CN103721713B - A kind of three-phase composite visible of efficient degradation dyestuff - Google Patents
A kind of three-phase composite visible of efficient degradation dyestuff Download PDFInfo
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- CN103721713B CN103721713B CN201410006052.XA CN201410006052A CN103721713B CN 103721713 B CN103721713 B CN 103721713B CN 201410006052 A CN201410006052 A CN 201410006052A CN 103721713 B CN103721713 B CN 103721713B
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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 discloses a kind of three-phase composite visible and its preparation method and application, belong to the technical field of material preparation and environmental pollution improvement.Adopt chemical oxidization method to prepare Graphene, then Graphene reduction is formed reduced graphene, adopt solvent structure reduced graphene/Bi
2moO
6compound, then adopt impregnation-reduction method to be carried on compound by Au, form reduced graphene/Bi
2moO
6/ Au three-phase composite thing.Photochemical catalyst specific area prepared by the present invention is large, and active component utilizes high, has the effect of efficient visible light photocatalysis to degrade organic matter.
Description
Technical field
The invention belongs to the technical field of material preparation and environmental pollution improvement, be specifically related to three-phase composite visible of a kind of efficient degradation dye organic pollutant and preparation method thereof.
Background technology
Along with the continuous discharge of the industrial wastewater such as Dyestuff synthesis, printing and dyeing and the continuous use of various dyestuff, dye quantity and the kind of entered environment constantly increase, and the environmental pollution that dyestuff causes is on the rise.According to statistics, the dyestuff in the whole world about 15% is discharged in waste water in process of production, and these colorful wastewaters can generate poisonous accessory substance by oxidation, hydrolysis and other chemical reaction in the environment.Pollution control means (physical treatment, biological treatment, conventional chemical process) traditional at present can not thoroughly be eliminated, and therefore develop a kind of green, free of contamination process means are imperative.
Photocatalysis technology is a kind of high-level oxidation technology, and its principle is that photochemical catalyst is as titanium dioxide (TiO
2) under the action of uv light, produce hole and electronics, and further by chemical action generation, there are some high activity groups such as highly active various free radicals, participate in redox reaction degradation of contaminant.This technology has very strong mineralization ability to organic matter, thus makes poisonous organic matter permineralization become inorganic matter or be converted into free of contamination product.At present, TiO
2the application of photocatalysis technology in environmental protection has relevant report.But, the TiO generally used
2there is the drawback that quantum efficiency is low and solar energy utilization ratio is low in based photocatalyst.For these problems, researchers are to TiO
2carry out a large amount of study on the modification and comprise various metal and nonmetal doping, precious metal surface deposition, semiconductors coupling, dye sensitization etc., make some progress, but fundamentally solve quantum efficiency and these two significant problems of solar energy utilization ratio not yet, thus impel researchers further sight line to be turned to non-TiO
2the compound of series, attempts the efficient photochemical catalyst of development of new and the response range widening photochemical catalyst.
Under we report radiation of visible light in previous work, bismuth molybdate can dyestuff organic matter in degradation water, but bismuth molybdate photochemical catalyst quantum efficiency is low, and the easy compound of light induced electron and hole, causes the photocatalysis performance of bismuth molybdate lower.For the problem of the easy compound of catalyst photo-generated carrier, be generally adopt to carry out modification to catalyst, suppress the compound of photo-generate electron-hole with this.In numerous method of modifying, build the effective way that composite photo-catalyst has been proved to be to improve catalyst photocatalysis degradation organic contaminant.In composite photo-catalyst, the interface between the semiconductor light-catalyst of compound or metal causes more effective Charge transfer on interface, thus photo-generated carrier is effectively separated.So far, the bismuth molybdate base composite photocatalyst reported mainly contains Bi
2moO
6/ TiO
2, Bi
2moO
6/ C, Ag/AgBr/Bi
2moO
6, Graphene/Bi
2moO
6deng, all effectively improve the activity of bismuth molybdate photocatalysis degradation organic contaminant.Wherein, complexing agent Graphene is a kind of superior co-catalyst, it is a kind of nano material of the bi-dimensional cellular shape lattice structure become by monolayer carbon atom close-packed arrays, due to the layer structure that Graphene is graphite, a large amount of not paired electronics is had to move about in its surface, this makes the electric conductivity of the existing metal of Graphene have again the performance of semiconductor, and CNT also has large specific area and is easy to adsorb organic compound, these factors theories all contribute to the interface light-catalyzed reaction based on electron transmission, adding of Graphene is conducive to the right compound of suppression photo-generate electron-hole, improve the photocatalytic activity of catalyst.Yuetal. Bi is constructed
2moO
6-RGO nano-complex, improve the bactericidal property of bismuth molybdate photochemical catalyst, but its activity still has much room for improvement, in recent years, research about three-phase composite photochemical catalyst shows, three-phase composite object light catalyst shows the catalytic activity higher than two-phase compound, traces it to its cause as three-phase composite photochemical catalyst better can suppress the compound of photo-generate electron-hole, thus greatly improves the performance of photochemical catalyst photocatalysis degradation organic contaminant.Numerous research shows, effectively can improve photocatalysis performance at catalyst surface loaded with nano gold grain, nanogold particle can serve as electric transmission track, thus the separation rate that the photo-generate electron-hole improving catalyst surface is right, the activity of catalyst is improved greatly.Based on this, on the basis of Graphene/bismuth molybdate two-phase compound, further supported nano-gold particle forms three-phase composite thing, is used for degradation of dye organic pollution, and this has greater significance to the application of popularization bismuth molybdate in degradation of dye organic wastewater.
Summary of the invention
The object of the present invention is to provide three-phase composite visible of a kind of efficient degradation dye organic pollutant and preparation method thereof.This photochemical catalyst specific area is large, and active component utilizes high, can realize the dye organic pollutant in efficient degradation waste water, has larger application potential.
For achieving the above object, the present invention adopts following technical scheme:
The present invention adopts solvent-thermal method and impregnation-reduction method respectively reduced graphene and gold to be carried on bismuth molybdate surface, and then the efficient visible light catalyst of synthesis reduced graphene/bismuth molybdate/golden three-phase composite, wherein the mass concentration of reduced graphene and gold is 0.1%-0.4%.
The concrete steps of described preparation method are: the preparation of (1) reduced graphene: take 3g graphite and 18g potassium permanganate respectively, after being ground, join in the concentrated sulfuric acid (360ml) and phosphoric acid (40ml) and form suspension, after suspension is incubated 12h at 50 DEG C, be cooled to room temperature, be poured in 400mL frozen water, after stirring, drip the H of 30wt.%
2o
2until in golden yellow, continue to be stirred to still after, centrifugal, taking precipitate, respectively with 10wt.%HCl solution and deionized water washing, until occur colloid substance cannot centrifugal till.Take out colloid substance, make the ion concentration of sol solution be less than 5ppm by dialysis.After jelly deionized water is diluted to desired concn, utilizes ultrasonication to be peeled off by graphite oxide, obtain graphene oxide.Get appropriate above-mentioned graphene oxide, add a certain amount of vitamin C (VC) solution, stir, after it is incubated 50min at 95 DEG C, obtain reduced graphene; (2) preparation of Graphene/bismuth molybdate two-phase compound: joined respectively by a certain amount of reduced graphene in polytetrafluoroethylene (PTFE) reactor, stirs, instills Bi (NO respectively
3)
35H
2o (0.27M) and Na
2moO
42H
2the ethylene glycol solution of O (0.13M), after 10min, drip NaOH (10M) solution, adjust ph is about 9, after continuing to stir 30min, take off reactor and put into stainless steel outer lining, in the baking oven of 160 DEG C, react 3h, after question response still is cooled to room temperature, the mixture in liner is carried out centrifugation, the precipitation priority distilled water of gained and absolute ethanol washing, after 80 DEG C of oven dry, grinding is for subsequent use in an oven; (3) preparation of Graphene/bismuth molybdate/golden three-phase composite thing: take a certain amount of Graphene/bismuth molybdate compound prepared, put into beaker, add appropriate amount of deionized water, stir, instill different volumes chlorauric acid solution (10mg/mL) respectively, stir one hour, 4h is irradiated under ultraviolet lamp, centrifugal, dry, obtain Graphene/bismuth molybdate/golden three-phase composite compound.
Remarkable advantage of the present invention is:
(1) reduced graphene and gold are carried on bismuth molybdate by the present invention first, have effectively been separated light induced electron and hole, are the catalyst of a kind of novel visible response.
(2) visible light catalyst of reduced graphene/bismuth molybdate/golden three-phase composite can the organic pollution such as rhodamine B degradation efficiently.
Accompanying drawing explanation
Fig. 1 is the powder X-ray RD figure of the Graphene/bismuth molybdate/golden three-phase composite photochemical catalyst of embodiment 2,4,5 and 6 gained.
Fig. 2 is that the powder TEM of the Graphene/bismuth molybdate/golden three-phase composite photochemical catalyst of embodiment 6 gained schemes.
Fig. 3 is the design sketch of the Graphene/bismuth molybdate/golden three-phase composite photocatalyst for degrading rhodamine B of embodiment 2,4,5 and 6 gained.
detailed description of the invention
Concrete steps of the present invention are:
(1) preparation of reduced graphene: take 3g graphite and 18g potassium permanganate respectively, after being ground, join in the concentrated sulfuric acid (360ml) and phosphoric acid (40ml) and form suspension, after suspension is incubated 12h at 50 DEG C, be cooled to room temperature, be poured in 400mL frozen water, after stirring, drip the H of 30%
2o
2until in golden yellow, continue to be stirred to still after, centrifugal, taking precipitate, respectively with 10%HCl solution and deionized water washing, until occur colloid substance cannot centrifugal till.Take out colloid substance, make the ion concentration of sol solution be less than 5ppm by dialysis.After jelly deionized water is diluted to desired concn, utilizes ultrasonication to be peeled off by graphite oxide, obtain graphene oxide.Get appropriate above-mentioned graphene oxide, add a certain amount of vitamin C (VC) solution, stir, after it is incubated 50min at 95 DEG C, obtain reduced graphene.
(2) preparation of Graphene/bismuth molybdate two-phase compound: joined respectively by the reduced graphene of 0.1%-0.4% load capacity in polytetrafluoroethylene (PTFE) reactor, stirs, instills Bi (NO respectively
3)
35H
2o (0.27M) and Na
2moO
42H
2the ethylene glycol solution of O (0.13M), after 10min, drip NaOH (10M) solution, adjust ph is about 9, after continuing to stir 30min, take off reactor and put into stainless steel outer lining, in the baking oven of 160-180 DEG C, react 3-5h, after question response still is cooled to room temperature, the mixture in liner is carried out centrifugation, the precipitation priority distilled water of gained and absolute ethanol washing, after 80 DEG C of oven dry, grinding is for subsequent use in an oven.
(3) preparation of Graphene/bismuth molybdate/golden three-phase composite thing: take a certain amount of Graphene/bismuth molybdate compound prepared, put into beaker, add appropriate amount of deionized water, stir, instill different volumes chlorauric acid solution (10mg/mL) respectively, stir 1-2 hour, 2-4h is irradiated under ultraviolet lamp, centrifugal, dry, obtain Graphene/bismuth molybdate/golden three-phase composite compound.
Be below several embodiments of the present invention, further illustrate the present invention, but the present invention is not limited only to this.
embodiment 1: the preparation of reduced graphene
Take 3g graphite and 18g potassium permanganate respectively, after being ground, joining in the concentrated sulfuric acid (360mL) and phosphoric acid (40mL) and form suspension, after suspension is incubated 12h at 50 DEG C, be cooled to room temperature, be poured in 400mL frozen water, after stirring, drip the H of 30%
2o
2until in golden yellow, continue to be stirred to still after, centrifugal, taking precipitate, respectively with 10%HCl solution and deionized water washing, until occur colloid substance cannot centrifugal till.Take out colloid substance, make the ion concentration of sol solution be less than 5ppm by dialysis.After jelly deionized water is diluted to desired concn, utilizes ultrasonication to be peeled off by graphite oxide, obtain graphene oxide.Get the above-mentioned graphene oxide of 100mL, add 1mL0.1M vitamin C (VC) solution, stir, after it is incubated 50min at 95 DEG C, obtain reduced graphene.
embodiment 2: the preparation of Graphene/bismuth molybdate two-phase compound
The reduced graphene 0.12mL that Example 1 obtains joins in polytetrafluoroethylene (PTFE) reactor, stirs, instills 15mLBi (NO successively
3)
35H
2o (0.27M) and Na
2moO
42H
2the ethylene glycol solution of O (0.13M), after 10min, drip NaOH (10M) solution, adjust ph is about 9, after continuing to stir 30min, take off reactor and put into stainless steel outer lining, 3h is reacted in the baking oven of 160 DEG C, after question response still is cooled to room temperature, mixture in liner is carried out centrifugation, the precipitation priority distilled water of gained and absolute ethanol washing, dry rear grinding for 80 DEG C in an oven, obtain Graphene/bismuth molybdate two-phase composite photo-catalyst that graphene-supported amount is 0.1%.
embodiment 3: the preparation of Graphene/bismuth molybdate two-phase compound
The reduced graphene 0.24mL that Example 1 obtains joins in polytetrafluoroethylene (PTFE) reactor, stirs, instills 15mLBi (NO successively
3)
35H
2o (0.27M) and Na
2moO
42H
2the ethylene glycol solution of O (0.13M), after 10min, drip NaOH (10M) solution, adjust ph is about 9, after continuing to stir 30min, take off reactor and put into stainless steel outer lining, 3h is reacted in the baking oven of 160 DEG C, after question response still is cooled to room temperature, mixture in liner is carried out centrifugation, the precipitation priority distilled water of gained and absolute ethanol washing, dry rear grinding for 80 DEG C in an oven, obtain Graphene/bismuth molybdate two-phase composite photo-catalyst that graphene-supported amount is 0.2%.
embodiment 4: the preparation of Graphene/bismuth molybdate/golden three-phase composite thing
Take Graphene/bismuth molybdate compound that 0.8g embodiment 2 is obtained, put into beaker, add appropriate amount of deionized water, stir, instill 80 μ L chlorauric acid solutions (10mg/mL), stir one hour, in suspension, add ethanol again, under ultraviolet lamp, irradiate 4h, centrifugal, dry, obtain Graphene/bismuth molybdate/golden three-phase composite compound that golden load capacity is 0.1%.
embodiment 5: the preparation of Graphene/bismuth molybdate/golden three-phase composite thing
Take Graphene/bismuth molybdate compound that 0.8g embodiment 2 is obtained, put into beaker, add appropriate amount of deionized water, stir, instill 160 μ L chlorauric acid solutions (10mg/mL), stir one hour, in suspension, add ethanol again, under ultraviolet lamp, irradiate 4h, centrifugal, dry, obtain Graphene/bismuth molybdate/golden three-phase composite compound that golden load capacity is 0.2%.
embodiment 6: the preparation of Graphene/bismuth molybdate/golden three-phase composite thing
Take Graphene/bismuth molybdate compound that 0.8g embodiment 2 is obtained, put into beaker, add appropriate amount of deionized water, stir, instill 320 μ L chlorauric acid solutions (10mg/mL), stir one hour, in suspension, add ethanol again, under ultraviolet lamp, irradiate 4h, centrifugal, dry, obtain Graphene/bismuth molybdate/golden three-phase composite compound that golden load capacity is 0.4%.
Performance test
Fig. 1 is the powder X-ray RD figure of the Graphene/bismuth molybdate/golden three-phase composite photochemical catalyst of embodiment 2,4,5 and 6 gained.Can find that from figure prepared catalyst is the bismuth molybdate of orthorhombic crystal phase, the introducing of Graphene and gold grain does not change the crystalline phase of bismuth molybdate.
Fig. 2 is that the powder TEM of the Graphene/bismuth molybdate/golden three-phase composite photochemical catalyst of embodiment 6 gained schemes.Can find bismuth molybdate and Graphene structure in the form of sheets in the Graphene/bismuth molybdate/golden three-phase composite thing prepared from figure, the two close contact, gold grain is then distributed on lamella.
Fig. 3 is the design sketch of the Graphene/bismuth molybdate/golden three-phase composite photocatalyst for degrading rhodamine B of embodiment 2,4,5 and 6 gained.Graphene/bismuth molybdate/golden three-phase composite photochemical catalyst visible light catalyst test, by rhodamine B degradation (1 × 10 under the irradiation of 300W xenon lamp
-5mol/L) characterize.Visible light catalytic reaction is carried out in HSX-F/UV300 xenon source system and device, and light source filters through optical filter, to ensure that incident light is for visible ray (λ >420nm); Catalyst amount is 40mg.Before reaction of turning on light, first adsorb 1h makes rhodamine B turn on light illumination after adsorption-desorption balance on a catalyst.The activity of the bismuth molybdate photocatalyst for degrading rhodamine B of simultaneously load gold and reduced graphene improves greatly as can be seen from Figure 3.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. a preparation method for three-phase composite visible, is characterized in that: adopt chemical oxidization method to prepare Graphene, then Graphene reduction is formed reduced graphene, adopts solvent structure reduced graphene/Bi
2moO
6compound, then adopt impregnation-reduction method to be carried on compound by Au, form reduced graphene/Bi
2moO
6/ Au three-phase composite thing;
Concrete steps are as follows:
(1) preparation of reduced graphene
Take 3g graphite and 18g potassium permanganate respectively, after being ground, joining in the mixed liquor of the 360mL concentrated sulfuric acid and 40mL phosphoric acid and form suspension, after being incubated 12h at 50 DEG C, be cooled to room temperature, be poured in 400mL frozen water, after stirring, drip the H of 30wt.%
2o
2until in golden yellow, continue to be stirred to still after, centrifugal, the HCl solution of sediment 10wt.% and deionized water washing, until occur colloid substance cannot centrifugal till; Take out colloid substance, dialyse to ion concentration and be less than 5ppm, dilute by deionized water, ultrasonic, obtain graphene oxide; Add vitamin c solution, stir, be incubated 50min at 95 DEG C, obtain reduced graphene;
(2) reduced graphene/Bi
2moO
6the preparation of compound
0.27MBi (NO is instilled while stirring in reduced graphene
3)
35H
2o and 0.13MNa
2moO
42H
2the ethylene glycol solution of O, after 10min, drip 10MNaOH solution, adjust ph is 9, and after continuing to stir 30min, 160 DEG C of reaction 3h, be cooled to room temperature, centrifugation, sediment distilled water and absolute ethanol washing, 80 DEG C of oven dry obtain reduced graphene/Bi
2moO
6compound;
(3) reduced graphene/Bi
2moO
6the preparation of/Au three-phase composite thing
Take reduced graphene/Bi
2moO
6compound, adds deionized water, stirs, and instillation 10mg/mL chlorauric acid solution, stirs 1 hour, under ultraviolet lamp, irradiate 4h, centrifugal, and dry, grinding obtains reduced graphene/Bi
2moO
6/ Au three-phase composite thing; Reduced graphene/Bi
2moO
6in/Au three-phase composite thing, the mass percent of reduced graphene is the mass percent of 0.1%-0.4%, Au is 0.1%-0.4%;
Described catalyst is used for liquid phase degradation of dye organic pollution.
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| CN103721713B true CN103721713B (en) | 2016-01-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106587028A (en) * | 2017-02-09 | 2017-04-26 | 山东佳星环保科技有限公司 | Method of preparing graphene by oxidation and reduction process |
| CN107138165B (en) * | 2017-05-08 | 2019-08-27 | 河南师范大学 | A kind of preparation method of 2/ graphene photo-catalyst of support type Bi2MoO6/Cu (OH) |
| CN108043400B (en) * | 2017-12-08 | 2019-10-18 | 浙江工业大学 | A kind of Au-Bi2MoO6/ diatomite composite material and the preparation method and application thereof |
| CN108031467B (en) * | 2017-12-08 | 2019-10-18 | 浙江工业大学 | A kind of Bi2MoO6Coat halloysite nanotubes composite material and preparation method and application |
| CN113351221B (en) * | 2021-06-08 | 2023-09-29 | 常州大学 | Preparation method and application of graphene-based bismuth-based heterostructure catalyst |
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2014
- 2014-01-07 CN CN201410006052.XA patent/CN103721713B/en active Active
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