CN103523831B - Preparation method of bismuth vanadate - Google Patents

Preparation method of bismuth vanadate Download PDF

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Publication number
CN103523831B
CN103523831B CN201210228971.2A CN201210228971A CN103523831B CN 103523831 B CN103523831 B CN 103523831B CN 201210228971 A CN201210228971 A CN 201210228971A CN 103523831 B CN103523831 B CN 103523831B
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bivo
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powder
reaction
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CN103523831A (en
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赵青燕
朱刘
李蓉
裴志明
刘华胜
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Kunming Forerunner New Material Technology Co ltd
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Vital Materials Co Ltd
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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

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 with the concentration of 0.1-2mol/L; preparing a NaVO3 mixed solution from NH4VO3, Na5P3O10, Na2MoO4, pure water and NaOH; adding the Bi(NO3)3 solution into the NaVO3 mixed solution, the molar ratio of the vanadium and bismuth, namely V:Bi being (0.6-1.8):1, the molar ratio of the molybdenum and bismuth, namely V:Bi being (0-1):1, the molar ratio of the sodium hydroxide and bismuth, namely NaOH:Bi=(5-10):1, the molar ratio of the sodium tripolyphosphate and bismuth, namely Na5P3O10:Bi=(0.01-1):1, adding the Bi(NO3)3 solution into the NaVO3 mixed solution with the flow rate of 1ml/min-500ml/min, adjusting the initial pH value of the reaction solution after the Bi(NO3)3 solution is added, the initial pH value of the reaction solution being 4-10, and stirring for 1h-5h, reacting at the temperature of 20DEG C-90DEG C; 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; and drying the BiVO4 powder subjected to ball milling to obtain a BiVO4 product.

Description

The preparation method of pucherite
Technical field
The present invention relates to a kind of preparation method of mineral dye, particularly relate to a kind of preparation method of pucherite.
Background technology
BiVO 4yellow ultramarine has nontoxic, good weatherability, bright color and environment amenable premium properties, it is a kind of novel pigment having rosy prospect, thus can be used to replace the pigment containing the toxic element 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 the stability of its excellence 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 composition is homogeneous not; Or temperature tolerance is poor, can not meet higher requirement.Comparatively speaking, liquid-phase precipitation method is simple to operate because of it, is with low costly suitable for BiVO 4the production of pigment.
The US Patent No. 5,536,309 of authorizing on July 16th, 1996 reports a kind of doping BiVO 4preparation method, preparing material composition by chemical precipitation method 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 had.The US Patent No. 4,937,063 checked and approved June 17 nineteen ninety describes a kind of solid state reaction and prepares BiVO 4method, the compound of bismuth oxide compound and vanadium is by mixing and ball milling, drying.The techniques such as calcining obtain BiVO 4pigment.European patent EP 0443981A1 disclosed in 28 days Augusts in 1991 proposes a kind of method obtaining baric or the glassy yellow pigment containing the strong coloring force of zinc by calcining the mixture be made up of bismuth oxide, Vanadium Pentoxide in FLAKES, barium carbonate.
Above preparation method all can prepare jonquilleous BiVO 4pigment, or complicated process of preparation; Or composition is homogeneous not; Or tinting strength is poor, or temperature tolerance is poor, can not meet higher requirement.
Therefore a kind of technical route is developed simple, the BiVO that product performance are excellent 4the technology of preparing of pigment is significant.
Summary of the invention
In view of prior art Problems existing, 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 the preparation method providing a kind 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 nitric acid and prepare Bi (NO 3) 3solution; By NH 4vO 3, Na 5p 3o 10, Na 2moO 4, pure water and NaOH prepare NaVO 3mixing solutions; By Bi (NO 3) 3solution adds NaVO 3in mixing solutions, Bi (NO 3) 3after solution adds, regulate the initial pH of reaction soln, and stir; After completion of the reaction, ripening is carried out; For the BiVO that reaction obtains 4throw out washing, separation, drying, to obtain dry BiVO 4powder; By the BiVO of drying 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.Wherein: Bi (NO 3) 3the concentration of solution is 0.1 ~ 2mol/L; At preparation NaVO 3during mixing solutions, the mol ratio of vanadium and bismuth is 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, and tripoly phosphate sodium STPP and bismuth mol ratio are Na 5p 3o 10: Bi=(0.01 ~ 1): 1; By Bi (NO 3) 3add NaVO 3in solution processes, flow velocity is 1ml/min ~ 500ml/min, and the initial pH of reaction soln is 4 ~ 10, churning time 1h ~ 5h, temperature of reaction 20 DEG C ~ 90 DEG C.
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 prepared.
Embodiment
First preparation method according to pucherite of the present invention is described.
Preparation method according to pucherite of the present invention comprises step: by Bi 2o 3be dissolved in nitric acid and prepare Bi (NO 3) 3solution; By NH 4vO 3, Na 5p 3o 10, Na 2moO 4, pure water and NaOH prepare 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 terminates, carry out ripening; For the BiVO that reaction obtains 4throw out through washing, be separated, dry, to obtain dry BiVO 4powder; By the BiVO of drying 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, at preparation 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, and 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 mixing, 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 NaVO 3in mixing solutions process, by Bi (NO 3) 3solution adds NaVO 3the flow velocity of mixing solutions is 1ml/min ~ 500ml/min, stirs while adding, and reaction 1h ~ 5h, temperature of reaction 20 DEG C ~ 90 DEG C, the initial pH of reaction soln is 4 ~ 10.More preferably, by Bi (NO 3) 3solution adds NaVO 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, for the BiVO that reaction obtains 4when throw out washing, separation, drying, described drying temperature is 60 DEG C ~ 120 DEG C.
According in the preparation method of pucherite of the present invention, preferably, by the BiVO of drying 4during powder calcination, the temperature of calcining is 200 DEG C ~ 800 DEG C, 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 DEG C ~ 80 DEG C.
Secondly embodiment according to the preparation method of pucherite of the present invention is described.
Embodiment 1
By 10g Bi 2o 3to be dissolved in the nitric acid of 18ml 65wt.% and to 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 slowly adds the 10g NaOH of weighing, after reaction, continues to add pure water and be mixed with 1mol/LNaVO after adding pure water mixing 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 peristaltic pump adds the NaVO of preparation 3in mixing solutions, flow velocity is 20ml/min, adds Bi (NO 3) 3solution, regulate reaction solution to make its initial pH=7, then mechanical stirring 1h, temperature of reaction is 60 DEG C, 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 DEG C;
By the BiVO of drying 4powder is placed in retort furnace, at 300 DEG C, calcine 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 DEG C of dryings, obtain BiVO 4product.
Embodiment 2
By 10gBi 2o 3to be dissolved in the nitric acid of 18ml 65wt.% and to 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 (i.e. Na 2moO 42H 2o does not exist) add pure water mixing, slowly add 17.16g NaOH, after reaction, continue to add pure water and 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 peristaltic pump adds the NaVO of preparation 3in mixing solutions, flow velocity 100ml/min, adds Bi (NO 3) 3solution, regulate reaction soln to make its initial pH=10, then mechanical stirring 5h, temperature of reaction is 90 DEG C, 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 DEG C;
By the BiVO of drying 4powder is placed in retort furnace, at 800 DEG C, calcine 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 DEG C of vacuum-dryings, obtain BiVO 4product.
Embodiment 3
By 10g Bi 2o 3to be dissolved in the nitric acid of 25ml 65wt.% and to 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 and is 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 peristaltic pump adds the NaVO of preparation 3in mixing solutions, flow velocity 500ml/min, adds Bi (NO 3) 3solution, regulate reaction soln to make its initial pH=8, then mechanical stirring 3h, temperature of reaction is 80 DEG C, 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 DEG C;
By the BiVO of drying 4powder is placed in retort furnace, at 200 DEG C, calcine 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 DEG C of dryings, obtain BiVO 4product.
Embodiment 4
By 10g Bi 2o 3to be dissolved in the nitric acid of 18ml 65wt.% and to 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 and is 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 peristaltic pump adds the NaVO of preparation 3in mixing solutions, flow velocity 1ml/min, adds Bi (NO 3) 3solution, regulate the initial pH=4 of reaction soln, then mechanical stirring 4h, temperature of reaction is 20 DEG C, 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 DEG C;
By the BiVO of drying 4powder is placed in retort furnace, at 400 DEG C 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 DEG C of dryings, obtain BiVO 4product.
Finally provide the detected result of the embodiment 1-4 of the preparation method of pucherite of the present invention.
When detecting, by Malvern 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/T 5211 standard testing BiVO 4saltiness, oil number, acid resistance, alkali resistance, solvent resistance; According to GB/T 9287-88 standard testing BiVO 4dispersiveness.
Table 1 gives the embodiment 1-4 BiVO finally obtained 4the detected result of product.As seen from Table 1, by the preparation-obtained BiVO of the preparation method of pucherite of the present invention 4excellent product performance.
The detected result of the sample that table 1 embodiment 1-4 finally obtains

Claims (7)

1. a preparation method for pucherite, comprises step:
By Bi 2o 3be dissolved in nitric acid and prepare Bi (NO 3) 3solution;
By NH 4vO 3, Na 5p 3o 10, Na 2moO 4, pure water and NaOH prepare NaVO 3mixing solutions;
By Bi (NO 3) 3solution adds NaVO 3in mixing solutions, Bi (NO 3) 3after solution adds, regulate the initial pH of reaction soln, and stir;
After completion of the reaction, ripening is carried out;
For the BiVO that reaction obtains 4throw out washing, separation, drying, to obtain dry BiVO 4powder;
By the BiVO of drying 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;
Wherein:
Bi (NO 3) 3the concentration of solution is 0.1 ~ 2mol/L;
At preparation NaVO 3during mixing solutions, the mol ratio of vanadium and bismuth is 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, and tripoly phosphate sodium STPP and bismuth mol ratio are Na 5p 3o 10: Bi=(0.01 ~ 1): 1;
By Bi (NO 3) 3add NaVO 3in solution processes, flow velocity is 1ml/min ~ 500ml/min, and the initial pH of reaction soln is 4 ~ 10, churning time 1h ~ 5h, temperature of reaction 20 DEG C ~ 90 DEG C.
2. 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 mixing, and then add NaOH, continue afterwards to add pure water, preparation NaVO 3mixing solutions.
3. the preparation method of pucherite according to claim 1, is characterized in that, digestion time is 2 ~ 30h.
4. the preparation method of pucherite according to claim 1, is characterized in that, for the BiVO that reaction obtains 4when throw out washing, separation, drying, drying temperature is 60 DEG C ~ 120 DEG C.
5. the preparation method of pucherite according to claim 1, is characterized in that, by the BiVO of drying 4during powder calcination, the temperature of calcining is 200 DEG C ~ 800 DEG C, and the time is 1h ~ 10h.
6. 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.
7. 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 DEG C ~ 80 DEG C under the vacuum tightness of 0.05 ~ 0.09MPa.
CN201210228971.2A 2012-07-03 2012-07-03 Preparation method of bismuth vanadate Active CN103523831B (en)

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CN105948119B (en) * 2016-04-28 2017-08-08 中南大学 A kind of method for preparing pucherite
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
CN106946289B (en) * 2017-03-16 2018-12-04 景德镇陶瓷大学 A kind of green phase glassy yellow inorganic nanometer pigment and preparation method thereof
CN107876052B (en) * 2017-10-16 2021-04-30 华南师范大学 Catalytic material Ag/BiV1-xMoxO4Preparation method of (1)
CN112960694B (en) * 2021-02-01 2022-07-01 北京交通大学 Preparation method of green bismuth vanadate particles
CN114105196A (en) * 2021-11-12 2022-03-01 成都先进金属材料产业技术研究院股份有限公司 Method for preparing bismuth vanadate superfine powder by gel combustion method and bismuth vanadate powder prepared by method
CN114229895A (en) * 2021-12-17 2022-03-25 湖南柿竹园有色金属有限责任公司 Method for preparing quantum material bismuth vanadate

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Patentee before: FIRST RARE MATERIALS Co.,Ltd.