CN112973743A - BC/Bi4O5Br2Preparation method of composite photocatalytic material - Google Patents

BC/Bi4O5Br2Preparation method of composite photocatalytic material Download PDF

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Publication number
CN112973743A
CN112973743A CN202110248026.8A CN202110248026A CN112973743A CN 112973743 A CN112973743 A CN 112973743A CN 202110248026 A CN202110248026 A CN 202110248026A CN 112973743 A CN112973743 A CN 112973743A
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China
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composite photocatalytic
photocatalytic material
composite
magnetic stirring
potassium bromide
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Inventor
孙晓杰
王春莲
王亚搏
张木喜
谭知涵
胡江良
张红霞
李洁
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Guilin University of Technology
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Guilin University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06Halogens; Compounds thereof
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/03Precipitation; Co-precipitation
    • B01J37/031Precipitation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

Abstract

The invention provides BC/Bi4O5Br2The preparation method of the composite photocatalytic material comprises the steps of preparing BC/Bi by using bismuth nitrate pentahydrate, BC and potassium bromide as raw materials and ethylene glycol as a reaction solvent through a simple and easily-operated room-temperature precipitation method4O5Br2Composite photocatalytic materialAnd (5) feeding. Using xenon lamp as light source, passing light of low wavelength (lambda) through filter<420nm) filtering off, and p-BC/Bi4O5Br2And carrying out a photocatalytic performance test on the composite photocatalytic material. Degradation of rhodamine B and tetracycline hydrochloride is carried out, and degradation rates of rhodamine B and tetracycline hydrochloride are used for representing BC/Bi4O5Br2The photocatalytic performance of the composite photocatalytic material. The material has the advantages of high chemical stability, large specific surface area, unique electronic structure, strong light absorption capacity and the like, so that the material has wide application prospect in the aspect of water pollution treatment.

Description

BC/Bi4O5Br2Preparation method of composite photocatalytic material
Technical Field
The invention belongs to the field of preparation of photocatalytic materials, and particularly relates to BC/Bi4O5Br2A preparation method of a composite photocatalytic material.
Background
In sewage treatment, photocatalytic oxidation is a novel advanced oxidation technology, is developed on the basis of photochemical oxidation, has strong oxidation capability and no secondary pollution, can be carried out at normal temperature and normal pressure, and has the characteristics of environmental protection, energy conservation and the like.
Bismuth-based semiconductors are a unique new class of photocatalytic materials that have been developed in recent years. Due to the special structure of Bi atoms, the compound can easily form a layered structure, and a bismuth-based compound with visible light response capability is generated. Wherein Bi is in the bismuth-rich halide material4O5Br2The organic light-emitting diode has attracted attention due to high chemical stability, large specific surface area, unique electronic structure and high light absorption capacity, and researches show that the organic light-emitting diode has excellent performance in the degradation aspect of organic matters.
Biochar (BC) is a carbon material that has been extensively studied in recent years and is produced by carbonizing wood, straw, grass, fallen leaves or other agricultural waste by pyrolysis under low oxygen and relatively low temperature conditions. It not only has a large number of pore channel structures and larger specific surface area, but also has good adsorption property when being compounded with the catalystThe conductivity, combined with the catalyst, can be used as an electron acceptor to conduct electrons in time so as to improve the separation efficiency of electron-hole pairs. Therefore, it is considered that Bi4O5Br2The high-efficiency photocatalyst can be prepared by compounding with a ZSM-5 zeolite molecular sieve.
Disclosure of Invention
The invention aims to provide BC/Bi4O5Br2A preparation method of a composite photocatalytic material is used for solving the environmental problem.
The method comprises the following specific steps:
(1) dissolving bismuth nitrate pentahydrate in ethylene glycol, adding BC under stirring, performing ultrasonic treatment, performing magnetic stirring, and adding potassium bromide to perform magnetic stirring until the potassium bromide is dissolved;
(2) sequentially and slowly adding ultrapure water and ammonia monohydrate into the solution obtained in the step (1), and magnetically stirring;
(3) filtering the reaction solution obtained in the step (2), collecting precipitate, and washing the precipitate;
(4) drying the precipitate obtained in the step (3), and grinding to obtain BC/Bi4O5Br2A composite photocatalytic material.
Preferably, the magnetic stirring time in the step (1) is 30min, and the ultrasonic time is 30 min.
Preferably, the magnetic stirring time of the step (2) is 6 h.
Preferably, the oven drying time is 12 h.
Preferably, the ratio of activated carbon BC: bi4O5Br2The mass fraction ratio is 0.75: 100. 1.5: 100. 5: 100, calculating.
Preparation of BC/Bi as described above4O5Br2The composite photocatalytic material can be used in the field of sewage treatment. The material is a composite of active carbon and a bismuth oxyhalide semiconductor, the existence of the active carbon improves the adsorption performance of the catalyst, and the active carbon is used as an electron acceptor to conduct electrons in time and improve the separation efficiency of electron-hole pairs. The composite photocatalytic material has strong oxidizing ability, no secondary pollution, can be carried out at normal temperature and normal pressure, has the characteristics of economy, environmental protection, energy conservation and the like, and is used for solving the problems of low cost and high costProvides a way to solve the environmental problem.
The method has the advantages that:
(1) the BC/Bi is prepared by a simple ultrasonic-assisted room temperature in-situ precipitation method4O5Br2The composite photocatalytic material is simple and easy to operate;
(2) prepared BC/Bi4O5Br2The composite photocatalytic material has the performance of effectively degrading rhodamine B (RhB) and tetracycline hydrochloride (TC) under visible light;
(3) prepared BC/Bi4O5Br2The composite photocatalytic material has better circulation stability, and the problem that the photocatalytic efficiency of the material is greatly reduced after primary photocatalysis is avoided;
(4) the application is simple, and only the prepared BC/Bi is needed4O5Br2The composite photocatalytic material powder is put into RhB or TC with a certain concentration, and degradation of RhB or TC can be carried out under visible light.
Drawings
FIG. 1: BC/Bi4O5Br2C/C of composite photocatalytic material for degrading RhB0Graph (a) and kinetic fit graph (b);
FIG. 2: BC/Bi4O5Br2C/C of composite photocatalytic material for degrading TC0Graph (a) and removal rate graph (b);
FIG. 3: BC/Bi4O5Br2SEM picture of the composite photocatalytic material;
FIG. 4: BC/Bi4O5Br2XRD spectrogram of the composite photocatalytic material;
FIG. 5: BC/Bi4O5Br2Nitrogen adsorption-desorption isotherms of the composite photocatalytic material;
FIG. 6: BC/Bi4O5Br2XPS full spectrum of the composite photocatalytic material;
FIG. 7: BC/Bi4O5Br2An ultraviolet-visible diffuse reflection spectrogram (a) and a forbidden band width chart (b) of the composite photocatalytic material;
FIG. 8:BC/Bi4O5Br2a Raman spectrogram of the composite photocatalytic material;
FIG. 9: BC/Bi4O5Br2PL profile of the composite photocatalytic material;
FIG. 10: BC/Bi4O5Br2A photocurrent response graph of the composite photocatalytic material;
FIG. 11: BC/Bi4O5Br2EIS diagram of composite photocatalytic material.
Detailed Description
The present invention is further described in detail with reference to the following specific examples 1-5, which are intended to be illustrative, but not limiting, of the invention.
Example 1:
BC/Bi was prepared as follows4O5Br2The composite photocatalytic material is as follows:
(1) dissolving 2.425g of bismuth nitrate pentahydrate in 20mL of ethylene glycol, adding 0.0182g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate pentahydrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 0.75 BC/BOB.
Example 2:
(1) dissolving 2.425g of pentahydrate bismuth nitrate in 20mL of ethylene glycol, adding 0.0364g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, and then adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 1.5 BC/BOB.
Example 3:
(1) dissolving 2.425g of pentahydrate bismuth nitrate in 20mL of ethylene glycol, adding 0.1213g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, and then adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 5 BC/BOB.
Under the irradiation of a xenon lamp, light below 420nm is filtered by using a filter plate, and the photocatalytic performance of the material is characterized by using the degradation efficiency of RhB and BPA.
Doping of BC increases Bi4O5Br2The specific surface area of the photocatalytic material enhances the adsorption performance of the catalyst, and the BC is used as an electron acceptor to conduct electrons in time, so that the separation efficiency of electron-hole pairs is improved. Cause BC/Bi4O5Br2The composite photocatalytic material shows better photocatalytic activity in a visible light area, so that organic pollutants can be efficiently degraded.

Claims (7)

1. BC/Bi4O5Br2The preparation method of the composite photocatalytic material is characterized by comprising the following specific steps:
(1) dissolving bismuth nitrate pentahydrate in ethylene glycol, adding BC under stirring, performing ultrasonic treatment, performing magnetic stirring, and adding potassium bromide to perform magnetic stirring until the potassium bromide is dissolved;
(2) sequentially and slowly adding ultrapure water and ammonia monohydrate into the solution obtained in the step (1), and magnetically stirring;
(3) filtering the reaction solution obtained in the step (2), collecting precipitate, and washing the precipitate;
(4) drying the precipitate obtained in the step (3), and grinding to obtain BC/Bi4O5Br2A composite photocatalytic material.
2. The method of claim 1, wherein: the magnetic stirring time in the step (1) is 30min, and the ultrasonic time is 30 min.
3. The method of claim 1, wherein: the magnetic stirring time in the step (2) is 6 h.
4. The method of claim 1, wherein: the drying time of the oven is 12 h.
5. The method of claim 1, wherein: the added raw materials comprise activated carbon BC: bi4O5Br2The mass fraction ratio is 0.75: 100. 1.5: 100. 5: 100, calculating.
6. BC/Bi obtained by the method of claim 14O5Br2A composite photocatalytic material.
7. BC/Bi obtained by the method of claim 14O5Br2The composite photocatalytic material is applied to the field of sewage treatment.
CN202110248026.8A 2021-03-07 2021-03-07 BC/Bi4O5Br2Preparation method of composite photocatalytic material Pending CN112973743A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115634702A (en) * 2021-07-20 2023-01-24 南昌航空大学 Bismuth oxycarbonate/biochar composite photocatalyst and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104226339A (en) * 2014-09-18 2014-12-24 玉林师范学院 Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof
CN108607590A (en) * 2018-03-30 2018-10-02 中国地质大学(武汉) g-C3N4Graft the preparation method and application of BiOX microsphere photocatalyst
CN112108166A (en) * 2020-09-29 2020-12-22 中国科学院生态环境研究中心 Ultrathin Bi4O5Br2/Bi2O2CO3Visible light catalyst and preparation method and application thereof
CN113171781A (en) * 2021-03-07 2021-07-27 桂林理工大学 BC composite Bi4O5Br2Method for treating recharge leachate by photocatalysis with photocatalytic material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104226339A (en) * 2014-09-18 2014-12-24 玉林师范学院 Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof
CN108607590A (en) * 2018-03-30 2018-10-02 中国地质大学(武汉) g-C3N4Graft the preparation method and application of BiOX microsphere photocatalyst
CN112108166A (en) * 2020-09-29 2020-12-22 中国科学院生态环境研究中心 Ultrathin Bi4O5Br2/Bi2O2CO3Visible light catalyst and preparation method and application thereof
CN113171781A (en) * 2021-03-07 2021-07-27 桂林理工大学 BC composite Bi4O5Br2Method for treating recharge leachate by photocatalysis with photocatalytic material

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* Cited by examiner, † Cited by third party
Title
李洁: ""改性Bi4O5Br2光催化剂的制备及其可见光下降解回灌渗滤液的研究"", 《中国优秀硕博士学位论文全文数据库(硕士)工程科技I辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115634702A (en) * 2021-07-20 2023-01-24 南昌航空大学 Bismuth oxycarbonate/biochar composite photocatalyst and preparation method and application thereof

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