CN101745402B - 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 PDFInfo
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- CN101745402B CN101745402B CN2009101975807A CN200910197580A CN101745402B CN 101745402 B CN101745402 B CN 101745402B CN 2009101975807 A CN2009101975807 A CN 2009101975807A CN 200910197580 A CN200910197580 A CN 200910197580A CN 101745402 B CN101745402 B CN 101745402B
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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
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 the environment of also 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 the characteristics such as reaction condition gentleness, oxidisability are strong, clean environment firendly, in recent years photocatalysis and correlation technique thereof all show goodish application potential in the conversion of environmental improvement, solar energy, all many-sides such as antibiotic, obtain fast development, 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 length (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 study hotspot and development trend.In recent years, Bi
2WO
6Because having higher visible light activity, become the study hotspot in visible light photocatalysis field.People adopt the 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.Although 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, affects the effective active area of catalyst, has reduced catalytic activity.The 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 that it is in the application of the aspects such as the depollution 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
6The aspects 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 visible light catalysis activity characteristics high and that easily reclaim.
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%, and 60~300 ℃ of lower reactions 5~70 hours, the product that obtains made 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, until required catalytic amount in the load finally by 100~950 ℃ of heat treatments, makes 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 porous Al
2O
3, porous TiO
2Or porous TiN.
The present invention has the following advantages:
1. the Bi for preparing
2WO
6Film has solved the in actual applications problem of difficult separation and recycling of nano-photocatalyst 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 application prospect (seeing embodiment for details) aspects such as rhodamine B degradation, air cleaning, antibacterial activity 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 the characteristics such as stability is high, the preparation method is simple, production cost is low, environmental friendliness, suitable batch production.And the Bi that provides
2WO
6Photocatalysis membrana is convenient to recovery and reuse; Solved a difficult problem that reclaims difficulty in the nano-photocatalyst practical application.
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 then transfers in the water heating kettle, 160 ℃ of lower heating 16 hours.After reaction finishes, that the product that obtains is lower dry 4 hours at 60 ℃ after centrifugal, washing.With the stainless steel cloth of the cleaning Bi that has been immersed in Uniform Dispersion
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, until about 20gm in the load
-2Bi
2WO
6, finally by 200 ℃ of heat treatments, make the Bi of stainless steel cloth load
2WO
6Photocatalysis membrana.
For the performance of the standby photocatalysis membrana of institute system in waste water control is used, the experiment of degraded RhB dyestuff under the design visible light.Utilize the character of RhB photocatalytic degradation decolouring, by the absorbance of ultraviolet/visible absorbance spectrometry solution at 553nm, observe the variation of solution colour, and then draw percent of decolourization.(the lower irradiation of λ>420nm) 90 minutes, 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 the result of circulation degradation 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 stability.
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 (the lower illumination of λ>420nm) after 1 hour about 70% acetaldehyde be degraded to carbon dioxide.
Utilize colony counting method to estimate prepared Bi
2WO
6Photocatalysis antibacterial active.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) lower irradiation is after 2 hours, and antimicrobial efficiency reaches more than 85% at the visible light of 500W xenon lamp.
Adopt the method identical with embodiment 1, press stoichiometric proportion with Bi (NO
3)
35H
2O and Na
2WO
42H
2O (analyzing pure) is 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 with embodiment 1, press stoichiometric proportion with Bi (NO
3)
35H
2O and Na
2WO
42H
2O (analyzing pure) is 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 then transfers in the water heating kettle of 50mL, 160 ℃ of lower heating 16 hours.Adopt the method identical with embodiment 1, with the Bi that obtains
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, 160 ℃ of lower heating 16 hours.Adopt the method identical with embodiment 1, with the Bi that obtains
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 then transfers in the water heating kettle of 50mL, 160 ℃ of lower heating 16 hours.Adopt the method identical with embodiment 1, with the Bi that obtains
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 (8)
1. the Bi of high-ratio surface base load
2WO
6Photocatalysis membrana is characterized in that Bi
2WO
6Nano-powder is deposited in the high-ratio surface substrate, and described high-ratio surface substrate is wire netting, foam metal or porous ceramics;
This Bi
2WO
6The preparation method of photocatalysis membrana comprises Bi
2WO
6The Bi of the preparation of nano-powder and high-ratio surface base load
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, 60~300 ℃ of lower reactions 5~70 hours, the product that obtains made Bi through centrifugal, washing, drying
2WO
6Nano-powder;
B) Bi of high-ratio surface base load
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, until required catalytic amount in the load, finally by 100~950 ℃ of heat treatments, thereby makes the Bi of high-ratio surface base load
2WO
6Photocatalysis membrana.
2. the Bi of high-ratio surface base load according to claim 1
2WO
6Photocatalysis membrana is characterized in that: described wire netting is 50~500 orders, and the porosity of described foam metal or porous ceramics is 30-90%.
3. the Bi of high-ratio surface base load according to claim 1
2WO
6Photocatalysis membrana is characterized in that:
(1) described wire netting is stainless steel, copper or iron;
(2) described foam metal is nickel foam or titanium foam;
(3) described porous ceramics is porous Al
2O
3, porous TiO
2Or porous TiN.
4. such as the Bi of each described high-ratio surface base load among the claim 1-3
2WO
6The preparation method of photocatalysis membrana is characterized in that comprising Bi
2WO
6The Bi of the preparation of nano-powder and high-ratio surface base load
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, 60~300 ℃ of lower reactions 5~70 hours, the product that obtains made Bi through centrifugal, washing, drying
2WO
6Nano-powder;
B) Bi of high-ratio surface base load
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, until required catalytic amount in the load, finally by 100~950 ℃ of heat treatments, thereby makes the Bi of high-ratio surface base load
2WO
6Photocatalysis membrana.
5. preparation method according to claim 4 is characterized in that it is 30-95% that the solution that mixes among the step a is put into the volume compactedness of water heating kettle.
6. preparation method according to claim 4, 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. preparation method according to claim 4 is characterized in that the described speed that lifts of step b is 0.1-10cmmin
-1
8. the Bi of each described high-ratio surface base load among the claim 1-3
2WO
6The application of photocatalysis membrana is characterized in that for rhodamine B degradation, air cleaning or photocatalysis antibacterial under the visible light.
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CN102500390B (en) * | 2011-11-17 | 2013-08-14 | 陕西科技大学 | Preparation method of iron oxide/bismuth tungstate composite photocatalyst |
CN102557472B (en) * | 2011-12-19 | 2014-04-16 | 陕西科技大学 | Method for preparing bismuth tungstate film in sol-gel method |
CN102963934B (en) * | 2012-12-12 | 2014-06-18 | 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 |
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 |
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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