CN107185564B - Spherical core-shell structure BiOCl/SnO2Visible light catalyst and preparation method and application thereof - Google Patents
Spherical core-shell structure BiOCl/SnO2Visible light catalyst and preparation method and application thereof Download PDFInfo
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- CN107185564B CN107185564B CN201710418584.8A CN201710418584A CN107185564B CN 107185564 B CN107185564 B CN 107185564B CN 201710418584 A CN201710418584 A CN 201710418584A CN 107185564 B CN107185564 B CN 107185564B
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000011258 core-shell material Substances 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002351 wastewater Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000011941 photocatalyst Substances 0.000 claims abstract description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 7
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 230000001699 photocatalysis Effects 0.000 claims description 19
- 230000009467 reduction Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RZUBARUFLYGOGC-MTHOTQAESA-L acid fuchsin Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=C(N)C(C)=CC(C(=C\2C=C(C(=[NH2+])C=C/2)S([O-])(=O)=O)\C=2C=C(C(N)=CC=2)S([O-])(=O)=O)=C1 RZUBARUFLYGOGC-MTHOTQAESA-L 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 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 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- JDIBGQFKXXXXPN-UHFFFAOYSA-N bismuth(3+) Chemical compound [Bi+3] JDIBGQFKXXXXPN-UHFFFAOYSA-N 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000243 mutagenic effect Toxicity 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 231100000175 potential carcinogenicity Toxicity 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- 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
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
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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
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- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/397—Egg shell like
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- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/10—Photocatalysts
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Abstract
The invention discloses a BiOCl/SnO with a spherical core-shell structure2A visible light catalyst and a preparation method and application thereof belong to the technical field of synthesis of visible light catalytic materials. The technical scheme provided by the invention has the key points that: adding Bi (NO)3)3·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; SnCl4·5H2Adding O into the solution A, and uniformly stirring to obtain a solution B; transferring the solution B into a polytetrafluoroethylene reaction kettle to react for 12 hours at 180 ℃, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant-temperature drying oven at 60 ℃ to obtain the spherical core-shell structure BiOCl/SnO2A visible light photocatalyst. The spherical core-shell structure BiOCl/SnO prepared by the invention2The visible light catalyst has better light absorption performance, larger specific surface area and pore volume, and has the performance of efficiently carrying out light catalytic oxidation on dye wastewater and carrying out light catalytic reduction on Cr (VI) wastewater under simulated sunlight.
Description
Technical Field
The invention belongs to the technical field of synthesis of visible light catalytic materials, and particularly relates to a spherical core-shell structure BiOCl/SnO2Visible light catalyst and its preparation method and application.
Background
Some dye wastewater discharged into natural water has the effects of toxicity, carcinogenesis and mutation, and poses serious threats to human health and ecological systems. In addition, Cr (VI) is also of great concern for pollutants in wastewater, chromium has a wide range of applications in different industrial activities, such as electroplating, textile dyeing, leather tanning, metallurgy and the like, resulting in the toxicity of chromium-containing wastewater, and Cr (VI) has potential carcinogenicity and mutagenicity and is listed as one of 20 substances causing the most serious threat to human health. Therefore, efficient removal of them from wastewater is crucial. Among various wastewater treatment technologies, the semiconductor photocatalysis technology can effectively degrade pollutants, and is a promising green technology for purifying the environment. At present, bismuth (III) -based oxide photocatalyst has become a photocatalytic material of great interest, wherein BiOCl is an excellent photocatalyst, and has a ratio of P25-TiO under ultraviolet irradiation2Has higher photocatalytic activity, but can not respond under visible light, so that the BiOCl is compounded with other photocatalysts to improve the performance of the BiOCl, which is an effective method. A number of BiOCl-based heterojunction photocatalysts have been published, including BiOCl/BiVO4、WO3BiOCl and BiOCl/BiOBr, etc. In contrast, few heterojunction catalysts that are composited from two wide bandgap semiconductors have been reported. BiOCl/SnO2The recombination of (a) results in the generation of defects, whereby the band gap can be narrowed, and therefore, the wide band gap semiconductor can exhibit good photocatalytic activity even under visible light irradiation. As a continuous renewable energy source, sunlight is an ideal light source for photocatalysis, occupies a large amount of visible light, and develops high-efficiency light with visible light response from the aspect of energy conservationA catalyst is necessary.
Disclosure of Invention
The invention solves the technical problem of providing a spherical core-shell structure BiOCl/SnO for photocatalytic oxidation of dye wastewater and photocatalytic reduction of Cr (VI) wastewater under visible light2A preparation method of a visible light photocatalyst.
The invention adopts the following technical scheme to solve the technical problems, namely the spherical core-shell structure BiOCl/SnO2The preparation method of the visible light catalyst is characterized by comprising the following specific steps: adding Bi (NO)3)3·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; SnCl4·5H2Adding O into the solution A, and uniformly stirring to obtain a solution B; transferring the solution B into a polytetrafluoroethylene reaction kettle to react for 12 hours at 180 ℃, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant-temperature drying oven at 60 ℃ to obtain the spherical core-shell structure BiOCl/SnO2A visible light photocatalyst.
Further preferably, said Bi (NO)3)3·5H2O and SnCl4·5H2The feeding molar ratio of O is 2: 1.
The spherical core-shell structure BiOCl/SnO2The visible light catalyst is characterized by being prepared by the method.
The spherical core-shell structure BiOCl/SnO2The visible light catalyst is used for photocatalytic oxidation of dye wastewater and photocatalytic reduction of Cr (VI) wastewater under visible light.
The spherical core-shell structure BiOCl/SnO prepared by the invention2The visible light catalyst has better light absorption performance, larger specific surface area and pore volume, and has the performance of efficiently carrying out light catalytic oxidation on dye wastewater and carrying out light catalytic reduction on Cr (VI) wastewater under simulated sunlight.
Drawings
FIG. 1 is an X-ray diffraction pattern of visible-light-induced photocatalyst prepared in examples 1 to 3 of the present invention;
FIG. 2 is a transmission electron micrograph of a visible light photocatalyst prepared in example 3 of the present invention;
FIG. 3 is a graph showing the degradation curve of methylene blue wastewater through photocatalytic oxidation by a visible light catalyst prepared in examples 1 to 3 of the present invention;
FIG. 4 is a graph showing the degradation curve of wastewater from the photocatalytic reduction of Cr (VI) by using visible light catalysts prepared in examples 1 to 3 of the present invention;
FIG. 5 is a degradation curve of 6 dye wastewater of the visible light catalyst prepared in example 3 of the present invention for photocatalytic oxidation of rhodamine B, methylene blue, crystal violet, orange yellow IV, acid fuchsin and methyl orange and wastewater of reduction of Cr (VI).
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
(1) Adding 1mM Bi (NO)3)3·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; (2) adding 1mM KCl into the solution A, and uniformly stirring to obtain a solution B; (3) and transferring the solution B into a 100mL polytetrafluoroethylene reaction kettle, reacting for 12h at 180 ℃, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant-temperature drying oven at 60 ℃ to obtain the BiOCl photocatalyst. The reaction is carried out for 60min under the illumination of 350W Xe lamp light, the methylene blue light catalytic oxidation rate of 10mg/L is 80%, and the photocatalytic reduction rate of Cr (VI) wastewater of 10mg/L is 2%.
Example 2
(1) 1mM of SnCl4·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; (2) transferring the solution A into a 100mL polytetrafluoroethylene reaction kettle, reacting at 180 ℃ for 12h, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant-temperature drying oven at 60 ℃ to obtain SnO2A photocatalyst. The reaction is carried out for 60min under the illumination of 350W Xe lamp light, and the photocatalytic oxidation rate of 10mg/L methylene blue wastewater is46 percent, and the photocatalytic reduction rate of 10mg/L Cr (VI) wastewater is 3 percent.
Example 3
(1) Adding 1mM Bi (NO)3)3·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; (2) 0.5mM of SnCl4·5H2Adding O into the solution A, and uniformly stirring to obtain a solution B; (3) transferring the solution B into a 100mL polytetrafluoroethylene reaction kettle to react for 12h at 180 ℃, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant temperature drying oven at 60 ℃ to obtain the spherical core-shell structure BiOCl/SnO2A visible light photocatalyst. The reaction is carried out for 60min under the illumination of 350W Xe lamp light, the photocatalytic oxidation rate of 6 dye wastewater of 10mg/L rhodamine B, methylene blue, crystal violet, orange yellow IV, acid fuchsin and methyl orange can reach 99 percent, and the photocatalytic reduction rate of 10mg/L Cr (VI) wastewater can reach 99.5 percent.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (4)
1. Spherical core-shell structure BiOCl/SnO2The preparation method of the visible light catalyst is characterized by comprising the following specific steps: adding Bi (NO)3)3·5H2Dissolving O in a mixed solution of ethanol and glycerol to obtain a solution A; SnCl4·5H2Adding O into the solution A, and uniformly stirring to obtain a solution B; transferring the solution B into a polytetrafluoroethylene reaction kettle to react for 12 hours at 180 ℃, naturally cooling to room temperature after the reaction is finished, filtering and separating, washing with water and ethanol for three times respectively, and drying in a constant-temperature drying oven at 60 ℃ to obtain the spherical core-shell structure BiOCl/SnO2A visible light photocatalyst.
2. According to the claimsSolution 1 of the spherical core-shell structure BiOCl/SnO2The preparation method of the visible light catalyst is characterized by comprising the following steps: said Bi (NO)3)3·5H2O and SnCl4·5H2The feeding molar ratio of O is 2: 1.
3. Spherical core-shell structure BiOCl/SnO2Visible light photocatalyst, characterized by being prepared by the method of claim 1 or 2.
4. Spherical core-shell structure BiOCl/SnO according to claim 32The visible light catalyst is used for photocatalytic oxidation of dye wastewater and photocatalytic reduction of Cr (VI) wastewater under visible light.
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| CN111558385A (en) * | 2020-05-13 | 2020-08-21 | 重庆工商大学 | P-n type heterojunction BiOBr/SnO2Composite photocatalyst and preparation method thereof |
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| CN102847546A (en) * | 2012-05-23 | 2013-01-02 | 上海师范大学 | Preparation method of SnO2/BiOCl heterojunction photocatalyst |
| CN105728004A (en) * | 2016-02-03 | 2016-07-06 | 三峡大学 | High-performance BiOCl/SnO2 heterojunction material and preparing method thereof |
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| CN102847546A (en) * | 2012-05-23 | 2013-01-02 | 上海师范大学 | Preparation method of SnO2/BiOCl heterojunction photocatalyst |
| CN105728004A (en) * | 2016-02-03 | 2016-07-06 | 三峡大学 | High-performance BiOCl/SnO2 heterojunction material and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Microwave-assisted synthesis of flower-like BN/BiOCl composites for photocatalytic Cr(VI) reduction upon visible-light irradiation;Hang Xu等;《Materials and Design》;20161106;第114卷;第129-138页 * |
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