CN102553619A - Visible-light catalyst Bi3O4Br and preparation method thereof - Google Patents
Visible-light catalyst Bi3O4Br and preparation method thereof Download PDFInfo
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- CN102553619A CN102553619A CN2011104357870A CN201110435787A CN102553619A CN 102553619 A CN102553619 A CN 102553619A CN 2011104357870 A CN2011104357870 A CN 2011104357870A CN 201110435787 A CN201110435787 A CN 201110435787A CN 102553619 A CN102553619 A CN 102553619A
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- quaternary ammonium
- bismuth
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- ammonium salt
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Abstract
Provided are a visible-light catalyst Bi3O4Br and a preparation method thereof. The method comprises adding deionized water, bismuth salt and quaternary ammonium salt into a reaction kettle to obtain the bismuth salt with concentration of 0.02-0.04 molar/liter and the quaternary ammonium salt with concentration of 0.02-0.05 molar/liter, wherein the molar ratio of the bismuth salt to the quaternary ammonium salt is larger than or equal to one; adding caustic soda solution with concentration of 1 molar/liter into the mixture with stirring to regulate potential of hydrogen (pH) to be 11.0-12.5; stirring and performing hydro-thermal treatment at the treatment temperature of 160-180 DEG C; after keeping the constant temperate for 12-18 hours, centrifugally separating solid products; respectively washing the obtained solid products through the deionized water and absolute ethyl alcohol for at least three times; and drying the products at the temperature of 50 DEG C for at least 6 hours to obtain light-yellow Bi3O4Br solid powder. The Bi3O4Br has good visible-light activity and can have strong degradation to various pollutants under the irradiation of the visible light. In addition, the method is simple in synthesis, the whole synthesis process is easy to control, raw materials are easily obtained, and the cost is low.
Description
Technical field
The present invention relates to a kind of novel visible catalyst bromine oxygen bismuth and preparation method thereof, particularly Bi
3O
4Br and preparation method thereof.
Background technology
Photocatalysis is the research field of rising gradually after nineteen seventies, and the photochemical catalyst of based semiconductor material mainly is because their extensive utilizations in the solar energy conversion and the depollution of environment in recent years by broad research.As everyone knows, very big ratio is because visible light is formed in the solar spectrum, and the Preparation of Catalyst and the research that therefore have visible light activity receive much concern.We know; Widely used titanium dioxide only has activity at ultraviolet region; In order to improve its visible light activity, the researcher is with mixing or ion implantation method comes modified titanic oxide, mixes usually also as the activated centre in light induced electron and hole; But the material that mixes often exists thermodynamic phase, and the process of mixing needs precious metal ion usually.Therefore many researchs have concentrated on design and have developed the photochemical catalyst that does not have oxide that mix, not single-phase and have visible light activity.
Oxyhalogen bismuth series is extremely important, BiOX (X, Cl; Br; I), because they have unique chemical property, magnetic, optical property and fluorescent characteristics, and they are being showed the treatment ability of microcosmic cancer and the good catalytic activity and the ability of selective oxidation coupling methane reaction.All oxyhalogen bismuths all are cubic configurations, are by [Bi
2O
2] structure of layer and the interlaced accumulation of halogen atom a kind of stratiform of getting up.They are used as the organic matter in the waste water that very strong photochemical catalyst is used for decomposing dye discoloration.For example Zhang seminar once reported BiOCl has better photocatalysis performance [Zhang, K.L. when the photocatalytic degradation methyl orange compared with P25; Liu, C.M.; Huang, F. Q.; Zheng, C.; Wang, W.D., Appl.Catal.B.2006,68,125].Yet for the oxyhalogen bismuth of layer structure, the relation of their structure and performance and light-catalysed potential are to be worth further research.
In the present invention, the applicant takes hydrothermal reaction at low temperature to control not homoatomic metering ratio in the oxyhalogen bismuth, thereby effectively improves the photocatalysis performance of catalyst, and this reaction is carried out at low temperatures, without any need for the heat treatment subsequent step.And the Bi that reaction obtains
3O
4The Br photochemical catalyst has good visible light catalysis activity, under radiation of visible light, can realize rhodamine B 100% degraded.Whole production technology is simple, operation easily, and synthesis temperature is low, and reaction yield is up to 91%, and industrial amplification factor is little, for the large-scale production visible light catalyst provides an effective way.
Summary of the invention
The object of the invention aims to provide a kind of not bismuth oxybromide visible light catalyst that mix, single-phase and preparation method thereof, and a kind of hydrothermal reaction at low temperature synthesizes Bi
3O
4The preparation method of Br visible light catalyst, its method are dissolved in bismuth salt and quaternary ammonium salt in the water, regulate the pH value to certain limit, can obtain corresponding Bi after handling through hydrothermal synthesis method then
3O
4The Br visible light catalyst.
The present invention adopts following technical scheme for realizing above-mentioned purpose:
A kind of visible-light photocatalyst Bi
3O
4The preparation method of Br, its preparation process is followed successively by:
Step 1: in agitated reactor, add deionized water, bismuth salt and quaternary ammonium salt; The concentration that is made into bismuth salt is 0.02～0.04 mol; The concentration of quaternary ammonium salt is 0.02～0.05 mol, and the mol ratio of quaternary ammonium salt and bismuth salt is more than or equal to 1, and described bismuth salt is five water bismuth nitrates; Described quaternary ammonium salt is a softex kw;
Step 2: in the agitated reactor of step 1, adding concentration is sodium hydroxide solution adjusting pH to 11.0～12.5 of 1 mol, stirs to be no less than 0.5 hour, carries out hydrothermal treatment consists then, and treatment temperature is 160～180 ℃, constant temperature 12～18 hours;
Step 3: after step 2 finished, the centrifugation solid product washed gained solid matter with deionized water and absolute ethyl alcohol respectively and to be no less than 3 times, and product is no less than 6 hours 50 ℃ of dryings then, promptly obtains flaxen Bi
3O
4The Br pressed powder.It is Bi
3O
4The Br nanometer sheet, size has good visible light catalysis activity tens to the hundreds of nanometer, under radiation of visible light, can have greater than 99.5% near 100% degraded rhodamine B in 20 minutes.
The invention has the advantages that:
1, the synthetic Bi of hydrothermal reaction at low temperature
3O
4The Br visible light catalyst.
2, the Bi that synthesizes
3O
4The Br visible light catalyst has good visible light catalysis activity, under radiation of visible light, can have near 100% degraded rhodamine B.
3, whole process of preparation is carried out under cryogenic conditions, and technical process is very easy to operation, and industrial amplification factor is little; And synthesis temperature is low, without any need for the heat treatment subsequent step, meets very much demand of practical production.
Description of drawings
Fig. 1, be prepared Bi
3O
4The XRD figure spectrum of Br
The picture in picture spectrum is corresponding to Bi
3O
4Br meets standard card JCPDS No.84-793.
Fig. 2 is prepared Bi
3O
4The TEM figure of Br
As can be seen from the figure this Bi
3O
4Br is made up of nanometer sheet, and size arrives the hundreds of nanometer tens.
Fig. 3 is prepared Bi
3O
4The uv drs spectrum of Br
As can be seen from the figure, Bi
3O
4Br has certain absorption from the ultraviolet region to the visible region, and the absorption maximum edge is in 470 nanometers.
Fig. 4 is Bi under the radiation of visible light
3O
4Br is for the degradation curve of rhodamine B.
As can beappreciated from fig. 4, the prepared Bi of the present invention
3O
4Br compares with Degussa (P25) and to have better visible light degrading activity, under radiation of visible light, can realize 100% degraded approaching to pollutant in 20 minutes.
The specific embodiment
The present invention further specifies through following embodiment.
Embodiment 1
Bi
3O
4The Br preparation, its preparation process is followed successively by:
Step 1: in the 150mL agitated reactor, add deionized water, bismuth salt and quaternary ammonium salt; The concentration that is made into bismuth salt is 0.02～0.04 mol; The concentration of quaternary ammonium salt is 0.02～0.05 mol, and the mol ratio of quaternary ammonium salt and bismuth salt is more than or equal to 1, and described bismuth salt is five water bismuth nitrates; Described quaternary ammonium salt is a softex kw;
Step 2: in the agitated reactor of step 1, adding concentration is sodium hydroxide solution adjusting pH to 11.0～12.5 of 1 mol, stirs to be no less than 0.5 hour, carries out hydrothermal treatment consists then, and treatment temperature is 160～180 ℃, constant temperature 12～18 hours;
Step 3: after step 2 finished, the centrifugation solid product washed gained solid matter with deionized water and absolute ethyl alcohol respectively and to be no less than 3 times, and product is no less than 6 hours 50 ℃ of dryings then, promptly obtains flaxen Bi
3O
4The Br pressed powder.
Embodiment 2
Bi
3O
4The Br preparation, preparation process is:
Step 1: in the 150mL agitated reactor, add the 50mL deionized water, add five water bismuth nitrate and softex kws, the concentration that makes bismuth nitrate is 0.02 mol, and the concentration of softex kw is 0.027 mol;
Step 2: the mixed solution normal temperature of step 1 stirred 10 minutes down, and using the NaOH adjusting pH of 1 mol is 11, stirs 1 hour, then mixed solution is carried out hydrothermal treatment consists, and treatment temperature is 160 ℃, constant temperature 18 hours;
Step 3: after step 2 finished, the centrifugation solid product respectively washed gained solid matter with deionized water and absolute ethyl alcohol 3 times, and product promptly obtains flaxen Bi 50 ℃ of dryings 6 hours
3O
4The Br pressed powder.
Embodiment 3
Bi
3O
4The Br preparation, preparation process is:
Step 1: in the 150mL agitated reactor, add the 50mL deionized water, add five water bismuth nitrate and softex kws, the concentration that makes bismuth nitrate is 0.03 mol, and the concentration of softex kw is 0.04 mol;
Step 2: the mixed solution normal temperature of step 1 stirred 10 minutes down, and using the NaOH adjusting pH of 1 mol is 12.5, stirs 1 hour, then mixed solution is carried out hydrothermal treatment consists, and treatment temperature is 180 ℃, constant temperature 18 hours;
Step 3: after step 2 finished, the centrifugation solid product respectively washed gained solid matter with deionized water and absolute ethyl alcohol 3 times, and product promptly obtains flaxen Bi 50 ℃ of dryings 6 hours
3O
4The Br pressed powder.
Embodiment 4
Bi
3O
4The Br preparation, preparation process is:
Step 1: in the 150mL agitated reactor, add the 50mL deionized water, add five water bismuth nitrate and softex kws, the concentration that makes bismuth nitrate is 0.04 mol, and the concentration of softex kw is 0.05 mol;
Step 2: the mixed solution normal temperature of step 1 stirred 10 minutes down, and using the NaOH adjusting pH of 1 mol is 11.3, stirs 1 hour, then mixed solution is carried out hydrothermal treatment consists, and treatment temperature is 160 ℃, constant temperature 24 hours;
Step 3: after step 2 finished, the centrifugation solid product washed gained solid matter with deionized water and absolute ethyl alcohol respectively 3 times, and product promptly obtains flaxen Bi 50 ℃ of dryings 6 hours
3O
4The Br pressed powder.
The XRD figure spectrum of the product that the foregoing description 1-4 makes is like Fig. 1, it is thus clear that meet the Bi of standard card JCPDS No.84-793
3O
4Br.The TEM of product schemes like Fig. 2, as can be seen from the figure this Bi
3O
4Br is made up of nanometer sheet, and size arrives the hundreds of nanometer tens.Product B i
3O
4Uv drs spectrum such as Fig. 3 of Br, as can be seen from the figure, Bi
3O
4Br has certain absorption from the ultraviolet region to the visible region, and the absorption maximum edge is in 470 nanometers.
Product B i under the radiation of visible light
3O
4Br is for degradation curve such as Fig. 4 of rhodamine B, as can beappreciated from fig. 4, and the Bi that the present invention is prepared
3O
4Br compares with Degussa (P25) and to have better visible light degrading activity, under radiation of visible light, can realize 100% degraded approaching to pollutant in 20 minutes.
Claims (2)
1. a visible-light photocatalyst bismuth oxybromide is characterized in that, it is Bi
3O
4Br nanometer sheet, size be tens to the hundreds of nanometer, under radiation of visible light, can have greater than 99.5% near 100% degraded rhodamine B in 20 minutes.
2. visible-light photocatalyst Bi
3O
4The preparation method of Br is characterized in that preparation process is followed successively by:
Step 1: in agitated reactor, add deionized water, bismuth salt and quaternary ammonium salt; The concentration that is made into bismuth salt is 0.02～0.04 mol; The concentration of quaternary ammonium salt is 0.02～0.05 mol, and the mol ratio of quaternary ammonium salt and bismuth salt is more than or equal to 1, and described bismuth salt is five water bismuth nitrates; Described quaternary ammonium salt is a softex kw;
Step 2: in the agitated reactor of step 1, adding concentration is sodium hydroxide solution adjusting pH to 11.0～12.5 of 1 mol, stirs to be no less than 0.5 hour, carries out hydrothermal treatment consists then, and treatment temperature is 160～180 ℃, constant temperature 12～18 hours;
Step 3: after step 2 finished, the centrifugation solid product washed gained solid matter with deionized water and absolute ethyl alcohol respectively and to be no less than 3 times, and product is no less than 6 hours 50 ℃ of dryings then, promptly obtains flaxen Bi
3O
4The Br pressed powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597794A (en) * | 2015-12-23 | 2016-05-25 | 镇江市高等专科学校 | Composite visible light photocatalyst and preparation method thereof |
| CN106861724A (en) * | 2017-03-24 | 2017-06-20 | 中南民族大学 | A kind of preparation method of square cavernous structure Bi3O4Br nanometer monocrystallines ring catalysis material |
| CN108262050A (en) * | 2018-01-03 | 2018-07-10 | 东南大学 | A kind of two dimension composite visible light catalyst and preparation method and application |
| CN109364958A (en) * | 2018-12-11 | 2019-02-22 | 江南大学 | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst |
| CN111482186A (en) * | 2020-04-15 | 2020-08-04 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN113275023A (en) * | 2021-05-28 | 2021-08-20 | 南开大学 | Bi3O4Br/CuBi2O4Preparation method and application of bimetallic heterojunction catalyst |
| CN115337941A (en) * | 2022-08-09 | 2022-11-15 | 河南科技大学 | Photocatalytic fresh-keeping material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811733A (en) * | 2009-12-04 | 2010-08-25 | 华中师范大学 | Visible light-responded basic bismuth bromide nanostructured microsphere material and preparation method thereof |
-
2011
- 2011-12-22 CN CN2011104357870A patent/CN102553619A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811733A (en) * | 2009-12-04 | 2010-08-25 | 华中师范大学 | Visible light-responded basic bismuth bromide nanostructured microsphere material and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| 《Chem. Eur. J.》 20051231 Hong Deng et. al. "Controlled Hydrothermal Synthesis of Bismuth Oxyhalide Nanobelts and Nanotubes" 第6519-6524页 , 第11期 * |
| 《International Journal of Nanotechnology》 20071231 WT Yao et. al. "Recent advances in hydrothermal syntheses of low dimensional nanoarchitectures" 第129-162页 第4卷, 第1-2期 * |
| 《洁净煤技术》 20081231 杨帆 等 "环境友好的BiOBr新型光催化剂制备、表征及其性能研究" 第47-48页 , 第6期 * |
| HONG DENG ET. AL.: ""Controlled Hydrothermal Synthesis of Bismuth Oxyhalide Nanobelts and Nanotubes"", 《CHEM. EUR. J.》 * |
| WT YAO ET. AL.: ""Recent advances in hydrothermal syntheses of low dimensional nanoarchitectures"", 《INTERNATIONAL JOURNAL OF NANOTECHNOLOGY》 * |
| 杨帆 等: ""环境友好的BiOBr新型光催化剂制备、表征及其性能研究"", 《洁净煤技术》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597794A (en) * | 2015-12-23 | 2016-05-25 | 镇江市高等专科学校 | Composite visible light photocatalyst and preparation method thereof |
| CN106861724A (en) * | 2017-03-24 | 2017-06-20 | 中南民族大学 | A kind of preparation method of square cavernous structure Bi3O4Br nanometer monocrystallines ring catalysis material |
| CN106861724B (en) * | 2017-03-24 | 2019-09-10 | 中南民族大学 | A kind of preparation method of rectangular cavernous structure Bi3O4Br nanometer monocrystalline ring catalysis material |
| CN108262050A (en) * | 2018-01-03 | 2018-07-10 | 东南大学 | A kind of two dimension composite visible light catalyst and preparation method and application |
| CN108262050B (en) * | 2018-01-03 | 2020-06-30 | 东南大学 | Two-dimensional composite visible light catalyst and preparation method and application thereof |
| CN109364958A (en) * | 2018-12-11 | 2019-02-22 | 江南大学 | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst |
| CN111482186A (en) * | 2020-04-15 | 2020-08-04 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN111482186B (en) * | 2020-04-15 | 2022-04-01 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN113275023A (en) * | 2021-05-28 | 2021-08-20 | 南开大学 | Bi3O4Br/CuBi2O4Preparation method and application of bimetallic heterojunction catalyst |
| CN115337941A (en) * | 2022-08-09 | 2022-11-15 | 河南科技大学 | Photocatalytic fresh-keeping material and preparation method and application thereof |
| CN115337941B (en) * | 2022-08-09 | 2023-07-07 | 河南科技大学 | Photocatalytic fresh-keeping material and preparation method and application thereof |
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Application publication date: 20120711 |