CN110560096A - bismuth-series heterojunction-loaded graphene oxide photocatalytic material and preparation method and application thereof - Google Patents
bismuth-series heterojunction-loaded graphene oxide photocatalytic material and preparation method and application thereof Download PDFInfo
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- CN110560096A CN110560096A CN201910924945.5A CN201910924945A CN110560096A CN 110560096 A CN110560096 A CN 110560096A CN 201910924945 A CN201910924945 A CN 201910924945A CN 110560096 A CN110560096 A CN 110560096A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011941 photocatalyst Substances 0.000 claims abstract description 18
- 239000002135 nanosheet Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- XQQSWXUDAPLMKD-UHFFFAOYSA-N N,N-dimethylheptadecan-1-amine hydrobromide Chemical compound Br.CCCCCCCCCCCCCCCCCN(C)C XQQSWXUDAPLMKD-UHFFFAOYSA-N 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004729 solvothermal method Methods 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 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
Classifications
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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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
The invention discloses a preparation method of a bismuth-series heterojunction-loaded graphene oxide photocatalytic material, which comprises the following steps of: firstly, preparing a BiOI/BixNbOy photocatalyst and graphene oxide, loading the synthesized BiOI/BixNbOy heterojunction catalyst on a graphene oxide nano-sheet, taking the loaded graphene nano-sheet as a precursor, and carrying out vacuum drying treatment on the pre-frozen compound to obtain the high-strength bismuth-series heterojunction-loaded graphene oxide photocatalytic material. The bismuth-series heterojunction-loaded graphene oxide photocatalytic material has the characteristics of high strength, high specific surface area, strong adsorption and the like, can effectively solve the problem that a powdery photocatalyst is difficult to separate and recycle after being used, and avoids the problems of secondary pollution and the like caused by a nano material to the environment; the photocatalytic reaction rate is improved; the separation rate of the photo-generated carriers of the catalyst is improved, the stability of the photocatalyst is improved, and the spectral response range is widened.
Description
Technical Field
The invention relates to a preparation method of a photocatalytic material, in particular to preparation and application of a bismuth-series heterojunction-loaded graphene oxide photocatalytic material.
Background
Persistent Organic Pollutants (POPs) are a general term for natural or synthetic organic substances and derivatives thereof with long-term residue, large-scale mobility, bioaccumulation, semi-volatility and high toxicity to living organisms, and the POPs pollution gradually becomes a new global environmental problem which is currently and internationally concerned. With the rapid development of domestic industrial and agricultural economy, the discharge of POPs in related water bodies through various ways is continuously increased, the pollution condition presents a worsening trend, and the caused health problems become more serious day by day, and research show that the surface water environment is generally polluted by persistent organic matters, and the water quality of water source water and underground water also faces severe tests.
Photocatalytic degradation is an important conversion pathway of POPs in the environment, and is also the most commonly used chemical degradation method. The existing conventional photocatalyst, niobium-series and bismuth-series composite oxides or heterojunction, graphene oxide-based composite catalyst and the like have certain defects. Therefore, the preparation of the novel photocatalyst which is nontoxic and stable, high in catalytic activity, high in green energy utilization rate and good in recycling performance has important significance for realizing efficient degradation of POPs in water. The invention aims to prepare a bismuth-loaded heterojunction-loaded graphene oxide photocatalytic material with high-efficiency catalytic performance.
Disclosure of Invention
The invention aims to overcome the defects of narrow spectral response range, poor recycling property, secondary pollution of generated water, low carrier separation efficiency and the like of the existing photocatalytic material, and provides a preparation method of an efficient bismuth-series heterojunction-loaded graphene oxide photocatalytic material.
The invention is realized by the following technical scheme.
A preparation method of a bismuth-series heterojunction-loaded graphene oxide photocatalytic material comprises the following steps:
First preparing BiOI/BixNbOyThe method comprises the steps of loading a synthesized BiOI/BixNbOy heterojunction catalyst on a graphene oxide nano-sheet, taking the loaded graphene nano-sheet as a precursor, and performing vacuum drying treatment on a pre-frozen compound by means of a directional vacuum freeze-drying technology to obtain the high-strength bismuth-series heterojunction-loaded graphene oxide photocatalytic material.
Preferably, Nb is used2O5And Bi (NO)3)3·5H2O preparation of BiOI/BixNbOyA photocatalyst.
Preferably, BiOI/BixNbOyDifferent surfactants are respectively added or different reaction conditions (such as reaction) are respectively controlled in the preparation process of the photocatalystTemperature, time, reactant ratio, etc.) to synthesize BiOI/Bi with different crystal formsxNbOyA heterojunction photocatalyst.
Preferably, the surfactant is sodium citrate, sodium dodecylbenzene sulfonate or cetyltrimethylammonium bromide.
Preferably, the vacuum degree is 3.3-13 pa in the vacuum freeze drying process.
The bismuth-series heterojunction-loaded graphene oxide photocatalytic material prepared by the method.
The bismuth-series heterojunction-loaded graphene oxide photocatalytic material is mainly applied to degradation of POPs (persistent organic pollutants) in a water body.
BiOI/Bi in the preparation method of the inventionxNbOythe load of the method is combined with the directional vacuum freeze drying technology, so that the mechanical strength of the graphene-based catalyst can be greatly improved.
The graphene oxide-based load in the preparation method can improve BiOI/BixNbOyDegree of catalyst dispersion and uniformity of dispersion.
Compared with the prior art, the technical scheme provided by the invention has the advantages that:
(1) The constructed bismuth-series heterojunction-loaded graphene oxide photocatalytic material has the characteristics of high strength, high specific surface area, strong adsorption and the like, can effectively solve the problem that the powdery photocatalyst is difficult to separate and recycle after being used, and avoids the problems of secondary pollution and the like caused by a nano material to the environment.
(2) Compared with the traditional photocatalyst carrier (such as activated carbon), the graphene oxide carrier is easier to transfer mass, and is beneficial to improving the photocatalytic reaction rate.
(3) Utilizing high-strength graphene oxide as BiOI/BixNbOyThe carrier combines the excellent photoelectric properties and structural characteristics of the two, improves the separation rate of the photo-generated carriers of the catalyst, increases the stability of the photocatalyst, and widens the spectral response range.
Drawings
FIG. 1 shows GO-BiOI/BixNbOySynthesis of photocatalyst and reduction of POPs by using sameAnd (4) a mechanism diagram is shown.
Detailed Description
Example 1
Firstly, preparing BiOI/Bi by adopting a solvothermal methodxNbOyAnd (3) adding a surfactant sodium citrate into the photocatalyst in the preparation process, and then preparing the graphene oxide by adopting an improved Hummers method. The synthesized BiOI/BixNbOyThe heterojunction catalyst is supported on the graphene oxide nanosheets. And thirdly, taking the loaded graphene nanosheet as a precursor, and performing vacuum drying under the vacuum degree of 3.3Pa by means of a directional vacuum freeze drying technology to obtain the high-strength bismuth-system-heterojunction-loaded graphene photocatalytic material.
Load BiOI/Bi is constructed by taking xenon lamp as simulated solar light sourcexNbOyHeterojunction graphene oxide continuous flow reactor. Model sewage containing POPs and actual sewage are respectively taken as treatment objects, after pollutants and photocatalysis reach adsorption balance, samples are taken at regular intervals to determine the concentration of the POPs and the contents of COD and TOC, and the degradation rate and the mineralization degree of the POPs are analyzed.
The invention discloses preparation and application of a bismuth-series heterojunction-loaded graphene oxide photocatalytic material. By loading BiOI/Bi on graphene oxidexNbOyAnd (3) carrying out vacuum freeze drying on the heterojunction to obtain the high-strength bismuth-series heterojunction-loaded graphene oxide photocatalytic material.
Example 2
Firstly, preparing BiOI/Bi by adopting a solvothermal methodxNbOyThe photocatalyst (surfactant sodium dodecyl benzene sulfonate is added in the preparation process), and then the improved Hummers method is adopted to prepare the graphene oxide. The synthesized BiOI/BixNbOythe heterojunction catalyst is supported on the graphene oxide nanosheets. And thirdly, taking the loaded graphene nanosheet as a precursor, and performing vacuum drying under the vacuum degree of 5.0Pa by means of a directional vacuum freeze drying technology to obtain the high-strength bismuth-system-heterojunction-loaded graphene photocatalytic material.
Example 3
Firstly, preparing BiOI/Bi by adopting a solvothermal methodxNbOyAnd (3) adding a surfactant cetyl trimethyl ammonium bromide in the photocatalyst (preparation process), and then preparing graphene oxide by adopting an improved Hummers method. The synthesized BiOI/BixNbOyThe heterojunction catalyst is supported on the graphene oxide nanosheets. And thirdly, taking the loaded graphene nanosheet as a precursor, and performing vacuum drying under the vacuum degree of 6.0Pa by means of a directional vacuum freeze drying technology to obtain the high-strength bismuth-system-heterojunction-loaded graphene photocatalytic material.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a bismuth-series heterojunction-loaded graphene oxide photocatalytic material is characterized by comprising the following steps:
First preparing BiOI/BixNbOyPhotocatalyst and graphene oxide, synthesized BiOI/BixNbOyAnd (2) loading the heterojunction catalyst on the graphene oxide nanosheets, taking the loaded graphene nanosheets as precursors, and performing vacuum drying treatment on the pre-frozen compounds by adopting a directional vacuum freeze-drying technology to obtain the bismuth-series heterojunction-loaded graphene oxide photocatalytic material with high strength.
2. The preparation method of the bismuth-based heterojunction-supported graphene oxide photocatalytic material according to claim 1, wherein Nb is adopted2O5And Bi5(NO3)3·5H2O preparation of BiOI/BixNbOyPhotocatalyst and process for producing the same。
3. The method for preparing the bismuth-based heterojunction-supporting graphene oxide photocatalytic material of claim 1, wherein the BiOI/BixNbOyAdding a surfactant in the preparation process of the photocatalyst to synthesize the BiOI/BixNbOyA heterojunction photocatalyst.
4. The preparation method of the graphene oxide photocatalytic material loaded with the bismuth-based heterojunction as claimed in claim 1, wherein the surfactant is sodium citrate, sodium dodecyl benzene sulfonate or hexadecyl trimethylamine bromide.
5. The preparation method of the bismuth-based heterojunction-supported graphene oxide photocatalytic material as claimed in claim 1, wherein the vacuum degree is 3.3-13 pa in the vacuum freeze drying process.
6. A bismuth-based heterojunction-supported graphene oxide photocatalytic material prepared by the method of any one of claims 1 to 5.
7. The graphene oxide photocatalytic material loaded with bismuth-based heterojunction as claimed in claim 6 is applied to degradation of POPs in water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113522321A (en) * | 2021-07-07 | 2021-10-22 | 浙江大学 | Surface/bulk junction visible-light-driven photocatalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941105A (en) * | 2012-11-23 | 2013-02-27 | 哈尔滨师范大学 | Preparation method for bismuth oxyiodide/graphene oxide compound visible light catalytic material |
| CN104069844A (en) * | 2014-07-23 | 2014-10-01 | 武汉理工大学 | Grading three-dimensional porous graphene/titanium dioxide photocatalyst and preparation method thereof |
| CN106732681A (en) * | 2016-12-07 | 2017-05-31 | 湖北工业大学 | The preparation method of three-dimensional foam shape reduced graphene bismuth oxyiodide composite photo-catalyst |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941105A (en) * | 2012-11-23 | 2013-02-27 | 哈尔滨师范大学 | Preparation method for bismuth oxyiodide/graphene oxide compound visible light catalytic material |
| CN104069844A (en) * | 2014-07-23 | 2014-10-01 | 武汉理工大学 | Grading three-dimensional porous graphene/titanium dioxide photocatalyst and preparation method thereof |
| CN106732681A (en) * | 2016-12-07 | 2017-05-31 | 湖北工业大学 | The preparation method of three-dimensional foam shape reduced graphene bismuth oxyiodide composite photo-catalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522321A (en) * | 2021-07-07 | 2021-10-22 | 浙江大学 | Surface/bulk junction visible-light-driven photocatalyst and preparation method thereof |
| CN113522321B (en) * | 2021-07-07 | 2022-07-01 | 浙江大学 | Surface/bulk junction visible-light-driven photocatalyst and preparation method thereof |
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