CN110624576A - 一种具有超强降解效果的BiOCl光催化剂的制备方法 - Google Patents
一种具有超强降解效果的BiOCl光催化剂的制备方法 Download PDFInfo
- Publication number
- CN110624576A CN110624576A CN201910971427.9A CN201910971427A CN110624576A CN 110624576 A CN110624576 A CN 110624576A CN 201910971427 A CN201910971427 A CN 201910971427A CN 110624576 A CN110624576 A CN 110624576A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- photocatalyst
- biocl
- degradation effect
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 230000015556 catabolic process Effects 0.000 title claims abstract description 34
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 31
- 230000000694 effects Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 38
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 36
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 24
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 12
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 12
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 12
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000005642 Oleic acid Substances 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 abstract description 10
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 abstract description 10
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 33
- 229940073609 bismuth oxychloride Drugs 0.000 description 22
- 238000012360 testing method Methods 0.000 description 17
- 238000002835 absorbance Methods 0.000 description 8
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 8
- 238000005286 illumination Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000011651 chromium Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 238000006552 photochemical reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical group C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
-
- 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
- B01J27/08—Halides
- B01J27/10—Chlorides
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J37/04—Mixing
-
- 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
- B01J37/06—Washing
-
- 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
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
- C02F2305/08—Nanoparticles or nanotubes
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biomedical Technology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
本发明公开了一种具有超强降解效果的BiOCl光催化剂的制备方法，通过将BiOCl制备成特殊的微纳米级的椭圆体结构，显著改善了光催化剂的可见光催化效率，对气相甲醛、刚果红溶液和六价铬溶液的降解率均可达到90％以上；而且由于该BiOCl光催化剂结构稳定，故有很好的重复使用性能，使得该光催化剂成本更低，能够更加广泛的应用于环境污染处理领域。
Description
技术领域
本发明涉及光催化剂技术领域，尤其涉及一种具有超强降解效果的BiOCl光催化剂的制备方法。
背景技术
基于半导体的光催化技术已经成为有效降解水污染的方法之一，较之其它方法(过滤、吸附和生物技术等)有如下优点：洁净无害，价格低廉，可以使用太阳光等。比如，TiO2、ZnO等半导体材料已经被应用于污水中污染物的光降解。但是，这些材料由于禁带宽度大(＞3.0eV)，只有利用太阳光中的紫外光，所以寻求高性可见光响应的催化剂是必然的趋势。
氯氧化铋(BiOCl)是禁带宽度为3.46eV的半导体，但是只能利用太阳光中的紫外光，限制了其实际应用。如何通过制备方法的改进来改善材料的形貌，从而提高材料的光催化性能是本领域研究的重点，故本发明提供了一种具有超强降解效果的BiOCl光催化剂的制备方法。
发明内容
基于背景技术存在的技术问题，本发明提出了一种具有超强降解效果的BiOCl光催化剂的制备方法。
本发明的技术方案如下：
一种具有超强降解效果的BiOCl光催化剂的制备方法，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.1-0.3mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在120-150℃条件下加热8-12h，自然冷却；
D、过滤后用乙醇反复洗涤固体3-5次，喷雾干燥，即可。
优选的，所述的步骤A中，所述的去离子水和乙醇的体积比为1：(6-10)。
优选的，所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的2-4倍。
优选的，所述的步骤B中，油酸与乙醇的体积比为(1-3)：10；甘油与乙醇的体积比为(0.2-0.5)：10。
本发明的有益之处在于：本发明制备的具有超强降解效果的BiOCl光催化剂，通过将BiOCl制备成特殊的300-800nm长、150-300nm宽、50-100nm厚度的微纳米级的椭圆体结构，显著改善了光催化剂的可见光催化效率；而且由于该BiOCl光催化剂结构稳定，故有很好的重复使用性能，使得该光催化剂成本更低，能够更加广泛的应用于环境污染处理领域。
附图说明
图1：实施例1方法制备得到的BiOCl光催化剂的SEM图。
具体实施方式
实施例1
一种具有超强降解效果的BiOCl光催化剂的制备方法，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.15mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在128℃条件下加热10h，自然冷却；
D、过滤后用乙醇反复洗涤固体4次，喷雾干燥，即可。
所述的步骤A中，所述的去离子水和乙醇的体积比为1：8.5。
所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的2.5倍。
所述的步骤B中，油酸与乙醇的体积比为1.5：10；甘油与乙醇的体积比为0.3：10。
实施例2
一种具有超强降解效果的BiOCl光催化剂的制备方法，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.3mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在150℃条件下加热8h，自然冷却；
D、过滤后用乙醇反复洗涤固体5次，喷雾干燥，即可。
所述的步骤A中，所述的去离子水和乙醇的体积比为1：6。
所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的4倍。
所述的步骤B中，油酸与乙醇的体积比为1：10；甘油与乙醇的体积比为0.5：10。
实施例3
一种具有超强降解效果的BiOCl光催化剂的制备方法，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.1mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在120℃条件下加热12h，自然冷却；
D、过滤后用乙醇反复洗涤固体3次，喷雾干燥，即可。
所述的步骤A中，所述的去离子水和乙醇的体积比为1：10。
所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的2倍。
所述的步骤B中，油酸与乙醇的体积比为3：10；甘油与乙醇的体积比为0.2：10。
以下对实施例1-3制备的的BiOCl光催化剂样品进行测试(测试结果见表1)，具体测试方法如下：
(1)气相甲醛降解测试：甲醛是常见的室内污染物，《GB/T 16127-1995居室空气中甲醛的卫生标准》规定的室内甲醛最高容许浓度为0.08mg/m3。本实施例中，采用湖南华思仪器有限公司生产的PFD-5060型光化学反应仪(250L)来模拟居室环境，并采用5支T5直管荧光灯管(14W)模拟居室内自然光以及照明光源，对实施例1-3得到的BiOCl样品光催化降解甲醛性能测试，步骤如下：
每次将1g制备样品涂在50cm×50cm的玻璃板上，待样品板自然干燥后，将其放入试验舱，调节升降台使得样品表面与灯的距离20cm，密闭试验舱，然后用微量注射器精确量取30μL浓度为0.016mg/μL的甲醛溶液，通过仪器自带的进样装置，同时由辅助升温和通气装置使得甲醛以气体形式进入并均匀的分散在试验舱中。随后打开灯管、风扇(20W)，进行光催化反应，光照12h后，用恒流大气采样器采样10L(流速1L/min，采气时间10min)。最后按照国家标准《GB/T 16129-1995居住区大气中甲醛卫生检验标准方法-分光光度法》测试甲醛浓度，甲醛的降解率计算公式为η＝(C0－C12)/C0×100％，式中：η为降解率，C0为测试结束时空白(无样品)试验舱的甲醛浓度值，C12为测试结束时放有样品试验舱的甲醛浓度值。
(2)刚果红溶液降解测试：刚果红是一种典型的联苯胺类直接偶氮染料，在特定条件下样品对刚果红溶液的降解率越大，说明其光催化性能越好。本具体实施方式中，所用刚果红溶液的浓度为20mg/L，所用光源为500W氙灯(模拟太阳光)，在上海比朗仪器有限公司生产的BL-GHX-V型光化学反应仪上测试产品的光催化性能。步骤如下：
每次取100ml刚果红溶液和0.1g产品混合，先在无光照条件下搅拌40min，使溶液混合均匀。然后开灯光照，进行光催化反应。光照5h时用离心管取样，经高速离心后，取上清液在分光光度计上500nm波长处测其吸光度值，则刚果红溶液的降解率计算公式为：降解率＝(A0－At)/A0×100％，式中A0为初始刚果红溶液的吸光度值，At为光照5h时刚果红溶液的吸光度值。
(3)六价铬溶液降解测试：六价铬可造成典型的重金属污染，毒性较强，本具体实施方式中，采用重铬酸钾(K2Cr2O7)溶液模拟含六价铬(Cr(Ⅵ))废水，对六价铬溶液降解即为将其还原为无毒或毒性较弱的三价铬等物质，所用重铬酸钾溶液的浓度为10mg/L，所用光源为500W氙灯(模拟太阳光)，在上海比朗仪器有限公司生产的BL-GHX-V型光化学反应仪上测试产品的光催化性能，并采用二苯碳酰二肼分光光度法(GB 7467-1987水质六价铬测定)测试六价铬(Cr(Ⅵ))的含量。步骤如下：
每次取100ml六价铬溶液和0.2g产品混合，先在无光照条件下搅拌40min，使溶液混合均匀。然后开灯光照，进行光催化反应。光照5h时用离心管取样，经高速离心后，取2mL上清液加入到50mL比色管里用蒸馏水定容，然后依次加入2mL硫酸溶液(体积比为1:1)和2mL含有二苯碳酰二肼的丙酮溶液，显色10min后，在分光光度计上540nm波长处测其吸光度值，则六价铬溶液的降解率计算公式为：降解率＝(B0－Bt)/B0×100％，式中B0为初始重铬酸钾溶液的吸光度值，Bt为光照5h时重铬酸钾溶液的吸光度值。
(4)BiOCl样品禁带宽度值Eg的计算：利用[F(R)hv]1/2对hv做图，利用直线部分外推至横坐标交点(做拐点的切线)，即为禁带宽度值，A(Absorbance)即为紫外可见漫反射中的吸光度。
表1：实施例1-3制备的的BiOCl样品对有机物的降解效果测试结果(以下降解率的测试结果均为5个测试样品的测试结果平均值)；
| 样品 | 实施例1 | 实施例2 | 实施例3 |
| 气相甲醛的降解率％ | 98.18 | 96.77 | 97.25 |
| 刚果红溶液的降解率％ | 93.76 | 92.88 | 92.62 |
| 六价铬溶液的降解率％ | 91.53 | 90.34 | 90.71 |
| BiOCl样品禁带宽度值Eg | 2.96 | 2.87 | 2.85 |
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种具有超强降解效果的BiOCl光催化剂的制备方法，其特征在于，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.1-0.3mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在120-150℃条件下加热8-12h，自然冷却；
D、过滤后用乙醇反复洗涤固体3-5次，喷雾干燥，即可。
2.如权利要求1所述的具有超强降解效果的BiOCl光催化剂的制备方法，其特征在于，所述的步骤A中，所述的去离子水和乙醇的体积比为1：(6-10)。
3.如权利要求1所述的具有超强降解效果的BiOCl光催化剂的制备方法，其特征在于，所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的2-4倍。
4.如权利要求1所述的具有超强降解效果的BiOCl光催化剂的制备方法，其特征在于，所述的步骤B中，油酸与乙醇的体积比为(1-3)：10；甘油与乙醇的体积比为(0.2-0.5)：10。
5.如权利要求1所述的具有超强降解效果的BiOCl光催化剂的制备方法，其特征在于，包括以下步骤：
A、将适量的硝酸铋溶于去离子水和乙醇的混合溶液中，搅拌得到澄清溶液，其中硝酸铋浓度为0.15mol/L；
B、称量氯化铵、甘油和油酸加入上述溶液中，搅拌均匀；
C、将步骤B得到的混合液转移到带有聚四氟乙烯内衬的不锈钢反应釜中，在128℃条件下加热10h，自然冷却；
D、过滤后用乙醇反复洗涤固体4次，喷雾干燥，即可；
所述的步骤A中，所述的去离子水和乙醇的体积比为1：8.5；
所述的步骤B中，所述的氯化铵的物质的量为硝酸铋物质的量的2.5倍；
所述的步骤B中，油酸与乙醇的体积比为1.5：10；甘油与乙醇的体积比为0.3：10。
6.如权利要求1-5所述的具有超强降解效果的BiOCl光催化剂的制备方法，由该方法制备的BiOCl光催化剂。
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910971427.9A CN110624576A (zh) | 2019-10-14 | 2019-10-14 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
| CN202010806840.2A CN111744509A (zh) | 2019-10-14 | 2020-08-12 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
| US17/038,897 US20210106982A1 (en) | 2019-10-14 | 2020-09-30 | Method for preparing biocl photocatalyst with super strong degradation effect |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910971427.9A CN110624576A (zh) | 2019-10-14 | 2019-10-14 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110624576A true CN110624576A (zh) | 2019-12-31 |
Family
ID=68974980
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910971427.9A Withdrawn CN110624576A (zh) | 2019-10-14 | 2019-10-14 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
| CN202010806840.2A Pending CN111744509A (zh) | 2019-10-14 | 2020-08-12 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010806840.2A Pending CN111744509A (zh) | 2019-10-14 | 2020-08-12 | 一种具有超强降解效果的BiOCl光催化剂的制备方法 |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US20210106982A1 (zh) |
| CN (2) | CN110624576A (zh) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573025A (zh) * | 2022-03-15 | 2022-06-03 | 南京邮电大学 | 一种BiOCl及其多相复合半导体材料的制备方法与应用 |
| CN115069276A (zh) * | 2022-06-29 | 2022-09-20 | 广州尚洁环保科技股份有限公司 | 一种Bi/BiOCl复合纳米光催化剂在光催化降解挥发性有机物中的应用 |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019409B (zh) * | 2021-03-23 | 2022-07-29 | 四川轻化工大学 | 一种Bi2O2CO3/BiOCl催化剂的制备方法及其应用 |
| CN113461054B (zh) * | 2021-07-28 | 2023-08-08 | 中国科学院上海硅酸盐研究所 | 一种BiOCl粉体及其制备方法和应用 |
| CN113663698A (zh) * | 2021-07-28 | 2021-11-19 | 南昌大学 | 一种间接取代法构建氯空位氯氧化铋高活性光催化材料的合成方法 |
| CN116062921A (zh) * | 2021-10-25 | 2023-05-05 | 华南理工大学 | 一种去除酸性高盐废水中氨氮的光催化方法 |
| CN114272943A (zh) * | 2021-11-26 | 2022-04-05 | 国家能源集团科学技术研究院有限公司 | 一种复合催化剂的制备方法及其应用 |
| CN114452985B (zh) * | 2022-02-14 | 2024-04-19 | 温州大学 | 一种用于光催化二氧化碳的CuSbS2纳米管材料制备方法 |
| CN114669309B (zh) * | 2022-05-07 | 2023-11-07 | 桂林电子科技大学 | 一种一维线状BiOCl光催化材料及其制备方法和应用 |
| JP7395064B1 (ja) | 2022-12-15 | 2023-12-08 | 三菱電機株式会社 | 光触媒担持体及び光触媒担持体の製造方法 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664687A (zh) * | 2009-09-29 | 2010-03-10 | 福州大学 | 一种染料敏化的卤氧化铋可见光催化剂的制备及其应用 |
| CN104071842B (zh) * | 2013-03-28 | 2015-12-02 | 浙江伟星实业发展股份有限公司 | 氯氧化铋的制备方法 |
| CN103464175A (zh) * | 2013-09-29 | 2013-12-25 | 南开大学 | 一种可见光光催化剂BiOCl纳米片的制备方法 |
| CN106311288A (zh) * | 2016-07-26 | 2017-01-11 | 南京信息工程大学 | 一种新型Bi7F11O5/BiOCl复合光催化剂的简易制备方法及其光催化性能 |
| CN107162051B (zh) * | 2017-04-27 | 2019-02-19 | 武汉纺织大学 | 花状BiOCl光催化剂的制备方法及制得的BiOCl光催化剂和应用 |
| CN106984340A (zh) * | 2017-04-27 | 2017-07-28 | 武汉纺织大学 | 一种片状BiOCl光催化剂的制备方法及制得的光催化剂和应用 |
-
2019
- 2019-10-14 CN CN201910971427.9A patent/CN110624576A/zh not_active Withdrawn
-
2020
- 2020-08-12 CN CN202010806840.2A patent/CN111744509A/zh active Pending
- 2020-09-30 US US17/038,897 patent/US20210106982A1/en not_active Abandoned
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573025A (zh) * | 2022-03-15 | 2022-06-03 | 南京邮电大学 | 一种BiOCl及其多相复合半导体材料的制备方法与应用 |
| CN114573025B (zh) * | 2022-03-15 | 2023-11-21 | 南京邮电大学 | 一种BiOCl及其多相复合半导体材料的制备方法与应用 |
| CN115069276A (zh) * | 2022-06-29 | 2022-09-20 | 广州尚洁环保科技股份有限公司 | 一种Bi/BiOCl复合纳米光催化剂在光催化降解挥发性有机物中的应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111744509A (zh) | 2020-10-09 |
| US20210106982A1 (en) | 2021-04-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110624576A (zh) | 一种具有超强降解效果的BiOCl光催化剂的制备方法 | |
| CN103264165B (zh) | 一种以单链dna为模板合成银纳米簇的方法 | |
| CN110082329B (zh) | 一种菠萝蛋白酶包裹的荧光铂纳米簇及制备方法和应用 | |
| CN108760701B (zh) | 一种以葵花籽壳为碳源的碳量子点及其制备方法和在检测硫离子中的应用 | |
| CN106442448B (zh) | 一种快速检测硫离子的方法 | |
| CN102507481B (zh) | 一种水环境中硫酸盐还原菌的检测方法 | |
| CN1936546A (zh) | 一种基于光催化化学发光测定化学需氧量的方法及其检测器件 | |
| CN112705195B (zh) | 一种降解和测定四环素的功能材料及制备方法和应用 | |
| Tai et al. | Photolysts of rhodamine-WT dye | |
| CN104399531A (zh) | 一种AgI基无机-有机杂化半导体材料的合成及光催化降解染料的应用 | |
| CN108254366B (zh) | 一种基于苯硼酸功能化的银纳米粒子检测微生物的方法 | |
| Ensafi et al. | Monitoring nitrite with optical sensing films | |
| CN108195828A (zh) | 一种非标记均相检测苯甲酸钠的比色法 | |
| CN114166772B (zh) | 一种利用Cu-g-C3N4纳米酶检测四环素残留的方法 | |
| Hamoudi et al. | Determination of nitrite in meat by azo dye formation | |
| CN108760702B (zh) | 一种硫离子的检测方法 | |
| CN110065989A (zh) | 一种利用微孔结构的金属有机骨架材uio-67衍生物吸附水中有机染料的方法 | |
| CN115155605A (zh) | 一种新型Cu2O/BiVO4复合光催化剂的制备方法及其应用 | |
| CN107185561B (zh) | 一种BiOIxBr(1-x)@SiO2光催化剂及其应用 | |
| CN108404924A (zh) | 一种具有可见光响应的复合光催化剂制备方法 | |
| CN110548864B (zh) | 一种荧光丝胶铂纳米簇及其制备方法和应用 | |
| CN209306989U (zh) | 有机物光解催化器 | |
| Kazemzadeh et al. | Optical nitrite sensor based on chemical modification of a polymer film | |
| CN113667064B (zh) | 一种可视化检测气液体中甲醛水凝胶及其制备方法和应用 | |
| Kampschmidt | Meat discoloration, effect of wave length of light on the discoloration of cured meats |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20191231 |