CN106861725B - A kind of chlorine bismuth vanadate photocatalyst, preparation method and applications - Google Patents
A kind of chlorine bismuth vanadate photocatalyst, preparation method and applications Download PDFInfo
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- CN106861725B CN106861725B CN201611265736.7A CN201611265736A CN106861725B CN 106861725 B CN106861725 B CN 106861725B CN 201611265736 A CN201611265736 A CN 201611265736A CN 106861725 B CN106861725 B CN 106861725B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- OINVEKJWDDEROE-UHFFFAOYSA-N [Cl].[Bi] Chemical compound [Cl].[Bi] OINVEKJWDDEROE-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000460 chlorine Substances 0.000 claims abstract description 70
- 239000000126 substance Substances 0.000 claims abstract description 25
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 22
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 18
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 230000000593 degrading effect Effects 0.000 claims abstract description 6
- 238000004332 deodorization Methods 0.000 claims abstract description 4
- 239000000675 fabric finishing Substances 0.000 claims abstract description 4
- 238000009962 finishing (textile) Methods 0.000 claims abstract description 4
- 239000000975 dye Substances 0.000 claims abstract description 3
- 239000004753 textile Substances 0.000 claims abstract description 3
- 239000002351 wastewater Substances 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 30
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 16
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 6
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 claims description 5
- -1 V5+ Compound Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 2
- 238000007704 wet chemistry method Methods 0.000 abstract description 5
- 229910052797 bismuth Inorganic materials 0.000 abstract description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 3
- 239000011147 inorganic material Substances 0.000 abstract description 3
- 229910001451 bismuth ion Inorganic materials 0.000 abstract description 2
- 231100001261 hazardous Toxicity 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 2
- 238000003836 solid-state method Methods 0.000 abstract 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 14
- 230000015556 catabolic process Effects 0.000 description 13
- 238000006731 degradation reaction Methods 0.000 description 13
- 229940043267 rhodamine b Drugs 0.000 description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000010532 solid phase synthesis reaction Methods 0.000 description 8
- 238000005286 illumination Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000003912 environmental pollution Methods 0.000 description 5
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- 238000003911 water pollution Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- WGKMWBIFNQLOKM-UHFFFAOYSA-N [O].[Cl] Chemical compound [O].[Cl] WGKMWBIFNQLOKM-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229940036348 bismuth carbonate Drugs 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- GMZOPRQQINFLPQ-UHFFFAOYSA-H dibismuth;tricarbonate Chemical compound [Bi+3].[Bi+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GMZOPRQQINFLPQ-UHFFFAOYSA-H 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 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 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 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
- B01J27/08—Halides
- B01J27/10—Chlorides
-
- B01J35/39—
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/30—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The invention discloses a kind of chlorine bismuth vanadate photocatalysts, preparation method and applications.Chlorine bismuth vanadate photocatalyst chemical expression is Bi9V2O18Cl.The present invention uses high temperature solid-state method or wet chemistry method, and the chlorine bismuth vanadate photocatalyst being prepared is that one kind contains Bi3+The inorganic material of bismuth ion, prepares convenient and efficient, realizes and generates light-catalysed reaction under the irradiation of visible light, and light-catalysed efficiency is higher, and the physics and chemical property of photochemical catalyst are stablized.Chlorine pucherite provided by the invention can be used for organic dyestuff, organic hazardous solvent in degrading waste water；Also it can be used as fabric finishing agent, be used as preparation antibacterial, deodorization functions textile.
Description
Technical field
The present invention relates to a kind of catalysis materials, preparation method and application, it is a kind of inorganic material, in particular to a kind of
Photochemical catalyst chlorine pucherite Bi for degradable organic pollutant9V2O18Cl and preparation method thereof.
Background technique
With the rapid development of industry, people enjoy while science and technology is brought convenience to life and also result in living environment
Deteriorate, especially the water pollution closely bound up with life.Present water pollution already leads to death and the biology of a large amount of marine organisms
Kind falls sharply；Simultaneously also by considerable influence in terms of domestic water.In order to meet the eager needs of sustainable development, urgently
It need to solve problem of environmental pollution.In many environmental pollutions, most common is water pollution, and anxious with people's work and life
Cut relevant problem.Therefore, effectively curbing environmental pollution is the emphasis of environmental protection.Currently, widely used solution environmental pollution
Method have: chemical oxidization method, physisorphtion, high temperature incineration method and microorganism treatment.These processing methods can not incite somebody to action
Pollutant is thoroughly innoxious, and it is also possible to the problem of bringing secondary pollution.How green, it is efficient solve water pollution at
The problem of for current urgent need to resolve.
Inorganic photocatalyst applications are in the major progress that the processing of environmental pollution is in recent years, wherein with titanium dioxide TiO2
Headed by conductor photocatalysis material have become a hot topic of research.But it since these material forbidden bandwidths are big, needs to absorb ultraviolet
The problem of light is just able to achieve photocatalysis, brings in this way is that application efficiency is low.So haveing been devoted to widen titanium dioxide both at home and abroad
Absorption spectrum.Researcher widens visible light by a series of modifications to catalysis material, such as doping, compound means at present
Response, or find other emerging catalysis materials.Finding novel high efficiency photocatalyst is photocatalysis field one difficult
Huge and long-term task is photocatalytic applications in contaminant degradation, the core in photolysis water hydrogen field.
Summary of the invention
The present invention for deficiency existing for existing catalysis material, provide a kind of preparation method simply, to organic pollutant
The chlorine bismuth vanadate photocatalyst of Photocatalytic Activity for Degradation function admirable, preparation method and applications.
To achieve the above object of the invention, the technical solution adopted by the present invention is that providing a kind of chlorine bismuth vanadate photocatalyst, it
Chemical general formula be Bi9V2O18Cl。
Technical solution of the present invention includes preparing two methods of chlorine bismuth vanadate photocatalyst as described above, and one is using solid
Phase method for calcinating, includes the following steps:
(1) chemical formula Bi is pressed9V2O18The metering ratio of Cl, weighs respectively containing Bi3+、V5+And Cl-Compound, filled in mortar
Divide grinding, is uniformly mixed, obtains mixture；
(2) mixture to be calcined in air atmosphere, calcination temperature is 300~600 DEG C, and calcination time is 3~9 hours,
Crude product is obtained after natural cooling；
(3) by crude product grinding, be uniformly mixed, calcined in air atmosphere, calcination temperature is 600~900 DEG C, when calcining
Between be 6~8 hours；A kind of chlorine pucherite catalysis material is obtained after natural cooling.
In solid phase calcination preparation method, calcination temperature described in step (2) is 300~500 DEG C, and calcination time is 3~6 small
When；Calcination temperature described in step (3) is 500~850 DEG C, and calcination time is 6~8 hours.
Another preparation method of chlorine bismuth vanadate photocatalyst of the present invention is to use wet chemical method, including walk as follows
It is rapid:
(1) chemical formula Bi is pressed9V2O18Cl measures ratio, is weighed respectively containing Bi3+、V5+And Cl-Compound；Bi will be contained3+And V5+
Compound be dissolved in deionized water or nitric acid solution respectively, then by mol, add 1~3 times of complexing agent of total cation
Oxalic acid or citric acid are obtained containing Bi3+And V5+ Compound solution；
(2) Cl will be contained-Compound be dissolved in nitric acid, diluted with deionized water, then add that step (1) obtains containing Bi3+
And V5+ Compound solution, obtain transparent mixed liquor；
(3) transparent mixed solution that step (2) obtains is stirred at room temperature 3~8 hours, then temperature be 37~80 DEG C
Under conditions of stand 3~6 hours；
(4) mixed liquor for obtaining step (3) is dried 10~20 hours under conditions of temperature is 100~120 DEG C,
Obtain fluffy presoma；
(5) obtained presoma is ground into powder, in air atmosphere calcine 2~8 hours, calcination temperature be 500~
It 850 DEG C, is cooled to room temperature, obtains chlorine bismuth vanadate photocatalyst.
In wet chemical method, the calcination temperature of step (5) is 600~750 DEG C, and calcination time is 2~7 hours.
In technical solution of the present invention, described contains Bi3+Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·
0.5H2One of O；Described contains V5+Compound be V2O5、NH4VO3One of；Described contains Cl-Compound be
NH4One of Cl, BiOCl.
Technical solution of the present invention further includes the application of prepared chlorine bismuth vanadate photocatalyst, first is that as inorganic photocatalysis
Material, for organic dyestuff, the organic hazardous solvent in degrading waste water.
Another purposes is to be used as preparation antibacterial, deodorization functions textile as fabric finishing agent.
Chlorine pucherite provided by the invention is that one kind contains Bi3+The inorganic material of bismuth ion prepares convenient and efficient, complete reality
Show and generated light-catalysed reaction under the irradiation of visible light, light-catalysed efficiency is higher, the physics of photochemical catalyst and chemically
Matter is stablized.
Compared with prior art, technical solution of the present invention advantage is:
1, Bi provided by the invention9V2O18The preparation of Cl catalysis material is simple, the photocatalysis of solid phase and wet chemistry method preparation
Material particle size is relatively uniform.
2, Bi prepared by the present invention9V2O18Cl catalysis material has preferable response, the catalysis material in visible light region
Material can efficient catalytic degradation rhodamine B, there is good photocatalytic activity, be a kind of efficient catalysis material.
3, pollution-free in catalysis material preparation process provided by the invention, no waste gas and waste liquid discharge, calcination temperature is lower,
Production cost is low, environmental-friendly.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction pattern that the embodiment of the present invention 1 prepares sample using solid phase method；
Fig. 2 embodiment of the present invention 1 is using Bi obtained by solid phase method9V2O18The SEM(scanning electron microscopy of Cl sample
Mirror) map；
Fig. 3 embodiment of the present invention 1 is using Bi obtained by solid phase method9V2O18The dynamics of Cl sample degradation rhodamine B
Curve graph；
Fig. 4 embodiment of the present invention 2 is using Bi obtained by solid phase method9V2O18The UV-Vis DRS light of Cl sample
Spectrum；
The Bi that Fig. 5 embodiment of the present invention 2 is prepared using solid phase method9V2O18The catalysis material of Cl and direct illumination degrading
The comparison diagram of rhodamine B effect；
Fig. 6 embodiment of the present invention 3 prepares the X-ray powder diffraction pattern of sample using wet chemical method；
Fig. 7 is the embodiment of the present invention 3 using Bi obtained by wet chemical method9V2O18The SEM spectrum of Cl sample；
Fig. 8 is the embodiment of the present invention 4 using Bi obtained by wet chemical method9V2O18Cl sample degradation rhodamine B moves
Force diagram figure；
Fig. 9 is the embodiment of the present invention 4 using Bi obtained by wet chemical method9V2O18The ultraviolet-visible of Cl sample is unrestrained anti-
Penetrate spectrum；
The Bi that Figure 10 embodiment of the present invention 4 is prepared using wet chemical method9V2O18The catalysis material of Cl and direct illumination
The comparison diagram of rhodamine B degradation effect.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in further detail.
Embodiment 1:
The present embodiment prepares Bi using solid sintering technology9V2O18Cl.Specific steps are as follows: press chemical formula Bi9V2O18Cl, respectively
Weigh bismuth oxide Bi2O3: 1.456 grams；BiOCl:1.302 grams of bismuth oxychloride；Ammonium metavanadate NH4VO3: 0.2925 gram；In mortar
It grinds and is uniformly mixed, air atmosphere is selected to calcine for the first time, temperature is 300 DEG C, and calcination time is 6 hours, is then cooled to room
Temperature takes out crude product.Obtained crude product is fully ground again, is uniformly mixed, is calcined in air atmosphere, calcination temperature is
850 DEG C, calcination time is 6 hours, is cooled to room temperature, and takes out sample to get chlorine pucherite Bi is arrived9V2O18Cl powder.
Referring to attached drawing 1, it is that the present embodiment prepares sample Bi9V2O18The X-ray powder diffraction figure of Cl, XRD test result
It has been shown that, prepared chlorine pucherite Bi9V2O18Cl is monophase materials, and no other miscellaneous phases exist, and has preferable crystallinity.
Referring to attached drawing 2, it is that the present embodiment prepares sample Bi9V2O18The SEM of Cl schemes, and material crystalline is functional, sample
Particle size is uniform.
By chlorine pucherite Bi provided in this embodiment9V2O18Cl material photocatalyst, applied in degradation water body
Rhodamine.Referring to attached drawing 3, it is sample Bi prepared by the present embodiment9V2O18The kinetic curve of Cl rhodamine B degradation, degradation
Constant is 0.11min-1。
Embodiment 2:
The present embodiment prepares Bi using solid sintering technology9V2O18Cl.Specific steps are as follows: according to chemical formula Bi9V2O18Cl, point
Also known as take V2O5: 0.23 gram, Bi (NO3)3·5H2O:5.46 grams, ammonium chloride NH4It Cl:0.267 grams, grinds and mixes in mortar
Uniformly, selection air atmosphere is calcined for the first time, and temperature is 450 DEG C, and calcination time is 5 hours, is then cooled to room temperature, takes out thick produce
Object.Then, crude product is fully ground again, is uniformly mixed, is calcined in air atmosphere, calcination temperature is 700 DEG C, when calcining
Between be 7 hours, be cooled to room temperature, take out sample to get arrive chlorine bismuth vanadate photocatalyst Bi9V2O18Cl powder.
Referring to attached drawing 4, it is the ultraviolet-visible diffuse reflectance spectrum of the present embodiment sample, from map as can be seen that can
There is preferable absorption in light-exposed range.Other performances are similar to Example 1.
Referring to attached drawing 5, it is the Bi that the embodiment of the present invention uses solid phase method preparation9V2O18The catalysis material of Cl and straight
Connect the comparison diagram of illumination degrading rhodamine B effect；Under visible light illumination, 120 minutes when rhodamine B degradation rate up to 88%,
It can be seen that Bi provided in this embodiment9V2O18Cl have photocatalysis, material to rhodamine B in water have it is good can
Light-exposed catalytic performance.
Embodiment 3:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl, specific steps include: according to chemical formula Bi9V2O18Cl, point
Also known as take bismuth oxide Bi2O3: 1.88 grams, it is dissolved in dust technology and is added 1 times (molar ratio) of citric acid progress complex reaction；
Weigh vanadic anhydride V2O5: 0.303 gram, it is dissolved in dust technology and is added 2 times (molar ratio) of citric acid progress complex reaction；
By weighed ammonium chloride NH4Cl:0.356 grams, be dissolved in suitable nitric acid, and diluted with deionized water, by the bismuth after complexing from
The nitrate solution of son and vanadium ion is added in the ammonium chloride solution of complexing, is stirred at room temperature 6 hours, is put in 37 DEG C of standings
6 hours, 100 DEG C drying 10 hours in baking oven are transferred to, obtain fluffy presoma, grinding obtains powder, and at 750 DEG C, calcining 2 is small
When, it is cooled to room temperature, obtains chlorine pucherite catalysis material.
Referring to attached drawing 6, it is Bi manufactured in the present embodiment9V2O18The X ray powder diffraction pattern of Cl sample, XRD test
The results show that prepared chlorine pucherite Bi9V2O18Cl is monophase materials, and no other miscellaneous phases exist, and crystallinity is preferable.
Referring to attached drawing 7, it is the present embodiment using Bi obtained by chemical method9V2O18The SEM(scanning electron of Cl sample
Microscope) map, the particle size of preparation is relatively uniform.
Embodiment 4:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl, step include: by chemical formula Bi9V2O18Cl is weighed respectively
Bismuth nitrate Bi (NO3)3·5H2It O:4.043 grams, is dissolved in dust technology and the oxalic acid that 3 times (molar ratios) are added is complexed, chlorine oxygen
Change BiOCl:1.7362 grams of bismuth, is dissolved in dust technology and the oxalic acid that 3 times (molar ratios) are added is complexed, by ammonium metavanadate
NH4VO3: it 2.0 grams, is dissolved in suitable nitric acid, and diluted with deionized water, three kinds of solution is mixed, it is small to be stirred at room temperature 8
When, it being put in 80 DEG C and stands 3 hours, be transferred to 120 DEG C drying 12 hours in baking oven, obtain fluffy presoma, grinding obtains powder,
It is calcined 7 hours at 500 DEG C, is cooled to room temperature, obtains chlorine pucherite catalysis material.
It is the embodiment of the present invention using Bi obtained by chemical method referring to attached drawing 89V2O18Cl sample degradation rhodamine B
Dynamic curve diagram, degradation constant is 0.018min-1；
Referring to attached drawing 9, for the ultraviolet-visible diffuse reflectance spectrum for being the present embodiment sample, from map as can be seen that can
There is preferable absorption in light-exposed range.Other performance is similar to Example 3.
It is the embodiment of the present invention using Bi obtained by chemical method referring to attached drawing 109V2O18The catalysis material of Cl with
The comparison diagram of direct illumination degrading rhodamine B effect, under visible light illumination, the degradation rate of rhodamine B is reachable at 120 minutes
90%, it can be seen that Bi9V2O18The Cl catalysis material has good visible light catalytic performance to rhodamine B in water.
Embodiment 5:
The present embodiment prepares Bi using solid sintering technology9V2O18Cl.By chemical formula Bi9V2O18Cl weighs basic carbonate respectively
Bismuth (BiO)2CO3·0.5H2O:1.622 grams, ammonium metavanadate NH4VO3: it 0.2925 gram, BiOCl:1.302 grams of bismuth oxychloride, is grinding
It grinds and is uniformly mixed in alms bowl, air atmosphere is selected to calcine for the first time, temperature is 500 DEG C, and calcination time is 3 hours, then cold
To room temperature, sample is taken out.Then, preceding step sample is fully ground again, is uniformly mixed, is calcined in air atmosphere, calcining temperature
Degree is 600 DEG C, and calcination time is 8 hours, is cooled to room temperature, and takes out sample to get chlorine bismuth vanadate photocatalyst Bi is arrived9V2O18Cl
Powder.Performance is similar to Examples 1 and 2.
Embodiment 6:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl.By chemical formula Bi9V2O18Cl weighs basic bismuth carbonate respectively
(BiO)2CO3·0.5H2It O:3.892 grams, is dissolved in dust technology and the citric acid that 1 times (molar ratio) is added is complexed, five oxidations
Two vanadium V2O5: it 1.0 grams, is dissolved in dust technology and the citric acid that 1 times (molar ratio) is added is complexed, by ammonium chloride NH4Cl:
It 0.3566 gram, is dissolved in suitable nitric acid, and diluted with deionized water, three kinds of solution is mixed, are stirred at room temperature 6 hours,
It being put in 60 DEG C and stands 5 hours, be transferred to 110 DEG C drying 11 hours in baking oven, obtain fluffy presoma, grinding obtains powder,
At 650 DEG C, calcines 5 hours, be cooled to room temperature, obtain chlorine pucherite catalysis material.Performance is similar to embodiment 3 and 4.
Embodiment 7:
Chlorine pucherite Bi prepared by the embodiment of the present invention 19V2O18Cl is dispersed in water, and the concentration of chlorine pucherite is
3000ppm is used as fabric finishing agent.Fabric is impregnated in finishing agent, the dosage of chlorine pucherite is dry cloth weight in finishing agent
5%, after second dipping and rolling process, the preliminary drying 5min in 100 DEG C of open width dryers, then dried in 140 DEG C of open width dryers
Dry 3min, obtains a kind of fabric with antibacterial and deodouring function.Due to chlorine pucherite Bi provided by the invention9V2O18Cl has light
The wide characteristic of response range is composed, is able to achieve and generates photochemical reaction under visible light illumination, microorganism death, organic matter drop can be made
Solution, thus have the function of antibacterial, deodorization and effect to fabric after handling.
Referring to table 1, sample is antibacterial when washing 50 times after chlorine pucherite finishing agent arranges front and back and arranges for fabric
Rate result.
Table 1: anti-bacteria test result
| Bacteriostasis rate | Before arrangement | After arrangement | It is washed 50 times after arrangement |
| Escherichia coli | 11.2% | 99.9% | 99.8% |
| Staphylococcus aureus | 8.5% | 99.9% | 99.9% |
Seen from table 1, after arranging by finishing agent provided in this embodiment to fabric, there is excellent antibacterial effect,
Antibacterial effect does not change substantially after washing 50 times.
Claims (7)
1. a kind of preparation method of chlorine bismuth vanadate photocatalyst, it is characterised in that use solid phase calcination method, include the following steps:
(1) chemical formula Bi is pressed9V2O18The metering ratio of Cl, weighs respectively containing Bi3+、V5+And Cl-Compound, sufficiently ground in mortar
Mill is uniformly mixed, obtains mixture；
(2) mixture is calcined in air atmosphere, calcination temperature is 300~600 DEG C, and calcination time is 3~9 hours, natural
Crude product is obtained after cooling；
(3) crude product ground, be uniformly mixed, calcined in air atmosphere, calcination temperature is 600~900 DEG C, and calcination time is
6~8 hours；A kind of chlorine pucherite catalysis material is obtained after natural cooling.
2. a kind of preparation method of chlorine bismuth vanadate photocatalyst according to claim 1, it is characterised in that: described contains Bi3 +Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·0.5H2One of O；Described contains V5+Compound be
V2O5、NH4VO3One of；Described contains Cl-Compound be NH4One of Cl, BiOCl.
3. a kind of preparation method of chlorine bismuth vanadate photocatalyst, it is characterised in that use wet chemical method, include the following steps:
(1) chemical formula Bi is pressed9V2O18Cl measures ratio, is weighed respectively containing Bi3+、V5+And Cl-Compound；Bi will be contained3+And V5+Change
It closes object to be dissolved in respectively in deionized water or nitric acid solution, then by mol, adds 1~3 times of complexing agent oxalic acid of total cation
Or citric acid, it obtains containing Bi3+And V5+ Compound solution；
(2) Cl will be contained-Compound be dissolved in nitric acid, diluted with deionized water, then add that step (1) obtains containing Bi3+And V5 + Compound solution, obtain transparent mixed liquor；
(3) transparent mixed solution that step (2) obtains is stirred at room temperature 3~8 hours, then the item for being 37~80 DEG C in temperature
3~6 hours are stood under part；
(4) mixed liquor for obtaining step (3) is dried 10~20 hours under conditions of temperature is 100~120 DEG C, is obtained
Fluffy presoma；
(5) obtained presoma is ground into powder, calcined 2~8 hours in air atmosphere, calcination temperature is 500~850
DEG C, it is cooled to room temperature, obtains chlorine bismuth vanadate photocatalyst.
4. a kind of preparation method of chlorine bismuth vanadate photocatalyst according to claim 3, which is characterized in that described contains
Bi3+Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·0.5H2One of O；Described contains V5+Compound
For V2O5、NH4VO3One of；Described contains Cl-Compound be NH4One of Cl, BiOCl.
5. a kind of preparation method of chlorine bismuth vanadate photocatalyst according to claim 3, it is characterised in that: step (5)
Calcination temperature is 600~750 DEG C, and calcination time is 2~7 hours.
6. a kind of product that the preparation method using chlorine bismuth vanadate photocatalyst described in claim 1 or 3 is prepared is answered
With as inorganic catalysis material, for the organic dyestuff in degrading waste water.
7. a kind of product that the preparation method using chlorine bismuth vanadate photocatalyst described in claim 1 or 3 is prepared is answered
With as fabric finishing agent, as preparation antibacterial, deodorization functions textile.
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Effective date of registration: 20200721 Address after: Room 2607, building 17, No. 3188 Renmin Road, Gusu District, Jinhua City, Zhejiang Province Patentee after: Xiong Ying Address before: 2607, room 17, building 3188, 215002 Renmin Road, Suzhou District, Jiangsu, Suzhou, China Patentee before: SUZHOU SECCRY CLOTHING Co.,Ltd. |
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