CN105731538A - High pressure-hydrothermal method for preparation of BiVO4 photocatalyst - Google Patents
High pressure-hydrothermal method for preparation of BiVO4 photocatalyst Download PDFInfo
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Abstract
The invention discloses a high pressure-hydrothermal method for preparation of a BiVO4 photocatalyst. The method comprises the following steps: dissolving bismuth nitrate and sodium dodecyl benzene sulfonate in a solution composed of glycol and water in a volume ratio of 1: 1 and dissolving ammonium metavanadate in distilled water; adding the obtained ammonium metavanadate solution into the aqueous glycol solution drop by drop, carrying out uniform mixing under stirring, and adjusting the pH value of the obtained solution to 3 by using ammonia water so as to obtain a precursor for the BiVO4 photocatalyst; transferring the precursor to a high-pressure reaction vessel, introducing any one selected from a group consisting of nitrogen, oxygen and argon so as to allow pressure intensity to be 2 to 10 MPa and carrying out alcohol-hydrothermal treatment at 100 to 120 DEG C for 4 to 12 h; successively carrying out cooling, centrifugation and washing; and then carrying out drying at 80 DEG C and then roasting at 450 DEG C for 4 h so as to obtain the BiVO4 photocatalyst with a high crystallization degree, good dispersibility, small granularity, a great specific surface area, a monoclinic scheelite structure and high catalytic activity. The obtained BiVO4 photocatalyst has good visible-light catalytic activity and can be extensively applied to treatment of industrial wastewater.
Description
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of high pressure-hydro-thermal method and prepare BiVO4The method of photocatalyst.
Background technology
Photocatalytic Oxidation With Semiconductors method can directly utilize sunlight and effectively decompose and the organic pollution of mineralising difficult degradation, and correlational study achieves greater advance in recent years.In numerous catalysis materials, BiVO4, catalysis active height narrow with its energy gap, the advantage such as nontoxic, cheap, it is believed that be one of the catalysis material of most application potential at present.
BiVO4Mainly there are three kinds of crystal formations: four directions Zircon cut, monocline scheelite type structure, four directions scheelite type structure, the highest with the photocatalytic activity of monocline scheelite type structure.BiVO prepared by conventional solid-state method4Sample, the shortcoming such as be usually present purity reunion low, easy, granularity is big, specific surface area is low so that it is the separation efficiency in light induced electron and hole is relatively low causes that photocatalysis effect is undesirable.
Summary of the invention
The present invention is directed to existing BiVO4Problems existing in solid phase method preparation, it is provided that a kind of high pressure-hydro-thermal method prepares BiVO4The method of photocatalyst.Can prepare degree of crystallinity height, good dispersion according to method provided by the invention, granularity is little, specific surface area is big, the high catalytic activity BiVO of monocline scheelite-type structure4Photocatalyst.
In order to achieve the above object, the technical solution used in the present invention is: by bismuth nitrate and dodecylbenzene sodium sulfonate ratio 1:(0.01 ~ 0.1 in molar ratio) it is dissolved in ethylene glycol with the solution that volume ratio is 1:1 of water, ammonium metavanadate is dissolved in distilled water；By bismuth: the mol ratio of vanadium is 1:1, is added drop-wise in above-mentioned glycol water by ammonium metavanadate solution, be uniformly mixed and with ammonia regulate solution pH be 3, formed BiVO4Presoma, proceeded in autoclave and passed into any one in nitrogen, oxygen, argon and reached the pressure of 2 ~ 10MPa, 100 ~ 120 DEG C of alcohol-hydrothermal treatment consists 4 ~ 12 hours, centrifugation after cooling, successively with deionized water and absolute ethanol washing, at 80 DEG C, within 4 hours, namely obtain BiVO prepared by a kind of high pressure-hydro-thermal method 450 DEG C of roastings after drying4Photocatalyst.Take 0.1gBiVO4Photocatalyst joins and forms suspension in the methylene blue solution of 100mL10mg/L, dark stirring carried out radiation of visible light after 0.5 ~ 1 hour, took a suspension (4mL) to be centrifuged every 15 minutes, take supernatant on ultraviolet-uisible spectrophotometer, measure the absorbance wherein remaining methylene blue, and calculate corresponding concentration, the relation of the catalyst degradation efficiency to methylene blue and light application time under visible light illumination can be obtained.
Accompanying drawing explanation
Fig. 1 is the X-ray diffracting spectrum of the embodiment of the present invention 1 and 2 products obtained therefrom；
Fig. 2 is the electron scanning micrograph of the embodiment of the present invention 1 products obtained therefrom；
Fig. 3 is the electron scanning micrograph of the embodiment of the present invention 2 products obtained therefrom；
Fig. 4 is the UV-Vis DRS collection of illustrative plates of the embodiment of the present invention 1 and 2 products obtained therefrom；
Fig. 5 is the embodiment of the present invention 1 and 2 products obtained therefrom under visible ray (λ > 420nm) irradiates, the relation of the course of reaction Methylene Blue concentration changes with time of catalytic degradation methylene blue solution.
Detailed description of the invention
Embodiment one:
1) 0.015mol bismuth nitrate (Bi (NO3)3·5H2O) and 0.68 × 10-3MolSDBS is dissolved in the solution that ethylene glycol is 1:1 with water volume ratio；2) 0.015mol ammonium metavanadate (NH4VO3) it is dissolved in distilled water；3) being added drop-wise in bismuth nitrate solution by ammonium metavanadate solution, stirring makes its mix homogeneously, and regulating its pH value with ammonia is 3, forms BiVO4Presoma；4) being proceeded in autoclave by presoma, and sealed reactor, then to nitrogen injection in autoclave, making the pressure gauge reading on autoclave is 4MPa, closes gas check valve, be placed in oil bath pan 110 DEG C react 4 hours；5) successively with deionized water and absolute ethanol washing after cooling, 80 DEG C dry, and by gained powder body 450 DEG C of roastings 4 hours, grind to obtain the BiVO for preparing of a kind of high pressure-hydro-thermal method4Photocatalyst；6) 0.1gBiVO is taken4Photocatalyst is scattered in the methylene blue solution of 100mL10mg/L and forms suspension, dark stirring 1 hour, open xenon lamp (power 300W) and carry out visible ray (λ > 420nm)) irradiate；7) took a suspension (4mL) every 15 minutes to be centrifuged, take supernatant on ultraviolet-uisible spectrophotometer, measure the absorbance wherein remaining methylene blue, and utilize the standard curve of methylene blue solution to calculate corresponding concentration, the relation of the catalyst degradation efficiency to methylene blue and light application time under visible light illumination can be obtained.
Embodiment two:
1) 0.015mol bismuth nitrate (Bi (NO3)3·5H2O) and 0.68 × 10-3MolSDBS is dissolved in the solution that ethylene glycol is 1:1 with water volume ratio；2) 0.015mol ammonium metavanadate (NH4VO3) be dissolved in distilled water；3) being added drop-wise in bismuth nitrate solution by ammonium metavanadate solution, stirring makes its mix homogeneously, and regulating its pH value with ammonia is 3, forms BiVO4Presoma；4) being proceeded in autoclave by presoma, and sealed reactor, then to nitrogen injection in autoclave, making the pressure gauge reading on autoclave is 9MPa, closes gas check valve, be placed in oil bath pan 100 DEG C react 12 hours；5) successively with deionized water and absolute ethanol washing after cooling, 80 DEG C dry, and by gained powder body 450 DEG C of roastings 4 hours, grind to obtain the BiVO for preparing of a kind of high pressure-hydro-thermal method4Photocatalyst；6) 0.1gBiVO is taken4Photocatalyst is scattered in the methylene blue solution of 100mL10mg/L and forms suspension, dark stirring 1 hour, open xenon lamp (power 300W) and carry out visible ray (λ > 420nm)) irradiate；7) took a suspension (4mL) every 15 minutes to be centrifuged, take supernatant on ultraviolet-uisible spectrophotometer, measure the absorbance wherein remaining methylene blue, and utilize the standard curve of methylene blue solution to calculate corresponding concentration, the relation of the catalyst degradation efficiency to methylene blue and light application time under visible light illumination can be obtained.
Claims (3)
1. high pressure-hydro-thermal method prepares BiVO4The method of photocatalyst, is characterised by comprising the steps:
1) bismuth nitrate and dodecylbenzene sodium sulfonate joining ethylene glycol with the solution that volume ratio is 1:1 of water, ammonium metavanadate is dissolved in distilled water；
2) being added drop-wise in above-mentioned glycol water by metavanadate solution and stir, the pH regulating solution with ammonia is 3, forms BiVO4Presoma, proceeded in autoclave and sealed；
3) in autoclave, pass into the gas of 2 ~ 10MPa, close gas check valve, 100 ~ 120 DEG C of alcohol-hydrothermal treatment consists 4 ~ 12 hours, the precipitation and centrifugal separation that will obtain, and successively with deionized water and absolute ethanol washing, dry in 80 DEG C；
4) by the powder body that obtains 450 DEG C of roastings 4 hours, BiVO prepared by a kind of high pressure-hydro-thermal method is namely obtained4Photocatalyst.
2. a kind of high pressure-hydro-thermal method according to claim 1 prepares BiVO4The method of photocatalyst, it is characterised in that: described bismuth: vanadium: the mol ratio of dodecylbenzene sodium sulfonate is 1:1:(0.01 ~ 0.1).
3. a kind of high pressure-hydro-thermal method according to claim 1 prepares BiVO4The method of photocatalyst, it is characterised in that: described gas is any one in oxygen, nitrogen, argon.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107469807A (en) * | 2017-09-08 | 2017-12-15 | 郑州轻工业学院 | A kind of monoclinic phase BiVO4：The high pressure method for preparing of Re catalysis materials |
| CN107626297A (en) * | 2017-09-29 | 2018-01-26 | 中南大学 | A kind of tiny balloon shape bismuth/composite bismuth vanadium photocatalyst and its preparation method and application |
| CN108479750A (en) * | 2018-03-21 | 2018-09-04 | 辽宁石油化工大学 | A kind of preparation method of microspheroidal pucherite catalysis material |
| CN108622934A (en) * | 2018-05-22 | 2018-10-09 | 天津城建大学 | A kind of self assembly micro nano structure BiVO4The simple preparation method of microballoon |
| CN108620056A (en) * | 2017-03-24 | 2018-10-09 | 中国科学院金属研究所 | A kind of active method and its application of regulation and control Aurivillius structure oxide material light catalysis |
| CN111204804A (en) * | 2020-01-15 | 2020-05-29 | 杭州电子科技大学 | BiVO4Preparation method of nano material |
| CN111952578A (en) * | 2020-08-28 | 2020-11-17 | 天津工业大学 | Preparation method of heterojunction structure nanowire for anode of water-based zinc ion battery |
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| CN101746825A (en) * | 2009-12-18 | 2010-06-23 | 北京工业大学 | Organic solvent-water heating method for preparing football-shaped mesoporous BiVO4 |
| CN103801284A (en) * | 2014-01-22 | 2014-05-21 | 浙江大学 | Method for preparing pucherite-graphene composite photocatalyst |
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| CN101746825A (en) * | 2009-12-18 | 2010-06-23 | 北京工业大学 | Organic solvent-water heating method for preparing football-shaped mesoporous BiVO4 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108620056A (en) * | 2017-03-24 | 2018-10-09 | 中国科学院金属研究所 | A kind of active method and its application of regulation and control Aurivillius structure oxide material light catalysis |
| CN108620056B (en) * | 2017-03-24 | 2021-01-19 | 中国科学院金属研究所 | Method for regulating and controlling photocatalytic activity of Aurivillius structure oxide material and application thereof |
| CN107469807A (en) * | 2017-09-08 | 2017-12-15 | 郑州轻工业学院 | A kind of monoclinic phase BiVO4：The high pressure method for preparing of Re catalysis materials |
| CN107469807B (en) * | 2017-09-08 | 2019-10-18 | 郑州轻工业学院 | A kind of monoclinic phase BiVO4: the high pressure method for preparing of Re catalysis material |
| CN107626297A (en) * | 2017-09-29 | 2018-01-26 | 中南大学 | A kind of tiny balloon shape bismuth/composite bismuth vanadium photocatalyst and its preparation method and application |
| CN107626297B (en) * | 2017-09-29 | 2019-09-17 | 中南大学 | A kind of tiny balloon shape bismuth/composite bismuth vanadium photocatalyst and its preparation method and application |
| CN108479750A (en) * | 2018-03-21 | 2018-09-04 | 辽宁石油化工大学 | A kind of preparation method of microspheroidal pucherite catalysis material |
| CN108622934A (en) * | 2018-05-22 | 2018-10-09 | 天津城建大学 | A kind of self assembly micro nano structure BiVO4The simple preparation method of microballoon |
| CN111204804A (en) * | 2020-01-15 | 2020-05-29 | 杭州电子科技大学 | BiVO4Preparation method of nano material |
| CN111952578A (en) * | 2020-08-28 | 2020-11-17 | 天津工业大学 | Preparation method of heterojunction structure nanowire for anode of water-based zinc ion battery |
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