CN107803210B - One-step method for preparing Bi with excellent photocatalytic performance2S3Method for preparing/BiOCl heterojunction - Google Patents
One-step method for preparing Bi with excellent photocatalytic performance2S3Method for preparing/BiOCl heterojunction Download PDFInfo
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- CN107803210B CN107803210B CN201610810768.4A CN201610810768A CN107803210B CN 107803210 B CN107803210 B CN 107803210B CN 201610810768 A CN201610810768 A CN 201610810768A CN 107803210 B CN107803210 B CN 107803210B
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 35
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 34
- 239000004202 carbamide Substances 0.000 claims abstract description 18
- 239000011780 sodium chloride Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 22
- 239000007864 aqueous solution Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 13
- 238000006731 degradation reaction Methods 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 11
- 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 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960003887 dichlorophen Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
- 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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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a one-step method for preparing Bi with excellent photocatalytic performance2S3A method of forming a/BiOCl heterojunction comprising the steps of: adding Bi (NO)3)3·5H2O, NaCl and thioacetamide are co-dissolved in an aqueous solution of urea; stirring for 4-5 hours at room temperature; after the reaction is finished, washing is carried out to obtain Bi2S3a/BiOCl heterojunction photocatalyst. Bi obtained by the method of the invention2S3a/BiOCl heterojunction with a large specific surface area and Bi2S3Can achieve microscopic close contact with BiOCl, and thus has more excellent photocatalytic degradation dye decomposition activity than a single material, and shows that the material has better application prospect in the aspect of removing pollutants such as dye in industrial wastewater.
Description
Technical Field
The present invention relates to Bi having excellent photocatalytic properties2S3a/BiOCl heterojunction and a preparation method thereof, in particular to a method for preparing Bi by adopting a one-step method2S3A method of a BiOCl heterojunction belongs to the field of inorganic nano material preparation.
Background
In recent years, a single photocatalyst is narrow in light absorption range, so that photo-generated electrons and holes are easy to recombine, and the photocatalytic performance cannot meet the actual industrial requirements. The heterojunction photocatalyst can enlarge the light absorption range and effectively prevent the recombination of photo-generated electrons and holes, so that the photocatalytic performance can be improved, and the heterojunction photocatalyst is more and more concerned.
With the development of industry, dyes and organic pollutants have become major environmental pollutants. The removal of pollutants by photocatalysis and the full use of green sunlight as an energy source have become one of the most important methods for removing pollutants. BiOCl may become a novel photocatalytic material due to its low or non-toxic, layered structure characteristics and excellent ultraviolet and visible light catalytic activity. However, when a single material is used as a photocatalyst, the defects of narrow light absorption range, low visible light utilization rate, easy recombination of carriers and the like exist, and Bi with photosensitive performance is obtained2S3After the photocatalyst is compounded with BiOCl to form a heterojunction, the photocatalytic performance is greatly improved.
Bi2S3the/BiOCl heterojunction has excellent photocatalytic performance, the Baibiao Huang and the like firstly prepare BiOCl by a hydrothermal method, and then prepare Bi by an ion exchange method at room temperature2S3A BiOCl heterojunction, research on the Bi produced2S3The photocatalysis performance of 2, 4-dichlorophen catalyzed and decomposed by a/BiOCl heterojunction. At present, Bi is not prepared by a one-step method2S3the/BiOCl heterojunction photocatalyst is reported.
Disclosure of Invention
The object of the present invention is to provide a Bi having excellent photocatalytic properties2S3A preparation method of a BiOCl heterojunction.
The technical solution for realizing the purpose of the invention is as follows: one-step method for preparing photocatalystBi having excellent conversion properties2S3A method of forming a/BiOCl heterojunction comprising the steps of: adding Bi (NO)3)3·5H2O, NaCl and Thioacetamide (TAA) are dissolved in the urea solution to obtain reaction solution, and the reaction is carried out at normal temperature; after the reaction is finished, washing is carried out to obtain Bi2S3a/BiOCl heterojunction.
In the above step, Bi (NO)3)3·5H2The molar concentration of O in the reaction solution was 2/3 mol/L.
In the above step, the molar concentration of the urea solution is 5.5-5.6 mol/L.
In the above step, the molar concentration of NaCl in the reaction solution was 2/3 mol/L.
In the above step, the molar ratio of thioacetamide to NaCl is 0.20-0.30.
In the above steps, the reaction time is 4-5 h.
Compared with the prior art, the invention has the following remarkable advantages:
1. the method is simple, no template agent is required to be added, and Bi is obtained by one-step reaction at room temperature2S3a/BiOCl heterojunction photocatalyst;
2. prepared Bi2S3the/BiOCl heterojunction has larger specific surface area;
3. the Bi2S3the/BiOCl heterojunction photocatalyst shows excellent catalytic performance on degradation of rhodamine B under the excitation of visible light, is 3.3 times higher than that of a single photocatalyst BiOCl, and is expected to have good application in the field of industrial wastewater treatment.
Drawings
FIG. 1 shows a one-step method for preparing Bi according to the present invention2S3Schematic flow diagram of/BiOCl heterojunction photocatalyst.
FIG. 2 shows Bi obtained in example 12S3TEM images of/BiOCl heterojunction photocatalysts and BiOCl prepared by comparative example, wherein (a) comparative example 3; (b) and (c) example 1; (d) comparative example 4.
FIG. 3 shows that Bi is obtained by the present invention2S3Degradation rate diagram of/BiOCl heterojunction photocatalyst for rhodamine B。
FIG. 4 shows comparative examples of different sulfur sources such as Na2Bi prepared when S and thiourea are used as sulfur source2S3A degradation rate graph of/BiOCl on rhodamine B.
FIG. 5 shows the amount of urea in comparative example versus Bi produced2S3Influence diagram of/BiOCl catalyzing degradation of rhodamine B.
FIG. 6 shows comparative example reaction time vs. Bi produced2S3Influence diagram of/BiOCl catalyzing degradation of rhodamine B.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
With reference to FIG. 1, the invention uses urea as a solvent to prepare Bi with excellent photocatalytic performance2S3The method for preparing the/BiOCl heterojunction photocatalyst is characterized by comprising the following steps:
the method comprises the following steps: adding Bi (NO)3)3·5H2O, NaCl and TAA in an aqueous urea solution, Bi (NO)3)3·5H2The molar concentration of O is 2/3mol/L, the molar concentration of urea is 5.5 +/-0.1 mol/L, the molar concentration of NaCl is 2/3mol/L, and the molar ratio of TAA to NaCl is 0.3 +/-0.5;
step two: placing the solution in the step one in a beaker to react for 4-5 h at room temperature;
step three: after the reaction is finished, washing is carried out to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The invention is explained in more detail below with reference to examples, comparative examples and the accompanying drawings:
example 1:
the method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O, 2mmol NaCl and 0.5mmol TAA in 30 ml of an aqueous solution containing 166mmol urea;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 5 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The transmission electron microscope picture 2 of the obtained product shows that the product is a nanosheet.
The experimental results of the degradation rate of the RhB solution in fig. 3 show that: under the excitation of visible light, the degradation rate reaches 98 percent within 20 min. Than without adding Bi2S3The activity of single BiOCl is improved by 3.3 times. Comparative example 1: (influence of Sulfur Source-Na2S）
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O、2 mmol NaCl、0.5mmol Na2S is dissolved in 30 ml of aqueous solution containing 166mmol of urea;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 5 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The photocatalytic performance of the resulting product is shown in fig. 4.
Comparative example 2: (influence of Sulfur Source-Thiourea)
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O, 2mmol NaCl and 0.5mmol thiourea were dissolved in 30 ml of an aqueous solution containing 166mmol urea; (ii) a
Step two: reacting the solution obtained in the step one in a beaker at room temperature for 5 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The photocatalytic performance of the resulting product is shown in fig. 4.
Comparative example 3: (Effect of Urea-0)
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2Dissolving O, 2mmol NaCl and 0.5mmol TAA in 30 ml water solution;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 5 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The transmission electron microscope picture of the obtained product is shown in figure 2, and the photocatalytic performance is shown in figure 5.
The photocatalytic performance of the obtained product shows that the degradation rate of RhB within 20min is 30% when urea is not added.
Comparative example 4: (Effect of Urea-60)
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O, 2mmol NaCl and 0.5mmol TAA in 30 ml of an aqueous solution containing 60mmol urea;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 5 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The transmission electron microscope picture of the obtained product is shown in fig. 2, and the photocatalytic performance of the obtained product is shown in fig. 5. The photocatalytic performance of the obtained product shows that when 60mmol of urea is added, the degradation rate of rhodamine B in 20min is 80%. The degradation rate was not as high as that of 166mmol of urea. Comparative example 5: (influence of reaction time-3 h)
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O, 2mmol NaCl and 0.5mmol TAA in 30 ml of an aqueous solution containing 166mmol urea;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 3 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The photocatalytic performance of the obtained product is shown in FIG. 6, and the degradation rate is not as high as 5 h.
Comparative example 6: (influence of reaction time-6 h)
The method comprises the following steps: 2mmol of Bi (NO)3)3·5H2O, 2mmol NaCl and 0.5mmol TAA in 30 ml of an aqueous solution containing 166mmol urea;
step two: reacting the solution obtained in the step one in a beaker at room temperature for 6 hours;
step three: washing the product obtained in the step two to obtain Bi2S3a/BiOCl heterojunction photocatalyst.
The photocatalytic performance of the obtained product is shown in FIG. 6, and the degradation rate is not as high as 5 h.
Claims (6)
1. One-step method for preparing Bi with excellent photocatalytic performance2S3A method of forming a/BiOCl heterojunction, comprising the steps of: adding Bi (NO)3)3·5H2O, NaCl and thioacetamide are dissolved in urea solution to obtain reaction solution, and the reaction solution is reacted at normal temperature; after the reaction is finished, washing is carried out to obtain Bi2S3a/BiOCl heterojunction.
2. The method of claim 1, wherein Bi (NO)3)3·5H2The molar concentration of O in the reaction solution was 2/3 mol/L.
3. The method of claim 1, wherein the urea solution has a molarity of 5.5 to 5.6 mol/L.
4. The method according to claim 1, wherein the molar concentration of NaCl in the reaction solution is 2/3 mol/L.
5. The method of claim 1, wherein the molar ratio of thioacetamide to NaCl is from 0.20 to 0.30.
6. The process according to claim 1, wherein the reaction time is 4 to 5 hours.
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| CN110227502A (en) * | 2019-06-11 | 2019-09-13 | 杭州电子科技大学 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
| CN110882705B (en) * | 2019-12-10 | 2022-10-21 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi 2 S 3 Catalyst and preparation method and application thereof |
| CN115999586A (en) * | 2023-02-06 | 2023-04-25 | 浙江工业大学 | Double-vacancy BiOCl/ZnS heterojunction catalyst and preparation method and application thereof |
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| CN102513134A (en) * | 2011-11-03 | 2012-06-27 | 山东大学 | Compound photocatalysis material with bismuth sulfide nano particles/bismuth oxychloride and preparation method thereof |
| CN103316701A (en) * | 2013-07-02 | 2013-09-25 | 辽宁石油化工大学 | Method for preparing Bi2S3/BiOCl heterojunction photocatalyst |
| CN104549375A (en) * | 2014-10-24 | 2015-04-29 | 阜阳师范学院 | Synthesis of novel compound photocatalyst Bi2S3/BiOCl as well as application of photocatalyst |
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Patent Citations (3)
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| CN102513134A (en) * | 2011-11-03 | 2012-06-27 | 山东大学 | Compound photocatalysis material with bismuth sulfide nano particles/bismuth oxychloride and preparation method thereof |
| CN103316701A (en) * | 2013-07-02 | 2013-09-25 | 辽宁石油化工大学 | Method for preparing Bi2S3/BiOCl heterojunction photocatalyst |
| CN104549375A (en) * | 2014-10-24 | 2015-04-29 | 阜阳师范学院 | Synthesis of novel compound photocatalyst Bi2S3/BiOCl as well as application of photocatalyst |
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| Effect of the counter ions on composition and morphology of bismuth oxyhalides and their photocatalytic performance;Qiaofeng Han等;《Chemical Engineering Journal》;20160419;第299卷;第218页2.1节，第219页右栏第3段 * |
| One-Pot Strategy to Bi2S3/BiOCl Heterojunction with Enhanced Photocatalytic Activity;Ji-Yao Tao等;《Journal of Nanoscience and Nanotechnology》;20180601;第18卷;全文 * |
| Photocatalytic activities of Bi2S3/BiOBr nanocomposites synthesized by a facile hydrothermal process;Yumin Cui等;《Applied Surface Science》;20131121;第290卷;全文 * |
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