CN101745402A - Bi2WO6 photocatalysis membrane loaded by base with high specific surface, method and application thereof - Google Patents

Bi2WO6 photocatalysis membrane loaded by base with high specific surface, method and application thereof Download PDF

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CN101745402A
CN101745402A CN200910197580A CN200910197580A CN101745402A CN 101745402 A CN101745402 A CN 101745402A CN 200910197580 A CN200910197580 A CN 200910197580A CN 200910197580 A CN200910197580 A CN 200910197580A CN 101745402 A CN101745402 A CN 101745402A
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photocatalysis
ratio surface
photocatalysis membrana
surface base
base load
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CN101745402B (en
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王文中
徐婕慧
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention relates to a Bi2WO6 photocatalysis membrane loaded by a base with a high specific surface, a method and application thereof. The preparation method comprises the following steps: firstly, Bi2WO6 nano-powder is prepared at the temperature of 60-300 DEG C, the clean base with the high specific surface is dipped into Bi2WO6 suspension to prepare a Bi2WO6 membrane, and finally the Bi2WO6 photocatalysis membrane loaded by the base with the high specific surface is prepared by heat treatment at the temperature of 100-950 DEG C. The bases with the high specific surface are a metal net, foam metal or porous ceramics; and the prepared Bi2WO6 membrane has the characteristics of small Bi2WO6 particle size, high photocatalysis activity, favourable cycle performance, simple preparation technology, low production cost and the like. Meanwhile, the photocatalysis membrane can be conveniently recycled and reused, thus solving the problem of difficult recovery in the practical application of a nanometer photochemical catalyst. The invention can be used for RhB degradation, air purification and photocatalysis antibacterial activity under visible light.

Description

High-ratio surface base load Bi 2WO 6Photocatalysis membrana, method and application
Technical field
The present invention relates to photocatalysis membrana and application, particularly Bi 2WO 6Photocatalysis membrana, preparation method, and it realizes the application of the depollution of environment under radiation of visible light.
Background technology
Industrial development has brought the variation of making rapid progress not only for human life, and also the environment of depending on for existence to the mankind has caused huge threat and harm.The oil crisis of early 1970s has not only been brought developing rapidly of Optical Electro-Chemistry, and has caused the extensive concern of people to photocatalysis field.Photocatalysis has characteristics such as reaction condition gentleness, oxidisability are strong, clean environment firendly, photocatalysis in recent years and correlation technique thereof all show goodish application potential in the conversion of environmental improvement, solar energy, all many-sides such as antibiotic, obtain development fast, especially obtained broad research aspect sewage disposal and the solar energy conversion.
At present, at the most widely used general TiO that is of photocatalysis field 2Based photocatalyst.Yet, TiO 2Band gap wide (3.2eV), excited less than 4% ultraviolet light (wavelength is less than 387nm) by gross energy in the sunshine only, account for about 43% and the sunshine medium wavelength is the visible light of 400～750nm.In order more effectively to utilize the regenerative resource sunshine to carry out environmental pollution improvement, developing visible light-responded high-performance optical catalysis material becomes present research focus and development trend.In recent years, Bi 2WO 6Because of having higher visible light activity, become the research focus in visible light photocatalysis field.People adopt methods such as coprecipitation, hydro-thermal method and the organic sedimentation of metal to control Bi 2WO 6The particle size of powder has promoted photocatalysis efficiency.But after particle size reduced, nano-photocatalyst easily reunited, is difficult to separate recovery from system, has limited nano-photocatalyst material application in practice.Present photocatalytic product mainly is with the fixing form of film, and photocatalyst coating is reacted in substrate.Though the fixing shortcoming that has overcome the difficult separation recovery of catalyst in the suspension system of nano-photocatalyst, the specific area of conventional base is little, influences the effective active area of catalyst, has reduced catalytic activity.People such as Zhang are with Bi 2WO 6Load on and make photocatalysis membrana (J.Solid State Chem, 2007,180,1456) on the conventional quartz substrate, but experimental result shows that the activity of its photocatalytic degradation rhodamine B (RhB) is lower, is unfavorable for its application at aspects such as the depollutions of environment.For improving the activity of photocatalysis membrana, effectively one of way is to utilize the material with high-specific surface area as substrate, and then increases the effective active area of photochemical catalyst.Simultaneously, the high-ratio surface substrate can reduce vapour lock and resistance to water-flow to a certain extent, is base material more satisfactory in the practical application.Therefore, the Bi of high-ratio surface base load 2WO 6Aspects such as photocatalysis membrana is expected to purify at sewage disposal, indoor-outdoor air, antibiotic have broad application prospects.
Summary of the invention
The object of the present invention is to provide a kind of photocatalytic activity height, good cycle, the simple high-ratio surface base load of production technology Bi 2WO 6Photocatalysis membrana, method and application thereof, the Bi of preparation 2WO 6Film has the high and characteristics that easily reclaim of visible light catalysis activity.
Described preparation method of the present invention is as follows:
1) Bi 2WO 6The preparation of nano-powder
By stoichiometric proportion a certain amount of reactant is mixed and to make solution, reactant is tungstates of the nitrate that contains bismuth ion, citrate, oxalates, chloride etc. and tungstenic etc., and solvent is water, ethanol, ethylene glycol, glycerine or polyethylene glycol etc.Above-mentioned mixed solution is put into water heating kettle, and the volume compactedness is 30～95%, reacts 5～70 hours down at 60～300 ℃, and the product that obtains makes Bi through centrifugal, washing, drying 2WO 6Nano-powder.
2) high-ratio surface base load Bi 2WO 6The preparation of photocatalysis membrana
With above-mentioned Bi 2WO 6Nano-powder forms suspension through ultrasonic being dispersed in water, the ethanol equal solvent, lifts through dipping in suspension with clean substrate and makes Bi 2WO 6Film, pull rate are 0.1～10cmmin -1Repeat to lift number of times after the drying, required catalytic amount in load is after 100～950 ℃ of heat treatments make high-ratio surface base load Bi 2WO 6Photocatalysis membrana.
The invention is characterized in Bi 2WO 6Nano-powder is deposited in the high-ratio surface substrate, generates Bi 2WO 6Photocatalysis membrana, described high-ratio surface substrate is wire netting, foam metal or porous ceramics;
Described wire netting is 50～500 orders, and the porosity of foam metal or porous ceramics is 30-90%;
Described woven wire is stainless steel, copper or iron;
Described foam metal is nickel foam or titanium foam;
Described porous ceramics is a porous Al 2O 3, porous TiO 2Or porous TiN.
The present invention has the following advantages:
1. Zhi Bei Bi 2WO 6Film has solved the nano-photocatalyst problem of difficult separation and recycling in actual applications effectively;
2. the Bi of high-ratio surface base load 2WO 6Photocatalysis membrana has the cyclical stability that high photocatalytic activity is become reconciled, the multiple pollutant of can degrading at short notice, and after recycling, still keep high catalytic activity, there is good prospects for application (seeing embodiment for details) aspects such as rhodamine B, air cleaning, antibacterial activity of degrading under visible light, specifically, Bi 2WO 6Photocatalysis membrana under 90 minutes-240 minutes conditions of irradiation under the visible light of wavelength＞420nm rhodamine B be degraded to 80-98%;
3. the Bi of high-ratio surface base load 2WO 6Photocatalysis membrana has characteristics such as stability is high, the preparation method is simple, production cost is low, environmental friendliness, suitable batch process.And the Bi that provides 2WO 6Photocatalysis membrana is convenient to recovery and reuse; Solved in the nano-photocatalyst practical application and reclaimed problem of difficult.
Description of drawings
The Bi of Fig. 1 stainless steel cloth load 2WO 6Photocatalysis membrana is degraded under radiation of visible light in the RhB process, the time dependent curve of RhB solution absorbance.
The Bi of Fig. 2 stainless steel cloth load 2WO 6Under radiation of visible light, the degrade circulation experiment result of RB of photocatalysis membrana.
The Bi of Fig. 3 stainless steel cloth load 2WO 6Photocatalysis membrana is degraded under radiation of visible light in the aldehydes gas process, the time dependent curve of the gas concentration lwevel of generation.
The Bi that Fig. 4 is foamed nickel supported 2WO 6Photocatalysis membrana is degraded under radiation of visible light in the RhB process, the time dependent curve of RhB solution absorbance.
Fig. 5 porous TiO 2The Bi of potsherd load 2WO 6Photocatalysis membrana is degraded under radiation of visible light in the RhB process, the time dependent curve of RhB solution absorbance.
The specific embodiment
Embodiment 1
Bi 2WO 6Use Bi (NO 3) 35H 2O and Na 2WO 42H 2O (analyzing pure) is synthetic for raw material, according to stoichiometric proportion, takes by weighing 0.97gBi (NO 3) 35H 2O and 0.329gNa 2WO 42H 2O is dissolved in respectively in the ethylene glycol, obtains settled solution after above-mentioned two kinds of solution mix, and transfers to then in the water heating kettle, heats 16 hours down at 160 ℃.After reaction finishes, with the product that obtains through centrifugal, washing back 60 ℃ of dryings 4 hours down.The stainless steel cloth of cleaning is immersed in the even Bi that disperseed 2WO 6In the alcohol suspension of nano-powder, adopt dip-coating method to make Bi 2WO 6Film repeats to lift number of times after the drying, about 20gm in load -2Bi 2WO 6,, make the Bi of stainless steel cloth load after 200 ℃ of heat treatments 2WO 6Photocatalysis membrana.
For research institute prepares the performance of photocatalysis membrana in waste water control is used, the design visible light is the experiment of degraded RhB dyestuff down.Utilize the character of RhB photocatalytic degradation decolouring,, observe the variation of solution colour, and then draw percent of decolourization by the absorbance of ultraviolet/visible absorbance spectrometry solution at 553nm.(irradiation 90 minutes down of λ＞420nm), 50mL concentration is 10 at the visible light of 500W xenon lamp -5The RhB of mol/L (rhodamine B) solution obviously fades, and Fig. 1 has provided Bi 2WO 6In the photocatalysis membrana degraded RhB process, the time dependent curve of RhB solution absorbance.After the illumination 90 minutes, the degradation rate of RhB solution is 98%.For determining the stability of this photocatalysis membrana, Fig. 2 has provided circulation degraded result of experiment under the same terms, C among the figure 0Be initial concentration solution, C is the solution concentration of t time.Through 5 circulation degradation experiments, this Bi 2WO 6The photocatalytic activity of film does not significantly reduce, and has good stable.
Design the experiment of this photocatalysis membrana in air cleaning is used, utilize the photocatalytic degradation experiment of acetaldehyde (100ppm) gas, measure the output of carbon dioxide by gas chromatograph, and then draw the degradation rate of aldehydes gas.Fig. 3 has provided the curve that carbon dioxide output changes with light application time, the visible light of 500W xenon lamp (λ＞420nm) down illumination after 1 hour about 70% acetaldehyde be degraded to carbon dioxide.
Utilize colony counting method to estimate prepared Bi 2WO 6The photocatalysis antibacterial activity.To spend the night with the Escherichia coli that the LB nutrient solution is cultivated, collection, centrifugal, the physiological saline washing with 0.9% three times, dilution is～10 more at last 7The suspension of cfu/ml.(λ＞420nm) irradiation is after 2 hours down, and antimicrobial efficiency reaches more than 85% at the visible light of 500W xenon lamp.
Embodiment 2
Adopt the method identical, press stoichiometric proportion with Bi (NO with embodiment 1 3) 35H 2O and Na 2WO 42H 2O (analyzing pure) is a raw material, and ethylene glycol is the synthetic Bi of solvent 2WO 6, and the mode that the employing dipping lifts is with Bi 2WO 6Nano-powder loads in the nickel foam substrate.Through the contrast experiment, the Bi that obtains 2WO 6After 4 hours, film has been degraded 90% RhB (as shown in Figure 4) at the radiation of visible light of wavelength X＞420nm.
Embodiment 3
Adopt the method identical, press stoichiometric proportion with Bi (NO with embodiment 1 3) 35H 2O and Na 2WO 42H 2O (analyzing pure) is a raw material, and ethylene glycol is the synthetic Bi of solvent 2WO 6, and the mode that the employing dipping lifts is with Bi 2WO 6Nano-powder loads on porous TiO 2On the potsherd.Through comparative experiments, the Bi that obtains 2WO 6After 4 hours, film has been degraded 95% RhB at the radiation of visible light of wavelength X＞420nm.
Embodiment 4
Bi 2WO 6Use bismuth citrate and Na 2WO 42H 2O (analyzing pure) is synthetic for raw material, according to stoichiometric proportion, takes by weighing 0.796g bismuth citrate and 0.329gNa 2WO 42H 2O is dissolved in respectively in the 20mL ethylene glycol, obtains settled solution after above-mentioned two kinds of solution mix, and transfers to then in the water heating kettle of 50mL, heats 16 hours down at 160 ℃.Adopt the method identical, with the Bi that obtains with embodiment 1 2WO 6It is online that nano-powder loads on 400 purpose stainless steel wires.Through comparative experiments, the Bi that obtains 2WO 6After 90 minutes, film has been degraded 81% RhB at the radiation of visible light of wavelength X＞420nm.
Embodiment 5
Bi 2WO 6Use bismuth citrate and Na 2WO 42H 2O (analyzing pure) is synthetic for raw material, according to stoichiometric proportion, takes by weighing the 0.796g bismuth citrate and is dissolved in the 20mL ethanol 0.329gNa 2WO 42H 2O (analyzing pure) is dissolved in the 20mL deionized water, transfers in the water heating kettle of 50mL after above-mentioned two kinds of solution mix, and heats 16 hours down at 160 ℃.Adopt the method identical, with the Bi that obtains with embodiment 1 2WO 6It is online that nano-powder loads on 400 purpose stainless steel wires.Through comparative experiments, the Bi that obtains 2WO 6After 90 minutes, film has been degraded 63% RhB at the radiation of visible light of wavelength X＞420nm.
Embodiment 6
Bi 2WO 6Use Bi (NO 3) 35H 2O and Na 2WO 42H 2O (analyzing pure) is synthetic for raw material, according to stoichiometric proportion, takes by weighing 0.97g Bi (NO 3) 35H 2O and 0.329gNa 2WO 42H 2O is dissolved in respectively in the 20mL glycerine, obtains settled solution after above-mentioned two kinds of solution mix, and transfers to then in the water heating kettle of 50mL, heats 16 hours down at 160 ℃.Adopt the method identical, with the Bi that obtains with embodiment 1 2WO 6It is online that nano-powder loads on 400 purpose stainless steel wires.Through comparative experiments, the Bi that obtains 2WO 6After 90 minutes, film has been degraded 83% RhB at the radiation of visible light of wavelength X＞420nm.

Claims (10)

1. high-ratio surface base load Bi 2WO 6Photocatalysis membrana is characterized in that Bi 2WO 6Nano-powder is deposited in the high-ratio surface substrate, generates Bi 2WO 6Photocatalysis membrana, described high-ratio surface substrate is wire netting, foam metal or porous ceramics.
2. by the described high-ratio surface base load of claim 1 Bi 2WO 6Photocatalysis membrana is characterized in that described wire netting is 50～500 orders, and the porosity of foam metal or porous ceramics is 30-90%.
3. by the described high-ratio surface base load of claim 1 Bi 2WO 6Photocatalysis membrana is characterized in that:
(1) described woven wire is stainless steel, copper or iron;
(2) described foam metal is nickel foam or titanium foam;
(3) described porous ceramics is a porous Al 2O 3, porous TiO 2Or porous TiN.
4. preparation is as each described high-ratio surface base load Bi among the claim 1-3 2WO 6The method of photocatalysis membrana is characterized in that described preparation method comprises Bi 2WO 6The preparation of nano-powder and high-ratio surface base load Bi 2WO 6In two steps of preparation of photocatalysis membrana, concrete steps are:
A) Bi 2WO 6The preparation of nano-powder
By stoichiometric proportion reactant is mixed and to make solution, reactant is the nitrate, citrate, oxalates or the chloride that contain bismuth ion and the tungstates of tungstenic, then the above-mentioned solution that mixes is put into water heating kettle, reacted 5～70 hours down at 60～300 ℃, the product that obtains makes Bi through centrifugal, washing, drying 2WO 6Nano-powder;
B) high-ratio surface base load Bi 2WO 6The preparation of photocatalysis membrana
The nano-powder that step a is made forms suspension through ultrasonic being dispersed in water or the alcohol solvent, lifts through dipping in suspension with the substrate of the cleaning after cleaning and makes Bi 2WO 6Film repeats after the drying to lift, and required catalytic amount in load after 100～950 ℃ of heat treatments, thereby makes high-ratio surface base load Bi 2WO 6Photocatalysis membrana.
5. by the described high-ratio surface base load of claim 4 Bi 2WO 6The preparation method of photocatalysis membrana is characterized in that the solution that mixes among the step a puts into the water heating kettle volume and be filled to 30-95%.
6. by the described high-ratio surface base load of claim 4 Bi 2WO 6The preparation method of photocatalysis membrana, the solvent that it is characterized in that the described homogeneous solution of step a is water, ethanol, ethylene glycol, glycerine or polyethylene glycol.
7. by the described high-ratio surface base load of claim 4 Bi 2WO 6The preparation method of photocatalysis membrana is characterized in that the described pull rate of step b is 0.1-10cmmm -1
8. by each described high-ratio surface base load Bi among the claim 1-3 2WO 6The application of photocatalysis membrana is characterized in that being used for degraded rhodamine B, air cleaning or photocatalysis antibacterial activity under the visible light.
9. by the described high-ratio surface base load of claim 8 Bi 2WO 6The application of photocatalysis membrana is characterized in that Bi 2WO 6Photocatalysis membrana under 90 minutes-240 minutes conditions of irradiation under the visible light of wavelength＞420nm rhodamine B be degraded to 80-98%.
10. by the described high-ratio surface base load of claim 8 Bi 2WO 6The application of photocatalysis membrana is characterized in that:
When (1) being used for air cleaning the wavelength of 500W xenon lamp greater than the radiation of visible light of 420nm after 1 hour 70% acetaldehyde be degraded to CO 2Gas;
(2) at the wavelength of 500W xenon lamp greater than the radiation of visible light of 420nm 2 hours, antimicrobial efficiency reaches more than 85%.
CN2009101975807A 2009-10-22 2009-10-22 Bi2WO6 photocatalysis membrane loaded by base with high specific surface, method and application thereof Expired - Fee Related CN101745402B (en)

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CN102500390A (en) * 2011-11-17 2012-06-20 陕西科技大学 Preparation method of iron oxide/bismuth tungstate composite photocatalyst
CN102557472A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing bismuth tungstate film in sol-gel method
CN102963934A (en) * 2012-12-12 2013-03-13 中国科学院上海硅酸盐研究所 Preparation method of bismuth tungstate quantum dot and preparation method of bismuth tungstate quantum dot-graphene composite material
CN103272583A (en) * 2013-02-04 2013-09-04 上海交通大学 Preparation method for transition of photocatalysis material on Yb3+-Er3+-Tm3+ doped CaF2 matrix loaded Cr3+-Bi2WO6
CN104383915A (en) * 2014-11-19 2015-03-04 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of supported photocatalyst Bi2WO6-TiO2/foam metal
CN104785260A (en) * 2015-04-24 2015-07-22 上海电力学院 Visible-light-driven photocatalyst for catalytic conversion of methane, as well as preparation method and application thereof
CN106732679A (en) * 2016-12-26 2017-05-31 苏州大学 A kind of composite of visible light catalytic and preparation method thereof and the application in water process
CN107159311A (en) * 2017-04-25 2017-09-15 西北师范大学 A kind of flower-shaped bismuth tungstate porphyrin composite and preparation method thereof
CN109772349A (en) * 2017-11-13 2019-05-21 广州中国科学院沈阳自动化研究所分所 A kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type zinc and its preparation method and application
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CN102500390A (en) * 2011-11-17 2012-06-20 陕西科技大学 Preparation method of iron oxide/bismuth tungstate composite photocatalyst
CN102500390B (en) * 2011-11-17 2013-08-14 陕西科技大学 Preparation method of iron oxide/bismuth tungstate composite photocatalyst
CN102557472A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing bismuth tungstate film in sol-gel method
CN102963934A (en) * 2012-12-12 2013-03-13 中国科学院上海硅酸盐研究所 Preparation method of bismuth tungstate quantum dot and preparation method of bismuth tungstate quantum dot-graphene composite material
CN103272583A (en) * 2013-02-04 2013-09-04 上海交通大学 Preparation method for transition of photocatalysis material on Yb3+-Er3+-Tm3+ doped CaF2 matrix loaded Cr3+-Bi2WO6
CN103272583B (en) * 2013-02-04 2015-01-21 上海交通大学 Preparation method for transition of photocatalysis material on Yb3+-Er3+-Tm3+ doped CaF2 matrix loaded Cr3+-Bi2WO6
CN104383915A (en) * 2014-11-19 2015-03-04 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of supported photocatalyst Bi2WO6-TiO2/foam metal
CN104785260A (en) * 2015-04-24 2015-07-22 上海电力学院 Visible-light-driven photocatalyst for catalytic conversion of methane, as well as preparation method and application thereof
CN106732679A (en) * 2016-12-26 2017-05-31 苏州大学 A kind of composite of visible light catalytic and preparation method thereof and the application in water process
CN107159311A (en) * 2017-04-25 2017-09-15 西北师范大学 A kind of flower-shaped bismuth tungstate porphyrin composite and preparation method thereof
CN109772349A (en) * 2017-11-13 2019-05-21 广州中国科学院沈阳自动化研究所分所 A kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type zinc and its preparation method and application
CN110772890A (en) * 2018-07-30 2020-02-11 天津大学 Ferroferric oxide-loaded SiC foamed ceramic and preparation method and application thereof
CN110772890B (en) * 2018-07-30 2021-11-19 天津大学 Ferroferric oxide-loaded SiC foamed ceramic and preparation method and application thereof
CN110639556A (en) * 2019-10-17 2020-01-03 扬州大学 Composite photocatalyst and preparation process thereof

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