CN111203244B - WO (WO) 3 Preparation method of BiOBr photocatalytic nano material - Google Patents
WO (WO) 3 Preparation method of BiOBr photocatalytic nano material Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 17
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 125000002091 cationic group Chemical group 0.000 claims abstract description 10
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 10
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 10
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 claims description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 4
- 229940043267 rhodamine b Drugs 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 description 1
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 239000008852 wen-xin Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a WO 3 A preparation method of BiOBr photocatalysis nano material. The invention adopts hydrophilic high molecular polymer sodium polyacrylate and cationic polyacrylamide to form gel in aqueous solution by crosslinking, thereby limiting WO 3 The growth of BiOBr material can obtain WO with the size of 12-18 nm and good dispersibility 3 the/BiOBr nano material has excellent performance of catalyzing and degrading rhodamine B.
Description
Technical Field
The invention belongs to the technical field of nano composite materials, relates to preparation of a visible light response photocatalyst, and particularly relates to WO 3 A preparation method of BiOBr photocatalysis nano material.
Background
The photocatalysis technology has the advantages of mild reaction conditions, high degradation efficiency, simple and convenient operation, no secondary pollution, capability of utilizing sunlight as a reaction light source and the like, and is a water treatment technology with wide prospect. Semiconductor photocatalysts such as TiO 2 And ZnO and the like are widely applied to catalytic degradation of organic matters, but can only absorb ultraviolet light accounting for less than 5% of sunlight due to high forbidden energy level, and has poor response to visible light. Bismuth has a unique 6S 2 The outer layer is electronically configured to have a forbidden band width that is easily excited by the visible light. Particularly, the heterojunction composite material of the BiOBr group can effectively improve the separation efficiency of the photo-generated electron-hole pair and improve the oxidation-reduction capability of the catalyst. The WO is prepared by taking bismuth nitrate pentahydrate, bismuth bromide and tungstic acid as raw materials, adjusting the pH to be =10.3 by NH 3. H2O, and adopting a hydrothermal reaction at the temperature of 100 ℃/6H under the condition of industrial catalysis, namely environment college Caojiang university, wangliqiong, yellow cedronson, li Wenxin, chenjian forest and the like (industrial catalysis, 8 th stage of 2018, 79-82 pages) 3 /BiOBr composite nano material. But the WO obtained 3 The BiOBr aggregates together and has poor dispersion effect in an aqueous solution, so that the catalytic performance of the catalyst is severely limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a WO 3 A preparation method of a BiOBr photocatalytic nano material.
One WO of the present invention 3 The preparation method of the BiOBr photocatalytic nano material comprises the following specific steps:
1) Weighing 0.01-0.03 mol of Bi (NO) 3 ) 3 ·5H 2 O and equimolar KBr are added into 50 to 100ml of deionized water, and then Bi (NO) is obtained through ultrasonic dispersion 3 ) 3 Mixed solution with KBr.
2) Weighing 0.002-0.006 mol of H 2 WO 4 Adding the mixture into 50 to 100ml of deionized water, and obtaining H by ultrasonic dispersion 2 WO 4 A solution;
3) Under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 9-10 by O; then 0.5-1.0 g of sodium polyacrylate and 0.01-0.03 g of cationic polyacrylamide are respectively added. Transferring the obtained solution into a stainless steel reaction kettle, and reacting for 8-12 h at the temperature of 100-140 ℃. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 a/BiOBr nano material.
The molecular formula of the cationic polyacrylamide is ([ CH) 2 CH(CONH 2 )] m [(CH 2 CH)COO-CH 2 CH 2 N + (CH 3 ) 3 Cl] n ) Molecular weight is 100-300 ten thousand;
the molecular weight of the sodium polyacrylate is 500-700 ten thousand.
The invention adopts hydrophilic high molecular polymer sodium polyacrylate and cationic polyacrylamide to form gel through crosslinking in aqueous solution, thereby limiting WO 3 The growth of BiOBr material can obtain WO with the size of 12-18 nm and good dispersibility 3 the/BiOBr nano material has excellent performance of catalyzing and degrading rhodamine B.
Detailed Description
The present invention is further analyzed with reference to the following specific examples.
Comparative example 1
0.01mol of Bi (NO) is weighed 3 ) 3 ·5H 2 O and 0.01mol of KBr are added into 50ml of deionized water, and the mixture is subjected to ultrasonic dispersion to obtain Bi (NO) 3 ) 3 Mixed solution with KBr.
0.002mol of H is weighed 2 WO 4 Adding into 50ml deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 9 by O; the resulting solution was then transferred to a stainless steel reaction kettle and reacted at a temperature of 100 ℃ for 12h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 a/BiOBr nano material.
Example 1:
0.01mol of Bi (NO) is weighed 3 ) 3 ·5H 2 O and 0.01mol KBr are added into 50ml deionized water, and then Bi (NO) is obtained by ultrasonic dispersion 3 ) 3 Mixed solution with KBr.
0.002mol of H is weighed 2 WO 4 Adding into 50ml deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 9 by O; then 0.5g of sodium polyacrylate and 0.01g of cationic polyacrylamide were added, respectively. The obtained solution is transferred into a stainless steel reaction kettle and reacted for 12 hours at the temperature of 100 ℃. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 /BiOBr nano material.
Example 2:
weighing 0.03mol of Bi (NO) 3 ) 3 ·5H 2 O and 0.03mol of KBr are added into 100ml of deionized water, and the mixture is subjected to ultrasonic dispersion to obtain Bi (NO) 3 ) 3 Mixed solution with KBr.
0.006mol of H is weighed 2 WO 4 Adding into 100ml deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 10; then 1.0g of sodium polyacrylate and 0.03g of cationic polyacrylamide were added, respectively. The resulting solution was transferred to a stainless steel reactor at a temperature of 14 deg.CThe reaction time is 8h at 0 ℃. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 /BiOBr nano material.
Example 3:
0.02mol of Bi (NO) is weighed 3 ) 3 ·5H 2 O and 0.02mol of KBr are added into 80ml of deionized water, and the mixture is subjected to ultrasonic dispersion to obtain Bi (NO) 3 ) 3 Mixed solution with KBr.
0.004mol of H is weighed 2 WO 4 Adding into 80ml deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 9.5 by O; then 0.8g of sodium polyacrylate and 0.02g of cationic polyacrylamide were added, respectively. The obtained solution is transferred to a stainless steel reaction kettle and reacted for 10 hours at the temperature of 120 ℃. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 a/BiOBr nano material.
Example 4:
0.01mol of Bi (NO) is weighed 3 ) 3 ·5H 2 O and 0.01mol of KBr are added into 100ml of deionized water, and the mixture is subjected to ultrasonic dispersion to obtain Bi (NO) 3 ) 3 Mixed solution with KBr.
0.003mol of H are weighed 2 WO 4 Adding into 100ml deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 10 by O; then 0.6g of sodium polyacrylate and 0.02g of cationic polyacrylamide were added, respectively. The resulting solution was transferred to a stainless steel reaction kettle and reacted at a temperature of 130 ℃ for 9h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain WO 3 /BiOBr nano material.
Photocatalytic degradation experiment
A300W xenon lamp is used as a light source, and a filter is arranged between the light source and the reactor to filter ultraviolet light below 420 nm. 20mg of the catalyst WO obtained in comparative example 1 and examples 1 to 4 were weighed out 3 the/BiOBr is added into 100mL of rhodamine B solution at the concentration of 5mg/L, a light source is arranged above a reaction kettle, and the distance between the light source and the liquid level of the RhB solution in the reaction kettle is fixed to be 6.5cm. Stirring in dark for 30min to disperse and adsorb the sample. The light source was then turned on and the magnetic stirring was continued, maintaining the temperature at 25 ℃. Detecting the change of the RhB concentration in the solution by adopting an ultraviolet-visible spectrometer, and calculating the degradation rate of RhB according to the formula: (Co-C)/Co 100%.
TABLE 1 catalyst WO 3 Catalytic degradation rate of BiOBr on rhodamine B under visible light
Claims (1)
1. WO (WO) 3 The preparation method of the BiOBr photocatalytic nano material is characterized by comprising the following steps:
1) Weighing 0.01-0.03 mol of Bi (NO) 3 ) 3 ·5H 2 O and KBr with equal molar weight are added into 50 to 100ml of deionized water, and then Bi (NO) is obtained by ultrasonic dispersion 3 ) 3 Mixed solution with KBr;
2) Weighing 0.002-0.006 mol of H 2 WO 4 Adding the mixture into 50 to 100ml of deionized water, and performing ultrasonic dispersion to obtain H 2 WO 4 A solution;
3) Under magnetic stirring, the above Bi (NO) is added 3 ) 3 Mixed solution with KBr and H 2 WO 4 Mixing the solution with NH 3 ·H 2 Adjusting the pH value to 9-10 by O; then respectively adding 0.5-1.0 g of sodium polyacrylate and 0.01-0.03 g of cationic polyacrylamide; transferring the obtained solution into a stainless steel reaction kettle, and reacting for 8-12 h at the temperature of 100-140 ℃; after the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the productWO 3 A BiOBr nanomaterial;
the molecular formula of the cationic polyacrylamide is [ CH ] 2 CH(CONH 2 )] m [(CH 2 CH)COO-CH 2 CH 2 N + (CH 3 ) 3 Cl] n The molecular weight is 100-300 ten thousand;
the molecular weight of the sodium polyacrylate is 500-700 ten thousand.
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| CN111589460B (en) * | 2020-06-03 | 2022-09-23 | 哈尔滨理工大学 | W 18 O 49 BiOX composite photocatalytic material and preparation method thereof |
| CN111939948A (en) * | 2020-09-01 | 2020-11-17 | 陕西科技大学 | BiOCl-WO3Preparation method of composite photocatalyst |
| CN112619672A (en) * | 2021-01-27 | 2021-04-09 | 福州大学 | Silicon-doped tungsten trioxide bismuth oxyhalide composite photocatalytic material and preparation method thereof |
| CN115299491A (en) * | 2022-07-20 | 2022-11-08 | 武汉职业技术学院 | Bionic preservative film coating for clean poultry eggs and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103657692A (en) * | 2013-11-22 | 2014-03-26 | 华东师范大学 | Compound bismuthyl bromide photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657692A (en) * | 2013-11-22 | 2014-03-26 | 华东师范大学 | Compound bismuthyl bromide photocatalyst |
Non-Patent Citations (2)
| Title |
|---|
| WO3/BiOBr复合催化剂的制备及其可见光催化活性研究;王莉琼;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20170915(第9期);第2.3.2.1节及第2.4.2.4节 * |
| 粒径可控的纳米铁酸铋的制备及其光催化性能;县涛等;《催化学报》;20110420;第32卷(第4期);第619-623页 * |
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