CN107008463A - A kind of silver metavanadate is combined the preparation method of silver bromide photochemical catalyst - Google Patents

A kind of silver metavanadate is combined the preparation method of silver bromide photochemical catalyst Download PDF

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Publication number
CN107008463A
CN107008463A CN201710201076.4A CN201710201076A CN107008463A CN 107008463 A CN107008463 A CN 107008463A CN 201710201076 A CN201710201076 A CN 201710201076A CN 107008463 A CN107008463 A CN 107008463A
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Prior art keywords
silver
metavanadate
colloid
solution
combined
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侯仔尧
赵文昌
冯婷
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Changzhou University
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Changzhou University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06Halogens; Compounds thereof
    • B01J27/08Halides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/0201Impregnation
    • B01J37/0211Impregnation using a colloidal suspension
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)

Abstract

The present invention discloses the preparation method that a kind of silver metavanadate is combined silver bromide photochemical catalyst, comprises the following steps that:12~16mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, 6.6~8mmol ammonium metavanadates are weighed, in 40~60 DEG C of water, 10mmol/L sodium metavanadate solution are configured to;Both the above solution is mixed under 350~400 revs/min of rotating speed, colloid substance is formed, 3~4h is persistently stirred, ammonium metavanadate and nitric acid silver reaction in whipping process generate silver metavanadate colloid;Silver metavanadate colloid is placed in pellicle bag, with distillation water washing 3~4 times, get rid of dissociated ion, the silver metavanadate colloid is added in the sodium bromide solution that 60~80mL concentration is 3~4mol/L again, soaked 2~4 days, in silver metavanadate particle surface formation bromination silver nano-grain, separation of solid and liquid, deionized water washing solid 2~3 times, 75~105 DEG C of drying are made a kind of silver metavanadate and are combined silver bromide photochemical catalyst.This method is that catalyst and carrier are combined closely in carrier surface formation catalyst.

Description

A kind of silver metavanadate is combined the preparation method of silver bromide photochemical catalyst
Technical field
The present invention relates to the preparation method that a kind of silver metavanadate is combined silver bromide photochemical catalyst, belong to sewage in environmental protection Processing technology field.
Background technology
Traditional method for treating water efficiency is low, cost is high, there are secondary pollution problems, and waste water control always cannot be well Solution.The development and application of nanometer technology are likely to thoroughly solve this problem.Start within 1972 to find TiO2Oxidation activity Higher, chemical stability is good, harmless to the human body, and cost is low, pollution-free, has a wide range of application, thus is most paid attention to, but TiO2 Larger (such as anatase TiO of energy gap2Energy gap Eg=3.2eV), be only capable of absorb ultraviolet region (wavelength is less than Light 387nm), the utilization ratio to solar energy is relatively low.
In contaminant degradation and production of energy field, conductor photocatalysis is one of most promising method.Work as energy Amount will produce point of electron-hole pair when being more than or equal to the photon irradiation of semiconductor energy gap in photocatalyst surface From this is the initial basic step of light-catalyzed reaction.In order to find efficient photochemical catalyst, numerous studies work is all concentrated on In the influence factor for studying photocatalytic activity.Because silver had not only had catalytic activity Yuan but also lewis acidic property can be shown, Meanwhile, silver is compared with other metals, such as gold, platinum, and price is more cheap, therefore with stronger industrial applicability.But inclined vanadium Sour silver is due to the limitation of itself characteristic, and in terms of photocatalytic degradation, performance need to be improved.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to propose that a kind of silver metavanadate is combined silver bromide photochemical catalyst Preparation method, this method be carrier surface formation catalyst, catalyst and carrier are combined closely.
The technical solution adopted by the present invention is to use following steps:
1) 12~16mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, the inclined vanadium of 6.6~8mmol is weighed Sour ammonium, in 40~60 DEG C of water, is configured to 10mmol/L sodium metavanadate solution;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3 ~4h, ammonium metavanadate and nitric acid silver reaction in whipping process generate silver metavanadate colloid;
3) silver metavanadate colloid is placed in pellicle bag, with water washing is distilled 3~4 times, gets rid of dissociated ion, then will The silver metavanadate colloid is added in the sodium bromide solution that 60~80mL concentration is 3~4mol/L, is soaked 2~4 days, in metavanadic acid Argent grain surface forms bromination silver nano-grain, separation of solid and liquid, deionized water washing solid 2~3 times, 75~105 DEG C of drying, system Obtain a kind of silver metavanadate and be combined silver bromide photochemical catalyst.
The beneficial effects of the invention are as follows:(1) this method utilizes the difference of solubility product constant, forms molten on silver metavanadate surface The smaller silver bromide grain of degree product constant.
(2) silver metavanadate and silver bromide are compound, synergy, and silver metavanadate can be made preferably to play under visible light and urged Change acts on and can obtain good catalytic effect.
Embodiment
Embodiment 1
16mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, 8mmol ammonium metavanadates are weighed, at 60 DEG C In water, 10mmol/L sodium metavanadate solution is configured to;Both the above solution is mixed under 400 revs/min of rotating speed, formed Colloid substance, persistently stirs 4h, ammonium metavanadate and nitric acid silver reaction in whipping process, generates silver metavanadate colloid;By inclined vanadium Sour silver colloid is placed in pellicle bag, with water washing is distilled 4 times, gets rid of dissociated ion, then the silver metavanadate colloid is added To 80mL concentration in 3mol/L sodium bromide solution, to soak 4 days, in silver metavanadate particle surface formation bromination silver nanoparticle Grain, separation of solid and liquid, deionized water washing solid 3 times, 105 DEG C of drying are made a kind of silver metavanadate and are combined silver bromide photochemical catalyst.
Obtained silver metavanadate is combined silver bromide photochemical catalyst 0.3g and is added to the acid orange that 300mL concentration is 40mg/L In II waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 96.8%, profit can be repeated after catalyst separation With.
Embodiment 2
12mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, 6.6mmol ammonium metavanadates are weighed, 40 In DEG C water, 10mmol/L sodium metavanadate solution is configured to;Both the above solution is mixed under 350 revs/min of rotating speed, shape Agglutination material, persistently stirs 3h, ammonium metavanadate and nitric acid silver reaction in whipping process, generates silver metavanadate colloid;Will be inclined Vanadic acid silver colloid is placed in pellicle bag, with water washing is distilled 3 times, gets rid of dissociated ion, then the silver metavanadate colloid is added Enter to 60mL concentration in 4mol/L sodium bromide solution, to soak 2 days, in silver metavanadate particle surface formation bromination silver nanoparticle Grain, separation of solid and liquid, deionized water washing solid 2 times, 75 DEG C of drying are made a kind of silver metavanadate and are combined silver bromide photochemical catalyst.
Obtained silver metavanadate is combined silver bromide photochemical catalyst 0.3g and is added to the rhodamine that 300mL concentration is 40mg/L In B waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 97.2%, can be reused after catalyst separation. For identical waste water under the same conditions, the degradation efficiency of pure silver metavanadate is 55.7%, substantially increases its effect Effect.
Embodiment 3
14mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, 7mmol ammonium metavanadates are weighed, at 60 DEG C In water, 10mmol/L sodium metavanadate solution is configured to;Both the above solution is mixed under 400 revs/min of rotating speed, formed Colloid substance, persistently stirs 4h, ammonium metavanadate and nitric acid silver reaction in whipping process, generates silver metavanadate colloid;By inclined vanadium Sour silver colloid is placed in pellicle bag, with water washing is distilled 4 times, gets rid of dissociated ion, then the silver metavanadate colloid is added To 80mL concentration in 4mol/L sodium bromide solution, to soak 4 days, in silver metavanadate particle surface formation bromination silver nanoparticle Grain, separation of solid and liquid, deionized water washing solid 3 times, 105 DEG C of drying are made a kind of silver metavanadate and are combined silver bromide photochemical catalyst.
Obtained silver metavanadate is combined silver bromide photochemical catalyst 0.3g and is added to the rhodamine that 300mL concentration is 40mg/L In B waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 98.1%, can be reused after catalyst separation.

Claims (1)

1. a kind of silver metavanadate is combined the preparation method of silver bromide photochemical catalyst, it is characterized in that in turn including the following steps:
1) 12~16mmol silver nitrates are weighed, 12mmol/L silver nitrate solution is configured to, 6.6~8mmol ammonium metavanadates are weighed, In 40~60 DEG C of water, 10mmol/L sodium metavanadate solution is configured to;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3~4h, Ammonium metavanadate and nitric acid silver reaction in whipping process, generate silver metavanadate colloid;
3) silver metavanadate colloid is placed in pellicle bag, with water washing is distilled 3~4 times, gets rid of dissociated ion, then this is inclined Vanadic acid silver colloid is added in the sodium bromide solution that 60~80mL concentration is 3~4mol/L, is soaked 2~4 days, in silver metavanadate Grain surface forms bromination silver nano-grain, and separation of solid and liquid, deionized water washing solid 2~3 times, 75~105 DEG C of drying are made one Plant silver metavanadate and be combined silver bromide photochemical catalyst.
CN201710201076.4A 2017-03-30 2017-03-30 A kind of silver metavanadate is combined the preparation method of silver bromide photochemical catalyst Pending CN107008463A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101279276A (en) * 2008-05-26 2008-10-08 山东大学 Tungstenic acid/silver bromide visible light photocatalyst and preparation thereof
CN103846096A (en) * 2014-03-28 2014-06-11 安徽师范大学 Silver/silver bromide/silver metavanadate plasma compound photocatalyst and preparation method thereof
WO2014122574A2 (en) * 2013-02-11 2014-08-14 Conceria Stefania S.P.A. Process of activation of metal silver
CN103990481A (en) * 2014-06-04 2014-08-20 常州大学 Preparation method of metavanadic silver/silver/silver phosphate composite catalyst
KR20160118414A (en) * 2015-04-01 2016-10-12 부경대학교 산학협력단 A Heterogeneous Nano Particle Manufacturing method Using the Block Copolymer Micelles and A Catalyst Manufactured by thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101279276A (en) * 2008-05-26 2008-10-08 山东大学 Tungstenic acid/silver bromide visible light photocatalyst and preparation thereof
WO2014122574A2 (en) * 2013-02-11 2014-08-14 Conceria Stefania S.P.A. Process of activation of metal silver
CN103846096A (en) * 2014-03-28 2014-06-11 安徽师范大学 Silver/silver bromide/silver metavanadate plasma compound photocatalyst and preparation method thereof
CN103990481A (en) * 2014-06-04 2014-08-20 常州大学 Preparation method of metavanadic silver/silver/silver phosphate composite catalyst
KR20160118414A (en) * 2015-04-01 2016-10-12 부경대학교 산학협력단 A Heterogeneous Nano Particle Manufacturing method Using the Block Copolymer Micelles and A Catalyst Manufactured by thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HUIDAN LU ET AL.,: ""In-situ anion-exchange synthesis AgCl/AgVO3 hybrid nanoribbons with highly photocatalytic activity"", 《MATERIALS LETTERS》 *

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