CN103157461A - Nanometer photocatalyst bismuth tungstate and preparation method thereof - Google Patents

Nanometer photocatalyst bismuth tungstate and preparation method thereof Download PDF

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CN103157461A
CN103157461A CN2013101167892A CN201310116789A CN103157461A CN 103157461 A CN103157461 A CN 103157461A CN 2013101167892 A CN2013101167892 A CN 2013101167892A CN 201310116789 A CN201310116789 A CN 201310116789A CN 103157461 A CN103157461 A CN 103157461A
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bismuth tungstate
nano
preparation
mixture
bismuth
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王雄
蓝燕
林颖
李柳
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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Abstract

The invention discloses a method for preparing nanometer bismuth tungstate by utilizing a fused salt method. According to the method, bismuth nitrate and sodium tungstate are adopted as raw materials, potassium nitrate/sodium nitrate and lithium nitrate are utilized as a fuse salt system, the raw materials are mixed and added into a molten salt system in a crucible, and the nanoscale bismuth tungstate powder is obtained through reaction. According to the method, the uniform mixing of raw material on a molecule scale can be realized, and the nanoscale bismuth tungstate powder with high purity is obtained. The method provided by the invention has the advantages that the equipment is simple, the technological process is short, the operation is simple, the product performance is excellent, and the method has an extensive application prospect.

Description

A kind of nano-photocatalyst bismuth tungstate and preparation method thereof
Technical field
The invention belongs to the inorganic functional material preparing technical field, relate to a kind of photochemical catalyst and preparation method thereof, particularly a kind of molten-salt growth method prepares the method for bismuth tungstate nano-powder.
Background technology
Bismuth tungstate has bismuth laminated, and at dielectric, ion conductor is widely studied in luminescent material, and due to its narrower energy gap, has caused again high concern in the visible light catalytic field recently.Bismuth tungstate is under illumination condition, but the decomposition of catalysis water prepares hydrogen and oxygen, also degrading organic pollutant.Preparation degree of crystallinity is high, the pattern homogeneous, and the bismuth tungstate powder that particle is tiny has extremely important effect to improving its photocatalysis performance.
At present, the method for preparing bismuth tungstate mainly contains the hot method of hydrothermal/solvent, critical state circumfluence method, sol-gal process, ball-milling method etc.Wenzhong Wang group has prepared bismuth tungstate flower-like structure (L.S. Zhang, W.Z. Wang and H.L. Xu, Journal of Materials Chemistry, 17 (2007): 2526-2532) under 160 ℃ with hydro-thermal method.In addition, they take ethylene glycol as solvent, have prepared bismuth tungstate cage-shaped nano particle (M. Shang, W.Z. Wang and H.L. Xu, the Crystal Growth of the homogeneous of taking measurements greatly take the self-control Nano carbon balls as template with the critical state circumfluence method; Design, 9 (2009): 991-996).Gaoke Zhang etc. are take bismuth nitrate and ammonium tungstate as raw material, citric acid is complexing agent, prepared bismuth tungstate powder (the G.K. Zhang of the outstanding photocatalysis performance of tool, F. Lu, M. Li, J.L. Yang, X.Y. Zhang and B.B. Huang, Journal of Physics and Chemistry of Solids, 71 (2010) 579-582).M.Maczka etc. are take sodium tungstate and bismuth nitrate as raw material, obtain unbodied predecessor by mechanical lapping, after predecessor is processed, can obtain bismuth tungstate nanometer sheet (M.Maczka, A.F.Fuentes and J.Hanuza, Materials Chemistry and Physics, 120 (2010) 289-295).Hydro-thermal method requires reaction vessel high pressure resistant, more difficult realization in industrial production; Circumfluence method and sol-gel process need to be carried out subsequent heat treatment to remove impurity to product, easily cause grain growth; And ball-milling method needs higher temperature, and prepared product purity is relatively low.
Also there is no relevant report about the method with the standby bismuth tungstate of fuse salt legal system.
Summary of the invention
The object of the present invention is to provide that a kind of equipment is simple, technique is simple, the bismuth tungstate nano-powder of excellent product performance and preparation method thereof.
For realizing this purpose, technical solution of the present invention is: a kind of nano-photocatalyst bismuth tungstate, described bismuth tungstate are layer structure.
A kind of preparation method of nano-photocatalyst bismuth tungstate specifically comprises the following steps:
The first step: with KNO 3Or NaNO 3Put into the crucible heating and melting with the mixture of LiNO, insulation;
Second step: with Bi (NO 3) 35H 2O and Na 2WO 42H 2The O mixing is placed on grinds in mortar evenly;
The 3rd step: under stirring state, second step gained mixture is added in first step gained fuse salt heat up, carry out molten salt reaction;
The 4th step: the 3rd step products therefrom is with distilled water and absolute ethanol washing, dry under lower than 80 ℃, make nanometer bismuth tungstate powder.
KNO in salt-mixture described in the first step 3Or NaNO 3With the ratio of the amount of substance of LiNO be (0.5-5): 1; Described heating-up temperature is that 140-180 ℃, temperature retention time are 1-5 hour.
Bi (NO described in second step 3) 35H 2O and Na 2WO 42H 2The ratio of the amount of substance of O is (2 ~ 8): 1.
Bi (NO described in second step 3) 35H 2O:Na 2WO 42H 2O: salt-mixture=(2-8): 1:(5 ~ 10).
The temperature of the molten salt reaction described in the 3rd step is 150-300 ℃, and the time is 4-24 hour.
The present invention compared with prior art has the following advantages and outstanding effect: (1) raw material is simple.The present invention is take bismuth nitrate and sodium tungstate as raw material, as the fuse salt system, can prepare a large amount of nanometer bismuth tungstate powders with potassium nitrate or sodium nitrate and lithium nitrate.(2) technique is simple.Need not pass through pre-treatment and post processing, technique is very simple, easy operating, and Modulatory character is strong, to the no requirement (NR) of reaction system pressure, is convenient to realize suitability for industrialized production.(3) purity is high, better crystallinity degree.(4) crystal grain is tiny.(5) because the size of photocatalytic activity and catalyst, degree of crystallinity, pattern etc. have substantial connection, can infer that this product has good photocatalytic activity.
Description of drawings
Fig. 1 is process chart of the present invention.
The XRD figure of the nanometer bismuth tungstate powder of Fig. 2 embodiment of the present invention 2 preparations.
The SEM figure of the nanometer bismuth tungstate powder of Fig. 3 embodiment of the present invention 3 preparations.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
In Fig. 1, a kind of method for preparing the photochemical catalyst bismuth tungstate of the present invention comprises following concrete steps:
One, with KNO 3/ LiNO 3Or NaNO 3/ LiNO 3Salt-mixture is pressed the ratio (0.5-5) of amount of substance: 1 mixes, and is heated to 140-180 ℃, is incubated 1-5 hour;
Two, with Bi (NO 3) 35H 2O and Na 2WO 42H 2O is (2 ~ 8) by the ratio of amount of substance: 1 mixing is placed on grinds in mortar evenly;
Three, under stirring state, second step gained mixture is added in first step gained fuse salt, carry out the molten salt reaction of 4-24h under 150-300 ℃;
Four, with the 3rd step products therefrom with distilled water and absolute ethanol washing, dry under lower than 80 ℃, make nanometer bismuth tungstate powder.
Embodiment 1
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 5.24gKNO 3And 2.63gLiNO 3Be placed in crucible, be heated to 140 ℃ of meltings, be incubated 5 hours.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 150 ℃ of insulations, reacted 24 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.
Embodiment 2
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 5.24gKNO 3And 2.63gLiNO 3Be placed in crucible, be heated to 140 ℃ of meltings, be incubated 4 hours.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 240 ℃ of insulations, reacted 8 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.The gained sample is pure oblique side's phase bismuth tungstate through XRD determining, there is no other impurity peaks (seeing Fig. 2).
Embodiment 3
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 5.24gKNO 3And 2.63gLiNO 3Be placed in crucible, be heated to 140 ℃ of meltings, be incubated 3 hours.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 200 ℃ of insulations, reacted 15 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.Resulting bismuth tungstate nanometer sheet thickness is between the 30-50 nanometer, and long and wide is 500-1000 nanometer (seeing Fig. 3).
Embodiment 4
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 5.24gKNO 3And 2.63gLiNO 3Be placed in crucible, be heated to 160 ℃ of meltings, be incubated 2 hours.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 180 ℃ of insulations, reacted 20 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.
Embodiment 5
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 3.54gNaNO 3And 3.34gLiNO 3Be placed in crucible, be heated to 180 ℃ of meltings, be incubated 2 hours.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 300 ℃ of insulations, reacted 4 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.
Embodiment 6
Take 10mmBi (NO 3) 35H 2O and 5mmNa 2WO 42H 2O is placed in mortar and grinds.Take 8.50gNaNO 3And 8.00gLiNO 3Be placed in crucible, be heated to 160 ℃ of meltings, be incubated 1 hour.To grind gained Bi (NO 3) 35H 2O and Na 2WO 42H 2The mixture of O adds crucible under stirring condition in, be warming up to 200 ℃ of insulations, reacted 6 hours.After reaction finishes, end product with deionized water, absolute ethanol washing 5-8 time, 80 ℃ of dryings 8 hours, is made the bismuth tungstate powder.

Claims (5)

1. the preparation method of a nano-photocatalyst bismuth tungstate is characterized in that specifically comprising the following steps:
The first step: with KNO 3Or NaNO 3Put into the crucible heating and melting with the mixture of LiNO, insulation;
Second step: with Bi (NO 3) 35H 2O and Na 2WO 42H 2The O mixing is placed on grinds in mortar evenly;
The 3rd step: under stirring state, second step gained mixture is added in first step gained fuse salt heat up, carry out molten salt reaction;
The 4th step: the 3rd step products therefrom is with distilled water and absolute ethanol washing, dry under lower than 80 ℃, make nanometer bismuth tungstate powder.
2. the preparation method of nano-photocatalyst bismuth tungstate according to claim 1, is characterized in that KNO in the salt-mixture described in the first step 3Or NaNO 3With the ratio of the amount of substance of LiNO be (0.5-5): 1; Described heating-up temperature is that 140-180 ℃, temperature retention time are 1-5 hour.
3. the preparation method of nano-photocatalyst bismuth tungstate according to claim 1, is characterized in that the Bi (NO described in second step 3) 35H 2O and Na 2WO 42H 2The ratio of the amount of substance of O is (2 ~ 8): 1.
4. the preparation method of nano-photocatalyst bismuth tungstate according to claim 1, is characterized in that the Bi (NO described in second step 3) 35H 2O:Na 2WO 42H 2O: salt-mixture=(2-8): 1:(5 ~ 10).
5. the preparation method of nano-photocatalyst bismuth tungstate according to claim 1, is characterized in that the temperature of the molten salt reaction described in the 3rd step is 150-300 ℃, and the time is 4-24 hour.
CN2013101167892A 2013-04-03 2013-04-03 Nanometer photocatalyst bismuth tungstate and preparation method thereof Pending CN103157461A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103771522A (en) * 2014-01-07 2014-05-07 洛阳理工学院 Method for preparing manganese tungstate nano-sheets by molten salt method
CN104209118A (en) * 2014-09-25 2014-12-17 天津师范大学 Method for preparing bismuth hydroxide/bismuth tungstate compound photo-catalyst by heating one-pot solvent
CN104891573A (en) * 2015-05-28 2015-09-09 新疆大学 Method for preparing bismuth tungstate nanosheets through solid state chemical reaction
CN106045556A (en) * 2016-06-06 2016-10-26 中南大学 High-strength, lightweight, environment-friendly and porous interior wall diatomite brick with visible light photocatalysis performance and preparation method of interior wall diatomite brick
CN106732535A (en) * 2016-12-19 2017-05-31 阜阳师范学院 A kind of photochemical catalyst Bi2Mo3O12And preparation method thereof
CN106807361A (en) * 2017-02-28 2017-06-09 重庆工商大学 A kind of unformed bismuth tungstate bismuth oxide ternary organic composite photochemical catalyst of bismuth and preparation method
CN107213912A (en) * 2017-06-16 2017-09-29 益阳医学高等专科学校 A kind of composite nano materials and its preparation method and application
CN111172743A (en) * 2020-01-16 2020-05-19 浙江大学 Method for rapidly preparing composite metal oxide nano film material at low temperature
CN112875755A (en) * 2020-12-29 2021-06-01 杭州电子科技大学 Preparation method of bismuth tungstate nano powder
CN114132964A (en) * 2022-02-07 2022-03-04 材料科学姑苏实验室 Preparation method of amorphous black bismuth tungstate, amorphous black bismuth tungstate and application thereof
CN114832850A (en) * 2022-03-16 2022-08-02 武汉轻工大学 Layered bismuth subnitrate hydroxide nanosheet and preparation method and application thereof

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103771522B (en) * 2014-01-07 2015-04-08 洛阳理工学院 Method for preparing manganese tungstate nano-sheets by molten salt method
CN103771522A (en) * 2014-01-07 2014-05-07 洛阳理工学院 Method for preparing manganese tungstate nano-sheets by molten salt method
CN104209118A (en) * 2014-09-25 2014-12-17 天津师范大学 Method for preparing bismuth hydroxide/bismuth tungstate compound photo-catalyst by heating one-pot solvent
CN104891573A (en) * 2015-05-28 2015-09-09 新疆大学 Method for preparing bismuth tungstate nanosheets through solid state chemical reaction
CN104891573B (en) * 2015-05-28 2017-04-12 新疆大学 Method for preparing bismuth tungstate nanosheets through solid state chemical reaction
CN106045556B (en) * 2016-06-06 2019-04-05 中南大学 A kind of high-strength light stephanoporate environment protection interior wall diatom brick and preparation method thereof with visible light catalytic performance
CN106045556A (en) * 2016-06-06 2016-10-26 中南大学 High-strength, lightweight, environment-friendly and porous interior wall diatomite brick with visible light photocatalysis performance and preparation method of interior wall diatomite brick
CN106732535A (en) * 2016-12-19 2017-05-31 阜阳师范学院 A kind of photochemical catalyst Bi2Mo3O12And preparation method thereof
CN106807361A (en) * 2017-02-28 2017-06-09 重庆工商大学 A kind of unformed bismuth tungstate bismuth oxide ternary organic composite photochemical catalyst of bismuth and preparation method
CN106807361B (en) * 2017-02-28 2019-02-15 重庆工商大学 A kind of unformed bismuth tungstate of bismuth-- bismuth oxide ternary organic composite photochemical catalyst and preparation method
CN107213912A (en) * 2017-06-16 2017-09-29 益阳医学高等专科学校 A kind of composite nano materials and its preparation method and application
CN107213912B (en) * 2017-06-16 2020-05-19 益阳医学高等专科学校 Composite nano material and preparation method and application thereof
CN111172743A (en) * 2020-01-16 2020-05-19 浙江大学 Method for rapidly preparing composite metal oxide nano film material at low temperature
CN111172743B (en) * 2020-01-16 2021-10-19 浙江大学 Method for rapidly preparing composite metal oxide nano film material at low temperature
CN112875755A (en) * 2020-12-29 2021-06-01 杭州电子科技大学 Preparation method of bismuth tungstate nano powder
CN114132964A (en) * 2022-02-07 2022-03-04 材料科学姑苏实验室 Preparation method of amorphous black bismuth tungstate, amorphous black bismuth tungstate and application thereof
CN114832850A (en) * 2022-03-16 2022-08-02 武汉轻工大学 Layered bismuth subnitrate hydroxide nanosheet and preparation method and application thereof
CN114832850B (en) * 2022-03-16 2023-12-01 武汉轻工大学 Layered bismuth oxynitrate nano-sheet and preparation method and application thereof

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Application publication date: 20130619