixing solutions, flow velocity 500ml/min, adds Bi (NO
3)
3solution, regulates reaction soln to make its initial pH=8, mechanical stirring 3h then, and temperature of reaction is 80 ℃, after question response, ageing 12h;
After reaction, mixed solution is through repeated precipitation, washing, separation, then by BiVO
4be placed in loft drier dry at 60 ℃;
By dry BiVO
4powder is placed in retort furnace, at 200 ℃, calcines 10h;
By the BiVO after sintering
4powder is according to zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=15:3:0.01:1 ball milling 5h;
Under 0.08MPa vacuum tightness, 80 ℃ dry, obtains BiVO
4product.
Embodiment 4
By 10g Bi
2o
3be dissolved in the nitric acid of 18ml65wt.% and add the Bi (NO of pure water preparation 0.8mol/L
3)
3solution;
By 4.517g NH
4vO
3, 5.526g Na
5p
3o
10, 5.19g Na
2moO
42H
2o mixes after adding pure water, slowly adds 12.012g NaOH, after reaction, continues to add pure water to be mixed with 1.2mol/LNaVO
3mixing solutions (V:Bi=0.9:1; Mo:Bi=0.5:1; Mol ratio NaOH:Bi=7:1; Na
5p
3o
10: Bi=0.35:1);
By the Bi (NO of preparation
3)
3solution adds the NaVO of preparation with peristaltic pump
3in mixing solutions, flow velocity 1ml/min, adds Bi (NO
3)
3solution, regulates the initial pH=4 of reaction soln, mechanical stirring 4h then, and temperature of reaction is 20 ℃, after question response, ageing 30h;
After reaction, mixed solution is through repeated precipitation, washing, separation, then by BiVO
4be placed in loft drier dry at 100 ℃;
By dry BiVO
4powder is placed in retort furnace, at 400 ℃ of calcining 5h;
By the BiVO after sintering
4powder is according to zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=11:3:0.005:1 adds ball milling 40h after zirconium ball, pure water, Sodium dodecylbenzene sulfonate;
Under the vacuum tightness of 0.09MPa, 50 ℃ dry, obtains BiVO
4product.
Finally provide the preparation method's of the pucherite of the present invention detected result of embodiment 1-4.
When detecting, by Ma Erwen laser particle analyzer test b iVO
4size-grade distribution; By 406LStatistical Glossmeter test b iVO
4glossiness; By MA68 II Multi-AngleSpectrophotometer test b iVO
4aberration; According to GB/T5211 standard testing BiVO
4saltiness, oil number, acid resistance, alkali resistance, solvent resistance; According to GB/T9287-88 standard testing BiVO
4dispersiveness.
Table 1 has provided the final BiVO obtaining of embodiment 1-4
4the detected result of product.As seen from Table 1, by the preparation-obtained BiVO of preparation method of pucherite of the present invention
4excellent product performance.
The detected result of the final sample obtaining of table 1 embodiment 1-4
Claims (10)
1. a preparation method for pucherite, comprises step:
By Bi
2o
3be dissolved in and in nitric acid, prepare Bi (NO
3)
3solution;
By NH
4vO
3, Na
5p
3o
10, Na
2moO
4, pure water and NaOH preparation NaVO
3mixing solutions;
By Bi (NO
3)
3solution adds NH
4vO
3in mixing solutions, Bi (NO
3)
3after solution adds, regulate the initial pH of reaction soln, and stir;
After completion of the reaction, carry out ripening;
The BiVO obtaining for reaction
4throw out washing, separated, dry, to obtain dry BiVO
4powder;
By dry BiVO
4powder calcination, to obtain the BiVO of sintering
4powder;
By the BiVO of sintering
4powder carries out ball milling;
By the BiVO after ball milling
4powder drying, to obtain BiVO
4product.
2. the preparation method of pucherite according to claim 1, is characterized in that, Bi (NO
3)
3the concentration of solution is 0.1 ~ 2mol/L.
3. the preparation method of pucherite according to claim 1, is characterized in that, described preparation NaVO
3the process of mixing solutions is: by NH
4vO
3, Na
5p
3o
10, Na
2moO
4add pure water to mix, and then add NaOH, continue afterwards to add pure water, preparation NaVO
3mixing solutions.
4. the preparation method of pucherite according to claim 1, is characterized in that, at preparation NaVO
3during mixing solutions, the mol ratio of vanadium and bismuth is V:Bi=(0.6 ~ 1.8): 1, and molybdenum and bismuth mol ratio are Mo:Bi=(0 ~ 1): 1, sodium hydroxide and bismuth mol ratio are NaOH:Bi=(5 ~ 10): 1, tripoly phosphate sodium STPP and bismuth mol ratio are Na
5p
3o
10: Bi=(0.01 ~ 1): 1.
5. the preparation method of pucherite according to claim 1, is characterized in that, by Bi (NO
3)
3add NH
4vO
3in solution process, flow velocity is 1ml/min ~ 500ml/min, and the initial pH of reaction soln is 4 ~ 10, churning time 1h ~ 5h, 20 ℃ ~ 90 ℃ of temperature of reaction.
6. the preparation method of pucherite according to claim 1, is characterized in that, digestion time is 2 ~ 30h.
7. the preparation method of pucherite according to claim 1, is characterized in that, the BiVO obtaining for reaction
4throw out washing, when separated, dry, drying temperature is 60 ℃ ~ 120 ℃.
8. the preparation method of pucherite according to claim 1, is characterized in that, by dry BiVO
4during powder calcination, the temperature of calcining is 200 ℃ ~ 800 ℃, and the time is 1h ~ 10h.
9. the preparation method of pucherite according to claim 1, is characterized in that, by the BiVO of sintering
4when powder carries out ball milling, ball-milling medium is zirconium ball, and dispersion agent is Sodium dodecylbenzene sulfonate, and adopts pure water, and zirconium ball, pure water, Sodium dodecylbenzene sulfonate, BiVO
4ratio be zirconium ball: pure water: Sodium dodecylbenzene sulfonate: BiVO
4=(8 ~ 15): 3:(0.001 ~ 0.01): 1, Ball-milling Time is 5 ~ 60h.
10. the preparation method of pucherite according to claim 1, is characterized in that, by the BiVO after ball milling
4during powder drying, dry at 50 ℃ ~ 80 ℃ under the vacuum tightness of 0.05 ~ 0.09MPa.
Priority Applications (2)
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CN201210228971.2A CN103523831B (en) | 2012-07-03 | 2012-07-03 | Preparation method of bismuth vanadate |
PCT/CN2013/078042 WO2014005491A1 (en) | 2012-07-03 | 2013-06-26 | Method for preparing bismuth vanadate |
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CN201210228971.2A CN103523831B (en) | 2012-07-03 | 2012-07-03 | Preparation method of bismuth vanadate |
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CN103523831A true CN103523831A (en) | 2014-01-22 |
CN103523831B CN103523831B (en) | 2015-06-10 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105948119A (en) * | 2016-04-28 | 2016-09-21 | 中南大学 | Method for preparing bismuth vanadate |
CN106349756A (en) * | 2016-08-27 | 2017-01-25 | 湖南汉瑞新材料科技有限公司 | Yellow inorganic pigment taking bismuth and vanadium as basic adulterants as well as preparation method and application thereof |
CN106946289A (en) * | 2017-03-16 | 2017-07-14 | 景德镇陶瓷大学 | A kind of green phase glassy yellow inorganic nanometer pigment and preparation method thereof |
CN107876052A (en) * | 2017-10-16 | 2018-04-06 | 华南师范大学 | A kind of catalysis material Ag/BiV1‑xMoxO4Preparation method |
CN112960694A (en) * | 2021-02-01 | 2021-06-15 | 北京交通大学 | Preparation method of green bismuth vanadate particles |
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FR2949456B1 (en) * | 2009-08-31 | 2013-04-12 | Saint Gobain | BISMUTH VANADATE PARTICLES AND PROCESS FOR OBTAINING THEM |
CN102502821B (en) * | 2011-09-29 | 2013-07-24 | 北京工业大学 | Mixed organic solvent-thermal method for preparing spherical or hollow spherical BiVO4 |
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US6464772B1 (en) * | 1999-11-22 | 2002-10-15 | Gebroeders Cappelle N.V. | Bismuth-based pigments and process for their manufacture |
CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
CN101070435A (en) * | 2007-03-27 | 2007-11-14 | 鲁东大学 | Method for preparing super-fine vanadic-acid bismuth-yellow pigment |
CN101104144A (en) * | 2007-06-28 | 2008-01-16 | 北京工业大学 | Method for preparing nanometer BiVO4 material visible-light photocatalyst |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105948119A (en) * | 2016-04-28 | 2016-09-21 | 中南大学 | Method for preparing bismuth vanadate |
CN106349756A (en) * | 2016-08-27 | 2017-01-25 | 湖南汉瑞新材料科技有限公司 | Yellow inorganic pigment taking bismuth and vanadium as basic adulterants as well as preparation method and application thereof |
CN106946289A (en) * | 2017-03-16 | 2017-07-14 | 景德镇陶瓷大学 | A kind of green phase glassy yellow inorganic nanometer pigment and preparation method thereof |
CN107876052A (en) * | 2017-10-16 | 2018-04-06 | 华南师范大学 | A kind of catalysis material Ag/BiV1‑xMoxO4Preparation method |
CN107876052B (en) * | 2017-10-16 | 2021-04-30 | 华南师范大学 | Catalytic material Ag/BiV1-xMoxO4Preparation method of (1) |
CN112960694A (en) * | 2021-02-01 | 2021-06-15 | 北京交通大学 | Preparation method of green bismuth vanadate particles |
Also Published As
Publication number | Publication date |
---|---|
WO2014005491A1 (en) | 2014-01-09 |
CN103523831B (en) | 2015-06-10 |
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