CN107597101A - Simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2The preparation method of nanometer sheet - Google Patents

Simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2The preparation method of nanometer sheet Download PDF

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Publication number
CN107597101A
CN107597101A CN201711058915.8A CN201711058915A CN107597101A CN 107597101 A CN107597101 A CN 107597101A CN 201711058915 A CN201711058915 A CN 201711058915A CN 107597101 A CN107597101 A CN 107597101A
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sno
nanometer sheet
suspension
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hours
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Inventor
邹学军
于鸣
于一鸣
李思佳
苑承禹
董玉瑛
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Dalian Minzu University
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Dalian Nationalities University
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Priority to CN201711358232.4A priority patent/CN108043390A/en
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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
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts 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
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/31Chromium, molybdenum or tungsten combined with bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • B01J35/39
    • B01J35/40
    • B01J35/61
    • 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
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • 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
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts
    • 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
    • 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
    • C02F2101/345Phenols

Abstract

Simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2The preparation method of nanometer sheet, by using the Bi of hydro-thermal method synthesis2WO6Add in ethylene glycol, stirring to obtain Bi2WO6Suspension.To Bi2WO6SnCl is added in suspension4·5H2O obtains mixing suspension.Urea is added into deionized water simultaneously, the solution obtained is rapidly added mixing suspension, and is stirred at room temperature.Then, mixed solution is transferred to heating response in reactor, the Bi finally obtained2WO6/SnO2Nanometer sheet.Bi prepared by the present invention2WO6/SnO2Nanometer sheet specific surface area is big, and adsorption capacity is strong;With more preferable visible absorption performance, photocatalytic oxidation degradation organic pollution is improved a lot;And Bi of the present invention2WO6/SnO2The preparation method of nanometer sheet is fairly simple, easily operated.

Description

Simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2Nanometer The preparation method of piece
Technical field
The present invention relates to a kind of semiconductor light-catalyst and preparation method for curbing environmental pollution.
Background technology
Energy crisis and environmental problem have been two Tough questions that the mankind have to face, and how effectively to control and control It is the emphasis in comprehensive environmental improvement to manage pollution of the various chemical pollutants to environment.In recent years, as high-level oxidation technology it One Photocatalytic Oxidation With Semiconductors technology, just by the widely studied of domestic and foreign scholars, this technology can using solar energy as The energy effectively utilizes solar energy, reduces the energy resource consumption of people come the pollutant in environment of degrading.
Photocatalytic Oxidation With Semiconductors technology starts from the TiO that Japanese Scientists Fujishima and Honda have found light irradiation2 Single Crystalline Electrodes can be by H2O is decomposed, and utilizes TiO2Semiconductor light-catalyst convert light energy into electric energy and chemical energy just turn into partly lead The study hotspot of body photocatalysis field.However, Detitanium-ore-type TiO2Energy gap be 3.2eV, its excitation wavelength is 387.5nm, the ultraviolet light range belonged in sunshine.And for solar energy, what its main energetic concentrated on 400~600nm can See optical range, this considerably reduce TiO2The efficiency of semiconductor light-catalyst, therefore, develop to visible light-responded new Semi-conducting material is one of key content of Study on photocatalyst.
At present, in numerous semiconductor light-catalysts newly developed, researcher develops tungstate compound, and finding should Class catalyst has less energy gap, can sufficiently utilize sunshine, is a kind of promising photochemical catalyst.But with Research is goed deep into, and it is poor that researcher has found that stability occurs in most tungstate compound, the defects of easy photoetch, limits it Development.
The content of the invention
To make up the deficiencies in the prior art, the present invention provide it is a kind of not only have it is visible light-responded, to organic pollution With degradation capability and stability is good, uncorruptible photochemical catalyst Bi2WO6/SnO2Nanometer sheet and preparation method.
The present invention is achieved in that hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2Nanometer sheet Preparation method, comprise the following steps:
S1. pure Bi2WO6With mixing Bi2WO6Sample is synthesized using hydro-thermal method.
By 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirs 30min, Obtained flaxen suspension.Suspension is transferred to 90 DEG C of -220 DEG C of reaction 12-36 hours in 100mL autoclaves, After reaction terminates, natural cooling, filtering, washing, dried 24 hours in 60 DEG C, obtain the pure Bi of product2WO6
S2.Bi2WO6/SnO2The synthesis of nanometer sheet:
Bi is added into ethylene glycol2WO6, stirring to obtain Bi2WO6Suspension;By Bi2WO6Suspension is added to SnCl4· 5H2Mixing suspension is prepared in O, aqueous solution of urea is prepared, aqueous solution of urea is rapidly added in mixing suspension, and in room temperature Lower stirring 1 hour, is then transferred into reactor 150-210 DEG C of 12-24 hour of heating, scrubbed, 80 DEG C of dryings 24 hours;Most Bi is made afterwards2WO6/SnO2Nanometer sheet, wherein Bi2WO6Account for SnO2The 24.47%-88.13% of quality.
The present invention has visible light-responded photochemical catalyst Bi by one pot process2WO6/SnO2Nanometer sheet, pass through simultaneously Reaction time and reaction temperature are controlled, forms the spherical morphology of bigger serface so that the material of preparation has larger ratio Surface area, be advantageous to the absorption degradation of pollutant.
Another object of the present invention is that the Bi prepared using the inventive method is claimed2WO6/SnO2Nanometer sheet catalysis drop The method for solving liguid phase pollutant, is comprised the following steps that:Weigh 100mgBi2WO6/SnO2Nanometer sheet, add 5mg/L 100mL phenol In solution, the magnetic agitation 30min under dark situation, it is then placed under xenon lamp and irradiates while stirring, carries out catalytic reaction.
The present invention by reasonably regulating and controlling Bi2WO6And SnO2Proportioning, technological parameter is adjusted, nanometer sheet is anti-through solvent heat It is flake nano level compound Bi that microstructure, which should be obtained,2WO6/SnO2.Compared with prior art, the present invention has advantages below:
1st, Bi prepared by the present invention2WO6/SnO2The specific surface area of nanometer sheet is big, and adsorption capacity is strong;
2nd, Bi prepared by the present invention2WO6/SnO2Nanometer sheet has and preferably may be used compared with traditional photochemical catalyst titanium dioxide See absorbing properties, photocatalytic oxidation degradation organic pollution is improved a lot;
3rd, Bi provided by the invention2WO6/SnO2The preparation method of nanometer sheet is fairly simple, easily operated, raw suitable for industry Production.
Brief description of the drawings
Fig. 1 is the Bi in embodiment 12WO6/SnO2The scanning electron microscope (SEM) photograph that 8000 times of nanometer sheet multiplication factor.
Fig. 2 is the Bi in embodiment 1 and embodiment 22WO6/SnO2Nanometer sheet XRD diffracting spectrums.
Fig. 3 is the Bi in embodiment 12WO6/SnO2Nanometer sheet UR-Vis DRS spectrum analysis figures.
Fig. 4 is the Bi of the different content in embodiment 12WO6/SnO2Heterojunction structure light degradation datagram.
Embodiment
The present invention is described in detail below by the drawings and specific embodiments, but not limited the scope of the invention.Such as without special Illustrate, experimental method of the present invention is conventional method, and experiment equipment used, material, reagent etc. can be chemically public Department's purchase.It is related to photocatalysis TiO in application examples2, model P25, buy and create industrial group in win.
Embodiment 1
(1) by 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirring 30min, obtained flaxen suspension, suspension is transferred in 100mL stainless steel autoclaves and is maintained at 180 DEG C 24 Hour.After natural cooling, product filtering, washed repeatedly with deionized water and ethanol, then dried at 60 DEG C and be made within 24 hours pure Bi2WO6
(2) 0.7g Bi are added in 50mL ethylene glycol2WO6, stir 3 hours and obtain Bi2WO6Suspension.To Bi2WO6Suspension Middle addition 0.7g SnCl4·5H2O obtains mixing suspension.0.4g urea is added into 30mL deionized waters, it is water-soluble to obtain urea Liquid.Aqueous solution of urea is rapidly added in mixing suspension, is stirred at room temperature 1 hour, is then transferred into polytetrafluoroethylene (PTFE) Lined steel reactor, heated 16 hours in 180 DEG C, collect, repeatedly washed with deionized water, dried in 80 DEG C 24 hours, finally obtain To 72.12wt%-Bi2WO6/SnO2Nanometer sheet.
Embodiment 2
(1) by 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirring 30min, obtained flaxen suspension, suspension is transferred in 100mL stainless steel autoclaves and is maintained at 90 DEG C 36 Hour.After natural cooling, product filtering, washed repeatedly with deionized water and ethanol, then dried at 60 DEG C and be made within 24 hours pure Bi2WO6
(2) 0.7g Bi are added in 50mL ethylene glycol2WO6, stir 3 hours and obtain Bi2WO6Suspension.To Bi2WO6Suspension Middle addition 0.86g SnCl4·5H2O obtains mixing suspension.Meanwhile 0.4g urea is added in 30mL deionized waters, obtain urea The aqueous solution.Aqueous solution of urea is rapidly added in mixing suspension, is stirred at room temperature 1 hour, is then transferred into polytetrafluoroethyl-ne Alkene inner lining steel reactor, heated 24 hours in 150 DEG C, collect and deionized water is repeatedly washed, it is dry 24 hours in 80 DEG C, finally Obtain 88.13wt%-Bi2WO6/SnO2Nanometer sheet.
Embodiment 3
(1) by 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirring 30min, obtained flaxen suspension, suspension is transferred in 100mL stainless steel autoclaves and is maintained at 220 DEG C 12 Hour.After natural cooling, product filtering, washed repeatedly with deionized water and ethanol, then dried at 60 DEG C and be made within 24 hours pure Bi2WO6
(2) 0.7g Bi are added in 50mL ethylene glycol2WO6, stir 3 hours and obtain Bi2WO6Suspension.To Bi2WO6Suspension Middle addition 0.86g SnCl4·5H2O obtains mixing suspension.Meanwhile 0.4g urea is added in 30mL deionized waters, obtain urea The aqueous solution.Aqueous solution of urea is rapidly added in mixing suspension, is stirred at room temperature 1 hour, is then transferred into polytetrafluoroethyl-ne Alkene inner lining steel reactor, heated 24 hours in 150 DEG C, collect and deionized water is repeatedly washed, it is dry 24 hours in 80 DEG C, finally Obtain 88.13wt%-Bi2WO6/SnO2Nanometer sheet.
Embodiment 4
(1) by 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirring 30min, obtained flaxen suspension, suspension is transferred in 100mL stainless steel autoclaves and is maintained at 90 DEG C 36 Hour.After natural cooling, product filtering, washed repeatedly with deionized water and ethanol, then dried at 60 DEG C and be made within 24 hours pure Bi2WO6
(2) 0.7g Bi are added in 50mL ethylene glycol2WO6, stir 3 hours and obtain Bi2WO6Suspension.To Bi2WO6Suspension Middle addition 0.23g SnCl4·5H2O obtains mixing suspension.Meanwhile 0.4g urea is added in 30mL deionized waters, obtain urea The aqueous solution.Aqueous solution of urea is rapidly added in mixing suspension, is stirred at room temperature 1 hour, is then transferred into polytetrafluoroethyl-ne Alkene inner lining steel reactor, heated 24 hours in 150 DEG C, collect and deionized water is repeatedly washed, it is dry 24 hours in 80 DEG C, finally Obtain 24.47wt%-Bi2WO6/SnO2Nanometer sheet.
Application examples 1
Buy business photocatalysis TiO2, without any processing, it is directly used in light-catalyzed reaction as a comparison.
Bi is prepared by the method in embodiment 12WO6/SnO2Nanometer sheet, take the pure Bi of 100mg2WO6, add 5mg/L 100mL In phenol solution, the magnetic agitation 30min under dark situation, it is put under xenon lamp and irradiates while stirring afterwards, is taken once per 15min Sample, the sample of taking-up centrifuges 20min under 2000r/min, then takes out supernatant with liquid-transfering gun, then goes out to survey it in 510nm Absorbance, and record data.
Experimental result is as shown in figure 4, under visible light conditions, pure Bi2WO6Pyrogentisinic Acid has when nanometer sheet is as catalyst In general catalytic oxidation activity.
Application examples 2
Buy business photocatalysis TiO2, without any processing, it is directly used in light-catalyzed reaction as a comparison.
72.12%Bi is prepared by the method in embodiment 12WO6/SnO2Nanometer sheet, take 100mg72.12%Bi2WO6/SnO2 Nanometer sheet, add in 5mg/L 100mL phenol solutions, the magnetic agitation 30min under dark situation, be put into xenon lamp afterwards and stir below Side irradiation is mixed, takes a sample per 15min, the sample of taking-up centrifuges 20min under 2000r/min, then is taken out with liquid-transfering gun Clear liquid, then go out in 510nm and survey its absorbance, and record data.
Experimental result is as shown in figure 4, under visible light conditions, 72.12%Bi2WO6/SnO2When nanometer sheet is as catalyst, Under visible light conditions, there is stronger catalytic oxidation activity to liguid phase pollutant.
It is described above, the only preferable embodiment of the invention, but the protection domain of the invention is not This is confined to, any one skilled in the art is in the technical scope that the invention discloses, according to the present invention The technical scheme of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection domain it It is interior.

Claims (4)

1. simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2The preparation method of nanometer sheet, its feature It is, comprises the following steps:
Bi is added into ethylene glycol2WO6, stirring to obtain Bi2WO6Suspension;By Bi2WO6Suspension is added to SnCl4·5H2In O Mixing suspension is prepared, aqueous solution of urea is prepared, aqueous solution of urea is rapidly added in mixing suspension, and is stirred at room temperature 1 hour, it is then transferred into reactor 150-210 DEG C of 12-24 hour of heating, scrubbed, 80 DEG C of dryings 24 hours;Finally it is made Bi2WO6/SnO2Nanometer sheet, wherein Bi2WO6Account for SnO2The 24.47%-88.13% of quality.
2. according to the method for claim 1, it is characterised in that Bi2WO6Preparation method be specially:By 1mmol Na2WO4·2H2O, 1.98mmol Bi (NO3)3·5H2O is dissolved in 100mL distilled water, stirs 30min, obtains suspension, will suspend Liquid is transferred to 90 DEG C of -220 DEG C of reaction 12-36 hours in 100mL autoclaves, after reaction terminates, natural cooling, filters, washes Wash, dried 24 hours in 60 DEG C, obtain Bi2WO6
3. nanometer sheet Bi as claimed in claim 12WO6/SnO2The method of catalytic degradation liguid phase pollutant, it is characterised in that tool Body step is as follows:Take 100mg samples Bi2WO6/SnO2, add in 5mg/L 100mL liguid phase pollutants, magnetic force stirs under dark situation 30min is mixed, is then placed under xenon lamp and irradiates while stirring, carries out catalytic reaction.
4. according to the method for claim 3, it is characterised in that the liguid phase pollutant is phenol.
CN201711058915.8A 2017-11-01 2017-11-01 Simple hydro-thermal method synthesis has visible light-responded photochemical catalyst Bi2WO6/SnO2The preparation method of nanometer sheet Pending CN107597101A (en)

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CN109772295A (en) * 2019-03-11 2019-05-21 中南大学 A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application
CN114392733A (en) * 2021-11-30 2022-04-26 盐城工学院 Method for preparing bismuth oxide composite material with photocatalytic performance

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CN109772295A (en) * 2019-03-11 2019-05-21 中南大学 A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application
CN114392733A (en) * 2021-11-30 2022-04-26 盐城工学院 Method for preparing bismuth oxide composite material with photocatalytic performance

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Application publication date: 20180119