CN114645286B - method for regulating and controlling surface phase oxygen vacancies of bismuth oxyhalide with high catalytic activity - Google Patents
method for regulating and controlling surface phase oxygen vacancies of bismuth oxyhalide with high catalytic activity Download PDFInfo
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- CN114645286B CN114645286B CN202210325895.0A CN202210325895A CN114645286B CN 114645286 B CN114645286 B CN 114645286B CN 202210325895 A CN202210325895 A CN 202210325895A CN 114645286 B CN114645286 B CN 114645286B
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 22
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 20
- 239000001301 oxygen Substances 0.000 title claims abstract description 20
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 16
- 230000001276 controlling effect Effects 0.000 title claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000003792 electrolyte Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 6
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; 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
- 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
- B01J35/30—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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
- C25B15/023—Measuring, analysing or testing during electrolytic production
- C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
- C25B15/027—Temperature
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- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
- C25B15/023—Measuring, analysing or testing during electrolytic production
- C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
- C25B15/029—Concentration
- C25B15/031—Concentration pH
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- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
A method for regulating and controlling the surface phase oxygen vacancy of bismuth oxyhalide with high catalytic activity. The invention adopts an electrochemical auxiliary method to treat the catalyst, and improves the concentration of surface oxygen vacancies of the bismuth oxyhalide photocatalyst, thereby greatly improving the photocatalytic performance for degrading organic pollutants. The method comprises the following steps: 1. placing bismuth oxyhalide into an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; 2. adjusting the pH value of the electrolyte by acid (or alkali) under the stirring state; 3. the electrodes are inserted into the electrolytic cell and maintained for a certain time in a constant voltage (or constant current) mode, and the temperature of liquid in the electrolytic cell is controlled in the electrifying process; 4. and (3) filtering the powder obtained in the step (III), cleaning to neutrality, and drying to obtain bismuth oxyhalide powder rich in high-concentration surface oxygen vacancies. The preparation method has the advantages of simplicity, low cost, high concentration of surface oxygen vacancies of the sample and the like.
Description
Technical Field
The invention relates to a method for regulating and controlling bismuth oxyhalide surface phase oxygen vacancies by an electrochemical method.
Background
With the rapid development of science and technology and industry, the emergence of many emerging industries has led to the discharge of large amounts of industrial waste into groundwater, which severely jeopardizes human health and the ecological environment of water resources that rely on survival. The semiconductor photocatalysis technology using solar energy as a main energy source is considered as one of the most ideal technical means for treating the current water pollution problem due to the characteristics of energy conservation, high efficiency, no secondary pollution and the like. However, titanium dioxide (TiO2) Typical conventional photocatalysts have limited applications in the field of environmental remediation due to limited spectral response ranges and low photon-generated carrier separation efficiency. Bismuth oxyhalide is considered to be one of the most promising new semiconductor photocatalysts due to its unique open layered structure and suitable energy band structure. However, the large forbidden bandwidth makes the catalytic degradation efficiency of BiOCl under visible light not ideal, and the photocatalytic performance of BiOCl needs to be improved. The introduction of oxygen vacancies into the BiOCl material is an effective method of improving its photocatalytic activity.
Disclosure of Invention
the invention provides a method for improving photocatalytic activity by regulating oxygen vacancies through an electrochemical method in order to find a regulating and controlling process of bismuth oxyhalide surface phase oxygen vacancies so as to meet the requirement of improving photocatalytic performance.
1. The method for regulating and controlling the surface phase oxygen vacancies of the bismuth oxyhalide with high catalytic activity is carried out according to the following steps:
1. Placing bismuth oxyhalide on one side of a negative electrode in an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of bismuth oxyhalide to water is 1:1-10000, wherein the aperture of the diaphragm of the electrolytic cell is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like;
2. Regulating the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 1-11;
3. Inserting electrodes into the electrolytic cell, wherein the voltage range is 0.1-10000V in a constant voltage mode, the current range is 0.0001-10000 mA in a constant current mode, the electrifying time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process;
4. filtering the powder obtained in the third step after the power is electrified, washing the powder with distilled water for 1 to 8 times to be neutral at 30 to 150 DEG C
The bismuth oxyhalide powder regulated and controlled by the invention has the advantages of simple preparation method, low cost, high catalytic activity and the like.
Drawings
FIG. 1 is a photograph of BiOCl scanning electron microscope prepared in experiment one;
FIG. 2 is a diagram of BiOCl phase analysis prepared by experiment one;
FIG. 3 EPR spectra of BiOCl samples prepared;
FIG. 4 is a graph of photocatalytic degradation of rhodamine B and CIP for a preparation BiOCl sample from experiment one;
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also includes any combination of the specific embodiments.
the first embodiment is as follows: the method for regulating and controlling the surface-phase oxygen vacancies of the bismuth oxyhalide with high catalytic activity in the embodiment is carried out according to the following steps:
1. Placing bismuth oxyhalide on one side of a negative electrode in an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of bismuth oxyhalide to water is 1:1-10000, wherein the aperture of the diaphragm of the electrolytic cell is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like;
2. Regulating the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 1-11;
3. Inserting electrodes into the electrolytic cell, wherein the voltage range is 0.1-10000V in a constant voltage mode, the current range is 0.0001-10000 mA in a constant current mode, the electrifying time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process;
4. and (3) filtering the powder obtained in the step (III) after the power is electrified, washing the powder for 1 to 8 times by using distilled water to be neutral, and drying the powder at the temperature of between 30 and 150 ℃ to obtain the bismuth oxyhalide powder rich in high-concentration surface oxygen vacancies.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is that the mass ratio of bismuth oxyhalide to water in the first step is 1:10-8000, wherein the aperture of the diaphragm of the electrolytic cell is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber, etc.
And a third specific embodiment: the difference between the present embodiment and the first to second embodiments is that in the second step, the pH value of the electrolyte is adjusted by an acid (or an alkali) and the pH value is in the range of 1 to 10.
the specific embodiment IV is as follows: the difference between the present embodiment and the first to third embodiments is that the voltage range in the constant voltage mode in the third step is 0.1 to 8000V.
Fifth embodiment: in the third step, the current range in the constant current mode is 0.001-9000 mA, which is different from the first to fourth embodiments.
Specific embodiment six: in the third step, the energizing time is 10-80000000 s, and the temperature of the liquid in the electrolytic cell is controlled to be 0-100 ℃ in the energizing process.
seventh embodiment: the difference between the embodiment and the specific embodiment is that the temperature of the liquid in the electrolytic cell is controlled between 0 and 90 ℃ in the electrifying process in the step three.
the following experiments are adopted to verify the effect of the invention:
experiment one:
A method for regulating and controlling high catalytic activity BiOCl surface phase oxygen vacancies is carried out according to the following steps:
1. placing BiOCl on the negative electrode side of an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of BiOCl to water is 1:100, wherein the aperture of the diaphragm of the electrolytic cell is 200nm, and the diaphragm can be made of PE;
2. Adjusting the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 7;
3. inserting electrodes into the electrolytic cell, wherein the voltage range is 300V under the constant voltage mode, the electrifying time is 19800s, and the temperature of liquid in the electrolytic cell is controlled to be 25 ℃ in the electrifying process;
4. And (3) filtering the powder obtained in the step (III) after the power is electrified, washing the powder with distilled water for 3 times to neutrality, and drying the powder at 50 ℃ to obtain the BiOCl powder rich in high-concentration surface oxygen vacancies.
Experiment II:
A method for regulating and controlling high catalytic activity BiOBr surface phase oxygen vacancies is carried out according to the following steps:
1. Placing BiOBr on the negative side of an electrolytic cell containing water, the electrolytic cell being separated by a diaphragm; the mass ratio of BiOBr to water is 1:500, wherein the aperture of the diaphragm of the electrolytic cell is 500nm, and the diaphragm can be made of PVDF;
2. Adjusting the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 6;
3. inserting an electrode into an electrolytic cell, wherein the voltage range in a constant current mode is 0.02A, the electrifying time is 28800s, and the temperature of liquid in the electrolytic cell is controlled to be 20 ℃ in the electrifying process;
4. And (3) filtering the powder obtained in the step (III) after the power is electrified, washing the powder for 5 times to neutrality by using distilled water, and drying the powder at 50 ℃ to obtain the BiOBr powder rich in high-concentration surface oxygen vacancies.
Claims (1)
1. A method for regulating and controlling the surface phase oxygen vacancies of bismuth oxyhalide with high catalytic activity is characterized in that the method for regulating and controlling the surface phase oxygen vacancies by electrochemical assistance is carried out according to the following steps:
1. Placing bismuth oxyhalide on one side of a negative electrode in an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of bismuth oxyhalide to water is 1:1-10000, wherein the aperture of the diaphragm of the electrolytic cell is 3-1000000 nm, and the diaphragm is made of PE, PVDF and glass fiber;
2. Regulating the pH value of the electrolyte by acid or alkali under the stirring state, wherein the pH value range is 1-11;
3. Inserting electrodes into the electrolytic cell, wherein the voltage range is 0.1-10000V in a constant voltage mode, the current range is 0.0001-10000 mA in a constant current mode, the electrifying time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process;
4. And (3) filtering the powder obtained in the step (III) after the power is electrified, washing the powder for 1 to 8 times by using distilled water to be neutral, and drying the powder at the temperature of between 30 and 150 ℃ to obtain the bismuth oxyhalide powder rich in high-concentration surface oxygen vacancies.
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Citations (3)
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CN112958116A (en) * | 2021-02-22 | 2021-06-15 | 西南大学 | Bi2O2.33-CdS composite photocatalyst and preparation process thereof |
CN113136602A (en) * | 2021-04-19 | 2021-07-20 | 西北师范大学 | Preparation and application of bismuth vanadate/Vo-FeNiOOH composite photo-anode |
CN113690453A (en) * | 2020-05-18 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Mn (manganese)5O8Nano cage-shaped oxygen reduction electrocatalyst and preparation method thereof |
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US9856567B2 (en) * | 2014-06-16 | 2018-01-02 | Wisconsin Alumni Research Foundation | Synthesis of high-surface-area nanoporous BiVO4 electrodes |
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CN113690453A (en) * | 2020-05-18 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Mn (manganese)5O8Nano cage-shaped oxygen reduction electrocatalyst and preparation method thereof |
CN112958116A (en) * | 2021-02-22 | 2021-06-15 | 西南大学 | Bi2O2.33-CdS composite photocatalyst and preparation process thereof |
CN113136602A (en) * | 2021-04-19 | 2021-07-20 | 西北师范大学 | Preparation and application of bismuth vanadate/Vo-FeNiOOH composite photo-anode |
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