CN106861725A - 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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- CN106861725A CN106861725A CN201611265736.7A CN201611265736A CN106861725A CN 106861725 A CN106861725 A CN 106861725A CN 201611265736 A CN201611265736 A CN 201611265736A CN 106861725 A CN106861725 A CN 106861725A
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- Prior art keywords
- chlorine
- bismuth vanadate
- compound
- hours
- vanadate photocatalyst
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- OINVEKJWDDEROE-UHFFFAOYSA-N [Cl].[Bi] Chemical compound [Cl].[Bi] OINVEKJWDDEROE-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000460 chlorine Substances 0.000 claims abstract description 72
- 239000000126 substance Substances 0.000 claims abstract description 26
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 23
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 230000000593 degrading effect Effects 0.000 claims abstract description 6
- 239000000675 fabric finishing Substances 0.000 claims abstract description 4
- 238000009962 finishing (textile) Methods 0.000 claims abstract description 4
- 238000004332 deodorization Methods 0.000 claims abstract description 3
- 239000000975 dye Substances 0.000 claims abstract description 3
- 231100001261 hazardous Toxicity 0.000 claims abstract description 3
- 239000002904 solvent 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 38
- 239000000463 material Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 19
- 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 17
- 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
- 150000001875 compounds Chemical class 0.000 claims description 11
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 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
- 238000000227 grinding Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 6
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- -1 V5+ Compound Chemical class 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 241000894006 Bacteria Species 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 238000007704 wet chemistry method Methods 0.000 abstract description 5
- 229910001451 bismuth ion Inorganic materials 0.000 abstract description 3
- 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
- 229910052797 bismuth Inorganic materials 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract 1
- 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 13
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
- 229940043267 rhodamine b Drugs 0.000 description 9
- 238000010532 solid phase synthesis reaction Methods 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000003912 environmental pollution Methods 0.000 description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 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
- 238000003911 water pollution Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 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
- 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
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229940036348 bismuth carbonate Drugs 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000536 complexating effect Effects 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
- 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 2
- 244000005700 microbiome Species 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 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
- 238000000862 absorption spectrum Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 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
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000011161 development 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
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 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
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 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
- 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
- B01J35/30—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
- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of chlorine bismuth vanadate photocatalyst, 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 for preparing is that one kind contains Bi3+The inorganic material of bismuth ion, prepares convenient and swift, realizes and light-catalysed reaction is produced under the irradiation of visible ray, and light-catalysed efficiency is higher, the physics and stable chemical nature of photochemical catalyst.Organic dyestuff, organic hazardous solvent that the chlorine pucherite that the present invention is provided can be used in degrading waste water;Also can be as fabric finishing agent, as preparation antibacterial, deodorization functions textile.
Description
Technical field
The present invention relates to a kind of catalysis material, preparation method and application, it is a kind of inorganic material, more particularly to a kind of
For the photochemical catalyst chlorine pucherite Bi of degradable organic pollutant9V2O18Cl and preparation method thereof.
Background technology
With developing rapidly for industry, people enjoy while science and technology brings convenience to life and also result in living environment
Deteriorate, particularly with closely bound up water pollution of living.Present water pollution already leads to the dead and biology of a large amount of marine organisms
Kind falls sharply;Domestic water aspect is also subject to considerable influence simultaneously.In order to meet the eager needs of sustainable development, urgently
Problem of environmental pollution need to be solved.In many environmental pollutions, most common is water pollution, is also to work and live anxious with people
The problem that cut is closed.Therefore, it is the emphasis of environmental protection effectively to curb environmental pollution.At present, widely used solution environmental pollution
Method have:Chemical oxidization method, physisorphtion, high temperature incineration method and microorganism treatment.These processing methods can not be by
Pollutant is thoroughly innoxious, and it is also possible to brings the problem of secondary pollution.How green, it is efficient solve water pollution into
It is the problem of current urgent need to resolve.
Inorganic photocatalyst applications in the major progress that the treatment of environmental pollution is in recent years, wherein with titanium dioxide TiO2
Headed by conductor photocatalysis material turn into research focus.But, because these material energy gaps are big, it is necessary to absorb ultraviolet
Light could realize photocatalysis, and the problem so brought is low application efficiency.So, it is devoted to widening titanium dioxide both at home and abroad always
Absorption spectrum.Current researcher is by a series of modified of catalysis material, such as adulterating, compound means widen visible ray
Response, or find other emerging catalysis materials.It is that photocatalysis field one is difficult to find new high efficiency photocatalyst
Huge and long-term task is photocatalytic applications in contaminant degradation, the core in photolysis water hydrogen field.
The content of the invention
The deficiency that the present invention exists for existing catalysis material, there is provided a kind of preparation method is simple, to organic pollution
Photocatalytic Activity for Degradation function admirable chlorine bismuth vanadate photocatalyst, preparation method and applications.
To achieve the above object of the invention, the technical solution adopted by the present invention is to provide 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 kind is using solid
Phase method for calcinating, comprises the following steps:
(1)By chemical formula Bi9V2O18The metering ratio of Cl, weighs containing Bi respectively3+、V5+And Cl-Compound, fully ground in mortar
Mill, is well mixed, and obtains mixture;
(2)Mixture is calcined in air atmosphere, calcining heat is 300~600 DEG C, calcination time is 3~9 hours, natural
Crude product is obtained after cooling;
(3)By crude product grinding, well mixed, the calcining in air atmosphere, calcining heat is 600~900 DEG C, and calcination time is
6~8 hours;A kind of chlorine pucherite catalysis material is obtained after natural cooling.
In solid phase calcination preparation method, step(2)Described calcining heat is 300~500 DEG C, and calcination time is 3~6 small
When;Step(3)Described calcining heat 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 following step
Suddenly:
(1)By chemical formula Bi9V2O18Cl meterings ratio, weighs containing Bi respectively3+、V5+And Cl-Compound;Bi will be contained3+And V5+Change
Compound is dissolved in deionized water or salpeter solution respectively, then by mol, adds 1~3 times of total cation of complexing agent oxalic acid
Or citric acid, obtain containing Bi3+And V5+ Compound solution;
(2)Cl will be contained-Compound be dissolved in nitric acid, diluted with deionized water, then add step(1)Obtain containing Bi3+And V5 + Compound solution, obtain transparent mixed liquor;
(3)By step(2)The transparent mixed solution for obtaining is stirred at room temperature 3~8 hours, then in the bar that temperature is 37~80 DEG C
3~6 hours are stood under part;
(4)By step(3)The mixed liquor for obtaining dried process 10~20 hours under conditions of temperature is for 100~120 DEG C, obtain
Fluffy presoma;
(5)The presoma that will be obtained grinds to form powder, calcines 2~8 hours in air atmosphere, and calcining heat is 500~850
DEG C, room temperature is cooled to, obtain chlorine bismuth vanadate photocatalyst.
In wet chemical method, step(5)Calcining heat be 600~750 DEG C, calcination time be 2~7 hours.
It is described containing Bi in technical solution of the present invention3+Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·
0.5H2One kind in O;It is described containing V5+Compound be V2O5、NH4VO3In one kind;It is described containing Cl-Compound be
NH4One kind in Cl, BiOCl.
Technical solution of the present invention also includes the application of prepared chlorine bismuth vanadate photocatalyst, and one is as inorganic photocatalysis
Material, for the organic dyestuff in degrading waste water, organic hazardous solvent.
Another purposes is as fabric finishing agent, as preparation antibacterial, deodorization functions textile.
The chlorine pucherite that the present invention is provided is that one kind contains Bi3+The inorganic material of bismuth ion, prepares convenient and swift, complete reality
Show and light-catalysed reaction has been produced under the irradiation of visible ray, light-catalysed efficiency is higher, the physics of photochemical catalyst and chemically
Matter stabilization.
Compared with prior art, technical solution of the present invention advantage is:
1st, the Bi that the present invention is provided9V2O18Cl catalysis materials prepare simple, catalysis material prepared by solid phase and wet chemistry method
Particle size is than more uniform.
2nd, Bi prepared by the present invention9V2O18Cl catalysis materials have preferably response, the catalysis material in visible region
Material can efficient catalytic degradation rhodamine B, be a kind of efficient catalysis material with good photocatalytic activity.
3rd, pollution-free in the catalysis material preparation process that the present invention is provided, without waste gas and waste liquid discharge, calcining heat is relatively low,
Low production cost, it is environment-friendly.
Brief description of the drawings
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 the Bi obtained by solid phase method9V2O18The SEM of Cl samples(SEM)Figure
Spectrum;
Fig. 3 embodiment of the present invention 1 is using the Bi obtained by solid phase method9V2O18The kinetic curve of Cl sample degradation rhodamine Bs
Figure;
Fig. 4 embodiment of the present invention 2 is using the Bi obtained by solid phase method9V2O18The UV-Vis DRS spectrum of Cl samples;
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 Luo Dan
The comparison diagram of bright B effects;
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 the Bi obtained by wet chemical method9V2O18The SEM spectrum of Cl samples;
Fig. 8 is the embodiment of the present invention 4 using the Bi obtained by wet chemical method9V2O18The dynamics of Cl sample degradation rhodamine Bs
Curve map;
Fig. 9 is the embodiment of the present invention 4 using the Bi obtained by wet chemical method9V2O18The UV-Vis DRS light of Cl samples
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 degrading
The comparison diagram of rhodamine B 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.Concretely comprise the following steps:By chemical formula Bi9V2O18Cl, weighs respectively
Bismuth oxide Bi2O3:1.456 grams;Bismoclite BiOCl:1.302 grams;Ammonium metavanadate NH4VO3:0.2925 gram;Ground in mortar
And be well mixed, selection air atmosphere is calcined for the first time, and temperature is 300 DEG C, and calcination time is 6 hours, is then cooled to room temperature, is taken
Go out crude product.The crude product that will be obtained is fully ground again, is well mixed, and is calcined in air atmosphere, and calcining heat is 850
DEG C, calcination time is 6 hours, is cooled to room temperature, takes out sample, that is, obtain chlorine pucherite Bi9V2O18Cl powder.
Referring to accompanying drawing 1, it is that the present embodiment prepares sample Bi9V2O18The X-ray powder diffraction figure of Cl, XRD test results
It has been shown that, prepared chlorine pucherite Bi9V2O18Cl is monophase materialses, is existed without other dephasigns, with preferable crystallinity.
Referring to accompanying drawing 2, it is that the present embodiment prepares sample Bi9V2O18The SEM figures of Cl, material crystalline is functional, sample
Particle size is uniform.
The chlorine pucherite Bi that the present embodiment is provided9V2O18Cl material photocatalysts, are applied in degraded water body
Rhodamine.Referring to accompanying drawing 3, it is sample Bi prepared by the present embodiment9V2O18The kinetic curve of Cl rhodamine B degradations, degraded
Constant is 0.11min-1。
Embodiment 2:
The present embodiment prepares Bi using solid sintering technology9V2O18Cl.Concretely comprise the following steps:According to chemical formula Bi9V2O18Cl, claims respectively
Take V2O5:0.23 gram, Bi (NO3)3·5H2O:5.46 grams, ammonium chloride NH4Cl:0.267 gram, ground in mortar and be well mixed,
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 crude product.So
Afterwards, crude product is fully ground again, is well mixed, calcined in air atmosphere, calcining heat is 700 DEG C, and calcination time is 7
Hour, room temperature is cooled to, take out sample, that is, obtain chlorine bismuth vanadate photocatalyst Bi9V2O18Cl powder.
Referring to accompanying drawing 4, it is the UV-Vis DRS spectrum of the present embodiment sample, as can be seen that can from collection of illustrative plates
See in optical range there is preferably absorption.Other performances are similar to Example 1.
Referring to accompanying drawing 5, it is the Bi that the embodiment of the present invention is prepared using solid phase method9V2O18The catalysis material of Cl with it is 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%,
As can be seen that the Bi that the present embodiment is provided9V2O18Cl has a photocatalysis, material have to rhodamine B in water it is good can
See photocatalysis performance.
Embodiment 3:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl, specific steps include:According to chemical formula Bi9V2O18Cl, claims respectively
Take bismuth oxide Bi2O3:1.88 grams, it is dissolved in dust technology and adds 1 times(Mol ratio)Citric acid carry out complex reaction;Weigh
Vanadic anhydride V2O5:0.303 gram, it is dissolved in dust technology and adds 2 times(Mol ratio)Citric acid carry out complex reaction;To claim
The ammonium chloride NH for taking4Cl:0.356 gram, be dissolved in appropriate nitric acid, and with deionized water dilute, by the bismuth ion after complexing with
The nitrate solution of 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 small
When, 100 DEG C of dryings 10 hours are transferred in baking oven, fluffy presoma is obtained, grinding obtains powder, at 750 DEG C, calcines 2 hours,
Room temperature is cooled to, chlorine pucherite catalysis material is obtained.
Referring to accompanying drawing 6, it is Bi manufactured in the present embodiment9V2O18The X ray powder diffraction patterns of Cl samples, XRD tests
Result shows, prepared chlorine pucherite Bi9V2O18Cl is monophase materialses, is existed without other dephasigns, and crystallinity is preferable.
Referring to accompanying drawing 7, it is the present embodiment using the Bi obtained by chemical method9V2O18The SEM of Cl samples(Scanning electron
Microscope)Collection of illustrative plates, the particle size of preparation is than more uniform.
Embodiment 4:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl, step includes:By chemical formula Bi9V2O18Cl, weighs nitric acid respectively
Bismuth Bi (NO3)3·5H2O:4.043 grams, it is dissolved in dust technology and adds 3 times(Mol ratio)Oxalic acid be complexed, bismoclite
BiOCl:1.7362 grams, it is dissolved in dust technology and adds 3 times(Mol ratio)Oxalic acid be complexed, by ammonium metavanadate NH4VO3:
2.0 grams, it is dissolved in appropriate nitric acid, and is diluted with deionized water, three kinds of solution are mixed, be stirred at room temperature 8 hours, is put in
80 DEG C stand 3 hours, are transferred in baking oven 120 DEG C of dryings 12 hours, obtain fluffy presoma, and grinding obtains powder, at 500 DEG C
Calcining 7 hours, is cooled to room temperature, obtains chlorine pucherite catalysis material.
It is the embodiment of the present invention using the Bi obtained by chemical method referring to accompanying drawing 89V2O18Cl sample degradation rhodamine Bs
Dynamic curve diagram, degradation constant is 0.018min-1;
Referring to accompanying drawing 9, to be the UV-Vis DRS spectrum of the present embodiment sample, as can be seen that in visible ray from collection of illustrative plates
In the range of have preferably absorption.Other performance is similar to Example 3.
It is the embodiment of the present invention using the Bi obtained by chemical method referring to accompanying drawing 109V2O18The catalysis material of Cl with
, according to the comparison diagram of rhodamine B degradation effect, under visible light illumination, the degradation rate of rhodamine B is reachable at 120 minutes for direct light
90%, it can be seen that Bi9V2O18The Cl catalysis materials have 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 bismuth carbonate respectively
(BiO)2CO3·0.5H2O:1.622 grams, ammonium metavanadate NH4VO3:0.2925 gram, bismoclite BiOCl:1.302 grams, in mortar
Middle grinding is simultaneously well mixed, and selection air atmosphere is calcined for the first time, and temperature is 500 DEG C, and calcination time is 3 hours, is then cooled to
Room temperature, takes out sample.Then, preceding step sample is fully ground again, is well mixed, calcined in air atmosphere, calcining heat
It is 600 DEG C, calcination time is 8 hours, is cooled to room temperature, take out sample, that is, obtains chlorine bismuth vanadate photocatalyst Bi9V2O18Cl powder
End.Performance is similar to embodiment 1 and 2.
Embodiment 6:
The present embodiment prepares Bi using wet chemistry method9V2O18Cl.By chemical formula Bi9V2O18Cl, weighs basic bismuth carbonate respectively
(BiO)2CO3·0.5H2O:3.892 grams, it is dissolved in dust technology and adds 1 times(Mol ratio)Citric acid be complexed, five oxidation
Two vanadium V2O5:1.0 grams, it is dissolved in dust technology and adds 1 times(Mol ratio)Citric acid be complexed, by ammonium chloride NH4Cl:
0.3566 gram, it is dissolved in appropriate nitric acid, and is diluted with deionized water, three kinds of solution are mixed, is stirred at room temperature 6 hours,
It is put in 60 DEG C and stands 5 hours, be transferred in baking oven 110 DEG C of dryings 11 hours, obtain fluffy presoma, grinding obtains powder,
At 650 DEG C, calcine 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,
As fabric finishing agent.During fabric impregnated in into finishing agent, the consumption of chlorine pucherite is the 5% of dry cloth weight in finishing agent, using two
After soaking the treatment of two roll process, the preliminary drying 5min in 100 DEG C of open width dryers, then 3min is dried in 140 DEG C of open width dryers, obtain
To a kind of fabric with antibacterial and deodouring function.Due to the chlorine pucherite Bi that the present invention is provided9V2O18Cl has spectral response model
Characteristic wide is enclosed, can realize producing photochemical reaction under visible light illumination, microorganism death, organic matter degradation can be made, thus
There is antibacterial, deodorant effect and effect after treatment to fabric.
It is the antibacterial of sample when fabric is washed 50 times after chlorine pucherite finishing agent arranges front and rear and arrangement referring to table 1
Rate result.
Table 1:Anti-bacteria test result
Bacteriostasis rate | Before arrangement | After arrangement | Washed 50 times after arrangement |
Escherichia coli | 11.2% | 99.9% | 99.8% |
Staphylococcus aureus | 8.5% | 99.9% | 99.9% |
From table 1, after the finishing agent provided by the present embodiment is arranged to fabric, with excellent antibacterial effect, washing
Antibacterial effect is not changed in substantially after 50 times.
Claims (9)
1. a kind of chlorine bismuth vanadate photocatalyst, it is characterised in that:Its chemical general formula is Bi9V2O18Cl。
2. a kind of preparation method of chlorine bismuth vanadate photocatalyst as claimed in claim 1, it is characterised in that use solid phase calcination
Method, comprises the following steps:
(1)By chemical formula Bi9V2O18The metering ratio of Cl, weighs containing Bi respectively3+、V5+And Cl-Compound, fully ground in mortar
Mill, is well mixed, and obtains mixture;
(2)Mixture is calcined in air atmosphere, calcining heat is 300~600 DEG C, calcination time is 3~9 hours, natural
Crude product is obtained after cooling;
(3)By crude product grinding, well mixed, the calcining in air atmosphere, calcining heat is 600~900 DEG C, and calcination time is
6~8 hours;A kind of chlorine pucherite catalysis material is obtained after natural cooling.
3. the preparation method of a kind of chlorine bismuth vanadate photocatalyst according to claim 2, it is characterised in that:It is described containing Bi3 +Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·0.5H2One kind in O;It is described containing V5+Compound be
V2O5、NH4VO3In one kind;It is described containing Cl-Compound be NH4One kind in Cl, BiOCl.
4. the preparation method of a kind of chlorine bismuth vanadate photocatalyst according to claim 2, it is characterised in that:Step(2)Institute
The calcining heat stated is 300~500 DEG C, and calcination time is 3~6 hours;Step(3)Described calcining heat is 500~850
DEG C, calcination time is 6~8 hours.
5. a kind of preparation method of chlorine bismuth vanadate photocatalyst as claimed in claim 1, it is characterised in that use wet-chemical side
Method, comprises the following steps:
(1)By chemical formula Bi9V2O18Cl meterings ratio, weighs containing Bi respectively3+、V5+And Cl-Compound;Bi will be contained3+And V5+Change
Compound is dissolved in deionized water or salpeter solution respectively, then by mol, adds 1~3 times of total cation of complexing agent oxalic acid
Or citric acid, obtain containing Bi3+And V5+ Compound solution;
(2)Cl will be contained-Compound be dissolved in nitric acid, diluted with deionized water, then add step(1)Obtain containing Bi3+And V5 + Compound solution, obtain transparent mixed liquor;
(3)By step(2)The transparent mixed solution for obtaining is stirred at room temperature 3~8 hours, then in the bar that temperature is 37~80 DEG C
3~6 hours are stood under part;
(4)By step(3)The mixed liquor for obtaining dried process 10~20 hours under conditions of temperature is for 100~120 DEG C, obtain
Fluffy presoma;
(5)The presoma that will be obtained grinds to form powder, calcines 2~8 hours in air atmosphere, and calcining heat is 500~850
DEG C, room temperature is cooled to, obtain chlorine bismuth vanadate photocatalyst.
6. the preparation method of a kind of chlorine bismuth vanadate photocatalyst according to claim 5, it is characterised in that described contains
Bi3+Compound be Bi2O3、Bi(NO3)3·5H2O、(BiO)2CO3·0.5H2One kind in O;It is described containing V5+Compound
It is V2O5、NH4VO3In one kind;It is described containing Cl-Compound be NH4One kind in Cl, BiOCl.
7. the preparation method of described a kind of chlorine bismuth vanadate photocatalyst according to claim 5, it is characterised in that:Step
(5)Calcining heat be 600~750 DEG C, calcination time be 2~7 hours.
8. a kind of application of chlorine bismuth vanadate photocatalyst as claimed in claim 1, as inorganic catalysis material, for degrading
Organic dyestuff, organic hazardous solvent in waste water.
9. a kind of application of chlorine bismuth vanadate photocatalyst as claimed in claim 1, it is anti-as preparing as fabric finishing agent
Bacterium, deodorization functions textile.
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CN108376742A (en) * | 2018-03-09 | 2018-08-07 | 湖南文理学院 | A kind of preparation method of cerium oxide base solar cell nanometer powder body material and application |
CN109422244A (en) * | 2017-08-21 | 2019-03-05 | 中国科学技术大学 | Can ultraviolet blocking-up photochromic nano material and its preparation method and application |
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CN104998665A (en) * | 2015-07-09 | 2015-10-28 | 三峡大学 | Preparation method and application of BiVO4-BiOBr photocatalyst |
CN105148949A (en) * | 2015-07-30 | 2015-12-16 | 中国石油大学(华东) | Bismuth oxyiodide-bismuth vanadium oxide heterojunction photocatalyst and preparation method thereof |
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CN102489324A (en) * | 2011-11-18 | 2012-06-13 | 陕西科技大学 | F and N co-doped visible-light response bismuth vanadate photocatalyst and preparation method thereof |
CN104998665A (en) * | 2015-07-09 | 2015-10-28 | 三峡大学 | Preparation method and application of BiVO4-BiOBr photocatalyst |
CN105148949A (en) * | 2015-07-30 | 2015-12-16 | 中国石油大学(华东) | Bismuth oxyiodide-bismuth vanadium oxide heterojunction photocatalyst and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109422244A (en) * | 2017-08-21 | 2019-03-05 | 中国科学技术大学 | Can ultraviolet blocking-up photochromic nano material and its preparation method and application |
CN108376742A (en) * | 2018-03-09 | 2018-08-07 | 湖南文理学院 | A kind of preparation method of cerium oxide base solar cell nanometer powder body material and application |
CN108376742B (en) * | 2018-03-09 | 2021-12-07 | 湖南文理学院 | Preparation method and application of cerium oxide-based solar cell nano powder material |
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