CN109529810A - The preparation method of composite bismuth vanadium photocatalyst - Google Patents
The preparation method of composite bismuth vanadium photocatalyst Download PDFInfo
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- CN109529810A CN109529810A CN201910067295.7A CN201910067295A CN109529810A CN 109529810 A CN109529810 A CN 109529810A CN 201910067295 A CN201910067295 A CN 201910067295A CN 109529810 A CN109529810 A CN 109529810A
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- DPSWNBLFKLUQTP-UHFFFAOYSA-N bismuth vanadium Chemical compound [V].[Bi] DPSWNBLFKLUQTP-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 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 abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 230000015556 catabolic process Effects 0.000 abstract description 16
- 238000006731 degradation reaction Methods 0.000 abstract description 16
- 239000002351 wastewater Substances 0.000 abstract description 16
- 238000012545 processing Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 22
- 238000004043 dyeing Methods 0.000 description 20
- 230000001699 photocatalysis Effects 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 12
- 238000007146 photocatalysis Methods 0.000 description 11
- 239000000975 dye Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 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 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- 229910002915 BiVO4 Inorganic materials 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 230000015271 coagulation Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000544061 Cuculus canorus Species 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000002306 biochemical method Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229960002163 hydrogen peroxide Drugs 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000013102 re-test Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004753 textile Substances 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
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 239000000982 direct dye Substances 0.000 description 1
- 239000005446 dissolved organic matter Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- -1 finish Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000985 reactive dye Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of waste water processing using solar energy, more particularly to a kind of preparation method of composite bismuth vanadium photocatalyst, the following steps are included: bismuth nitrate solution is added into ammonium metavanadate solution by A., then pH to 2-12 is adjusted, 60-100 DEG C of hot water and melamine is then added, stirs 1-6h at 90-160 DEG C；B. it cools down, filters, wash to neutrality, then dry, calcination.The light degradation ability of composite bismuth vanadium photocatalyst made from method of the invention is significantly improved.
Description
Technical field
The invention belongs to the technical field of waste water processing using solar energy, and in particular to a kind of composite bismuth vanadium photocatalyst
Preparation method.
Background technique
Since reform and opening-up, China's dyeing is quickly grown, and industry size has ranked among the best in the world.2011,
The national above printing and dyeing enterprise of 1800 scales completes 3383.04 hundred million yuan of total industrial output value, it has also become the weight in Chinese national economy
Want industry " Zhejiang Province's dyeing water pollution control technical system research ", Zhou Guowang etc., printing and dyeing assistant, 2015 volume 32
3 phases, the 1-5 pages, publication date on 03 31st, 2015.
However, the entrainment containing fibrous raw material itself and process make in the waste water discharged due to dyeing
There is biochemistry to need oxygen demand height, coloration height, pH value height, difficult for biological degradation, more for slurry, finish, fuel and chemical assistant etc.
(" status and prospectives of techniques of Dyeing Wastewater Treatment ", week is red etc., Chinese nonmetallic for " three Gao Yinan mono- changes " feature of variation
Miner's industry guide, the 1st phase in 2007, the 60-62 pages, publication date on December 31st, 2007).According to China national Chinese Ministry of Environmental Protection " 2011
Year environmental statistics annual report " data shows that it is total that the waste water total amount of textile printing and dyeing industry discharge occupies national each industrial department discharge of wastewater
The 3rd of amount, whole industry wastewater discharge is about 24.0 hundred million m3/ a, Pollutants in Wastewater total emission volumn (in terms of COD) are located at the 4th
Position.Compared with foreign countries, the water consumption of China's dyeing unit product is about 2 times higher than external, and total amount of pollutants discharged is external product
1.2-1.8 again.Dyeing has become one of China's water pollution industry the most serious, is presently most main water pollution
One of source.Therefore, the comprehensive treatment of dyeing waste water has become problem (" Zhejiang Province's dyeing water in the urgent need to address
Pollutant abatement technology architectural study ", Zhou Guowang etc., printing and dyeing assistant, the 3rd phase of volume 32 in 2015, the 1-5 pages, publication date 2015
31 days 03 month year；" techniques of Dyeing Wastewater Treatment progress ", Liu Meihong, textile journal, the 1st phase of volume 28 in 2007, the
116-119 pages, publication date on 01 31st, 2007).
Currently, the processing common method of dyeing waste water is roughly divided into three classes: (1) based on the absorption of natural mineral matter porous material and
The physical method of membrane separation technique；(2) theoretical based on colloid chemistry, using the chemical method of coagulation means；(3) microorganism is utilized
Metabolism remove waste water in organic matter biological method (" status and prospectives of techniques of Dyeing Wastewater Treatment ",
Week is red etc., Chinese non-metallic mineral industry guide, the 1st phase in 2007, and the 60-62 pages, publication date on December 31st, 2007).Wherein,
Absorption method is most widely used in physical method, is to make one of waste water or more using porous solid matter
Kind substance is attracted to the surface of solids to the method for removal.The active charcoal of industrial common adsorbent, activated silica diatomaceous earth, work
Change coal, natural montmorillonite and cinder etc..Active carbon is only to water such as the dye of positive ion, direct dyes, acid dyes, reactive dye
Soluble dye has preferable absorption property, for going dissolved organic matter in water removal also highly effective, it can however not going to remove water
In colloid hydrophobic dye (" Study on processing method and progress of dyeing waste water ", Weng Liang etc., printing and dyeing assistant, 2005 the 22nd
Roll up o. 11th, the 7-10 pages, publication date on November 30th, 2005).Coagulation Method is one kind of chemical method, has been generally used.
The engineering investment cost of Coagulation Method is low, occupied area is small and treating capacity is big, preferable to the coagulation effect of hydrophobic dye, still,
It needs the condition that feeds intake with change of water quality change, and poor to the decolorizing effect of hydrophilic dye, and COD removal rate is low, in addition, also
Generate a large amount of body refuse, and be dehydrated it is difficult (" discoloration method of dyeing waste water ", Dong Xuqing etc., Guangdong chemical industry, the 2nd phase in 2004,
The 61-66 pages, publication date on December 31st, 2004).Bioanalysis operating cost is low, safe and pollution-free, environmentally friendly.However,
Currently, using fluctuation of service in Biochemical method process of dyeing and printing, applicability is not wide due to technical aspect, by
Being affected of extraneous factor (" research and progress of Biochemical method waste water from dyestuff ", Feng Kai etc., Treatment of Industrial Water, 2009
The 2nd phase of volume 29, the 19-21 pages, publication date on February 28th, 2009).
In recent years, with the development of photocatalysis technology, using sunlight catalytic oxidation processes industrial wastewater, have to save and throw
Money, efficiently, energy conservation, be not present secondary pollution the characteristics of, show good application prospect (" discoloration method of dyeing waste water ",
Dong Xuqing etc., Guangdong chemical industry, the 2nd phase in 2004, the 61-66 pages, publication date on December 31st, 2004), it is purified in air/water body
Cleaning, noxious pollutant improvement etc. receive great attention and study (" iron-based oxide narrow bandgap semiconductor material extensively
Preparation and performance study ", Zhang Tong, Zhejiang University's master thesis, abstract, publication date on December 31st, 2010), and semiconductor
Catalyst can absorb the organic matter that sunlight this green energy resource comes in catalytic degradation waste water, and photocatalysis efficiency is high, safety
It is good, the organic pollutant (" SnO that almost can degrade all2Preparation and its Photocatalytic Performance Study ", XIAN cyanines, Dalian University of Science & Engineering
University's master thesis, 2016, abstract, publication date on November 14th, 2016).Therefore, high efficiency semiconductor catalysis is developed
Agent is the key that one of photocatalysis technology (" preparation of iron-based oxide narrow bandgap semiconductor material and performance study ", Zhang Tong, Zhejiang
Jiang great Xue master thesis, abstract, publication date on December 31st, 2010).
However, traditional catalysis material greater band gap, only there is ultraviolet light photocatalysis activity, and to accounting for solar energy
Visible light energy greater than 40 percent is almost without response, and still, UV energy only accounts for 4% or so of sunlight, because
This, sun light utilization efficiency is lower.In order to preferably utilize the visible light (43% or so) in sunlight, design and exploitation visible light
The catalysis material of response becomes the research hotspot (" SrTiO of Material Field in recent years3Photoelectric material and dye sensitization of solar
The performance study of battery ", Yang Xiaoli, He'nan University's master thesis, 2012, abstract and page 1, publication date 2012 10
The moon 31).
Bi sill, especially contains Bi3+Material (such as Bi2MoO6、Bi2O2CO3、Bi2WO6、BiVO4Deng), because of its tool
There is the advantages that visible light-responded, corrosion-resistant, chemical property stabilization, less toxic, has been widely studied (" containing bismuth composite oxide
Visible light catalytic material progress ", Wang Wen is medium, Journal of Inorganic Materials, the 1st phase of volume 27 in 2012, the 11-19 pages, public
Open on December 2012 day 31；" controlledly synthesis of pucherite and the research of photocatalysis performance ", cuckoo, Shaanxi Tech Univ,
2012 page 1, publication date on 09 03rd, 2012).Wherein, pucherite (BiVO4) be used as one kind without toxic members such as lead, chromium
The Yellow organic dye of element, has many advantages, such as nontoxic, bright color, good corrosion resistance, is concerned for many years.In addition, vanadic acid
The good ferroelectricity of bismuth, ionic conductivity, good photocatalysis hydrogen performance and the characteristic of light degradation organic pollutant can also be expanded
Its technically application (" controlledly synthesis of pucherite and the research of photocatalysis performance ", cuckoo, Shaanxi Tech Univ,
2012 page 1, publication date on 09 03rd, 2012).
However, the forbidden bandwidth of pucherite is 2.3-2.4eV, in practical applications, because of its internal light induced electron and sky
Cave is easy compound, and absorption property is weak, so that limit it can be by photocatalytic activity (" preparation of pucherite composite material, characterization
And the research of photocatalysis performance ", Wang Jianan, Ningxia University's master thesis, 2015, the 4-7 pages, publication date 2015 12
The moon 29).
Currently, the method for commonly improving photo-generate electron-hole utilization efficiency has building Z-type catalyst, with other semiconductors
It is compound, and area load noble metal etc. (" titania-based Z-type photochemical catalyst summary ", Qi Kezhen etc., are catalyzed journal, and 2017 years the
12 phases, the 1936-1955 pages, publication date on December 31st, 2017；" progress of nano titanium dioxide photocatalyst ", Hao Jing
Jade etc., Ti industry progress, the 1st phase of volume 24 in 2007, the 36-41 pages, publication date on February 28th, 2007；" silver-based photocatalysis
The synthesis and application study of agent ", Li Gaiping, university, the Chinese Academy of Sciences, Institute of Chemistry, Academia Sinica's post-doctor's academic dissertation,
2012, page 2, publication date on December 31st, 2012).These methods although can the short time improve its photocatalysis efficiency, however,
If depth extends the light-catalyzed reaction time or recycles, it is easy to appear the unstable problem of semiconductor structure.Therefore, how entirely
Efficiency of light absorption is low, photo-generated carrier separating capacity is weaker, photocatalytic activity is poor, catalyst structure existing for face improvement pucherite
The problems such as stability is still the technical problem of this field urgent need to resolve.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation methods of composite bismuth vanadium photocatalyst.
To achieve the above object, the technical solution of the present invention is as follows:
The preparation method of composite bismuth vanadium photocatalyst, comprising the following steps:
A. bismuth nitrate solution is added into ammonium metavanadate solution, then adjusts pH to 2-12, is then added, 60-100 DEG C
Hot water and melamine stir 1-6h at 90-160 DEG C；
B. it cools down, filters, wash to neutrality, then dry, calcination.
Further, in step A, the bismuth nitrate that contains in the ammonium metavanadate and bismuth nitrate solution that contain in ammonium metavanadate solution
The ratio between the amount of substance be 1:1-1:5.
Further, in step A, the dosage of the melamine is and the substance of the bismuth nitrate contained in bismuth nitrate solution
The ratio between amount is 100:1-1:1.
Further, the temperature of the drying is 60-120 DEG C, time 1-6h.
Further, the temperature of the calcination is 400-600 DEG C, time 1-6h.
Further, the preparation method of the composite bismuth vanadium photocatalyst, comprising the following steps:
A. bismuth nitrate solution is added into ammonium metavanadate solution, then adjusts pH to 2-12, is then added 60-100 DEG C
Hot water and melamine stir 1-6h at 90-160 DEG C, the ammonium metavanadate and bismuth nitrate contained in the ammonium metavanadate solution
The ratio between amount of substance of bismuth nitrate contained in solution is 1:1-1:5, the dosage of the melamine be in bismuth nitrate solution
The ratio between amount of substance of bismuth nitrate contained is 100:1-1:1；
B. it cools down, filters, wash to neutrality, then dry 1-6h at 60-120 DEG C, the calcination 1- at 400-600 DEG C
6h。
The beneficial effects of the present invention are:
The light degradation ability of composite bismuth vanadium photocatalyst made from method of the invention is significantly improved.
The present invention solves the problems, such as that semiconductor structure is unstable in the prior art.
Detailed description of the invention
Fig. 1 is projection Electronic Speculum and high-resolution-ration transmission electric-lens figure, wherein 1a, 1b and 1c are the transmission electron microscope of common pucherite
Electron microscope is projected with high-resolution, Fig. 1 d, 1e and 1f are the transmission electricity of compound composite bismuth vanadium photocatalyst made from embodiment 1-2
Mirror and high-resolution project electron microscope；
Fig. 2 is X-ray diffractogram.
Specific embodiment
Illustrated embodiment is to preferably be illustrated to the contents of the present invention, but is not that the contents of the present invention only limit
In illustrated embodiment.So those skilled in the art carry out nonessential change to embodiment according to foregoing invention content
Into and adjustment, still fall within protection scope of the present invention.
Embodiment 1
The preparation method of composite bismuth vanadium photocatalyst, specific preparation process is as follows:
(1) taking 10mL concentration is the metavanadic acid that the bismuth nitrate solution of 0.05mol/L gently pours into 10mL 0.05mol/L
In ammonium salt solution, pH=4 is adjusted with (1+1) ammonium hydroxide；
(2) 40mL hot water at a temperature of 90 °C is added, adds 1g melamine, dissolves, is maintained at 90 DEG C；
(3) under magnetic agitation, 90 DEG C of water-bath 3h；
(4) it is cooled to room temperature, filters, with deionized water washing 3-4 times, until pH=7；
(5) precipitating by washing to pH=7 is placed in baking oven in 80 DEG C of drying and processing 1h；
(6) be transferred in crucible after grinding sample, in Muffle furnace at 550 DEG C calcination 2h.
Embodiment 2
The preparation method of composite bismuth vanadium photocatalyst, specific preparation process is as follows:
(1) taking 5mL concentration is the ammonium metavanadate that the bismuth nitrate solution of 0.05mol/L gently pours into 5mL 0.05mol/L
In solution, pH=4 is adjusted with (1+1) ammonium hydroxide；
(2) 20mL hot water at a temperature of 90 °C is added, adds 1g melamine, dissolves；
(3) it is transferred in reaction kettle, under magnetic agitation, 160 DEG C of oil bath 3h；
(4) it is cooled to room temperature, filters, with deionized water washing 3-4 times, until pH=7；
(5) precipitating by washing to pH=7 is placed in baking oven in 80 DEG C of drying and processing 1h；
(6) be transferred in crucible after grinding sample, in Muffle furnace at 550 DEG C calcination 2h.
Performance detection
To composite bismuth vanadium photocatalyst made from embodiment 1-2 and common BiVO4Photocatalytic degradation effect experiment is carried out,
Specific step is as follows:
1, using colored dyes rhodamine B as target degradation product
It disperses 20mg photochemical catalyst in the rhodamine B solution that 200mL concentration is 10mg/L, 1mL concentration, which is added, is
After 30% hydrogenperoxide steam generator, dark reaction 60min is stirred continuously during dark reaction.Then light is carried out at normal temperatures and pressures
Catalysis reaction, light source choose 300W xenon lamp (λ >=420nm), and the absorbance every 10min sampling analysis, rhodamine B solution is purple
Outer visible spectrophotometer is tested at wavelength 554nm.The degradation rate for calculating photochemical catalyst, according to formula degradation rate=
[1- (initial concentration-endpoint concentration)/initial concentration] × 100% calculates the degradation rate of photochemical catalyst, and 60min degradation results are such as
Shown in table 1.
2, using no methylene blue as target degradation product
It disperses 10mg photochemical catalyst in the rhodamine B solution that 100mL concentration is 10mg/L, 0.5mL concentration, which is added, is
After 30% hydrogenperoxide steam generator, dark reaction 60min is stirred continuously during dark reaction.Then light is carried out at normal temperatures and pressures
Catalysis reaction, light source choose 300W xenon lamp (λ >=420nm), and the absorbance every 10min sampling analysis, methylene blue solution is used
Ultraviolet-uisible spectrophotometer is tested at wavelength 664nm.The degradation rate for calculating photochemical catalyst, according to formula degradation rate
=[1- (initial concentration-endpoint concentration)/initial concentration] × 100% calculates the degradation rate of photochemical catalyst, 60min degradation results
As shown in table 1.
1 the performance test results of table
As shown in Table 1, with common BiVO4It compares, composite bismuth vanadium photocatalyst made from embodiment 1-2 is to rhodamine B
The degradation rate of rhodamine B and methylene blue solution Methylene Blue is significantly improved in solution.Thus it proves, it is of the invention
The light degradation ability of composite bismuth vanadium photocatalyst made from method is significantly improved.
Meanwhile transmission electron microscope, height are carried out to the common pucherite of pucherite composite catalyst or more made from embodiment 1-2
Resolved transmittance electron-microscope scanning and X-ray diffraction, as a result as shown in Figs. 1-2；Wherein, Fig. 1 is that transmission electron microscope (TEM) and high-resolution are saturating
Radio mirror (HRTEM) figure, 1a, 1b and 1c are that the transmission electron microscope of common pucherite and high-resolution project electron microscope, Fig. 1 d, 1e and 1f
Electron microscope is projected for the transmission electron microscope of compound composite bismuth vanadium photocatalyst made from embodiment 1-2 and high-resolution；Fig. 2 penetrates for X
Line diffraction (XRD) figure.
As shown in Figure 1, (110) crystal face of composite bismuth vanadium photocatalyst made from embodiment 1-2 and (040 crystal face) are formed
Homojunction.
Repetitive test
Repeated experiment is carried out to rhodamine B photocatalytic degradation effect to composite photocatalyst material made from embodiment 1-2,
Test method is same as above, and three times, test result is as shown in table 2 for photochemical catalyst retest made from each embodiment.
The repeated the performance test results of table 2 (to the degradation rate of rhodamine B)
| Sample | For the first time | Second | For the third time |
| Embodiment 1 | 87% | 86% | 90% |
| Embodiment 2 | 87% | 83% | 85% |
As shown in Table 2, the photocatalysis effect of composite photo-catalyst retest three times made from embodiment 1-2 is without under obvious
Drop.Thus it proves, the performance of composite bismuth vanadium photocatalyst made from method of the invention is stablized, and the present invention solves existing skill
The unstable problem of semiconductor structure in art.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (6)
1. the preparation method of composite bismuth vanadium photocatalyst, which comprises the following steps:
A. bismuth nitrate solution is added into ammonium metavanadate solution, then adjusts pH to 2-12,60-100 DEG C of hot water is then added
And melamine, 1-6h is stirred at 90-160 DEG C；
B. it cools down, filters, washing to solution is neutrality, is then dried, calcination.
2. the preparation method of composite bismuth vanadium photocatalyst according to claim 1, which is characterized in that in step A, inclined vanadium
The ratio between amount of substance of bismuth nitrate contained in the ammonium metavanadate and bismuth nitrate solution contained in acid ammonium solution is 1:1-1:5.
3. the preparation method of composite bismuth vanadium photocatalyst according to claim 1 or 2, which is characterized in that in step A,
It is 1/126:0.0005 that the dosage of the melamine, which is with the ratio between the amount of substance of bismuth nitrate contained in bismuth nitrate solution,.
4. the preparation method of composite bismuth vanadium photocatalyst according to claim 1,2 or 3, which is characterized in that the baking
Dry temperature is 60-120 DEG C, time 1-6h.
5. the preparation method of composite bismuth vanadium photocatalyst according to claim 1,2,3 or 4, which is characterized in that described
The temperature of calcination is 400-600 DEG C, time 1-6h.
6. the according to claim 1, preparation method of composite bismuth vanadium photocatalyst described in 2,3,4 or 5, which is characterized in that
The following steps are included:
A. bismuth nitrate solution is added into ammonium metavanadate solution, then adjusts pH to 2-12,60-100 DEG C of hot water is then added
And melamine, 1-6h is stirred at 90-160 DEG C, the ammonium metavanadate and bismuth nitrate solution contained in the ammonium metavanadate solution
In the ratio between the amount of substance of bismuth nitrate that contains be 1:1-1:5, the dosage of the melamine is and contains in bismuth nitrate solution
The ratio between the amount of substance of bismuth nitrate be 100:1-1:1；
B. it cools down, filters, wash to neutrality, then dry 1-6h at 60-120 DEG C, the calcination 2h at 400-600 DEG C.
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