CN103638929B - A kind of Graphene-wolframic acid silver composite photocatalyst material and preparation method thereof - Google Patents
A kind of Graphene-wolframic acid silver composite photocatalyst material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Graphene-wolframic acid silver composite photocatalyst material and preparation method thereof, belong to composite and photocatalysis technology field.The present invention obtains the dispersion liquid of graphene oxide by ultrasonic stripping graphite oxide, then in dispersion liquid, successively add silver nitrate and sodium tungstate solution, stir, regulate pH to 1.5-3.0, hydrothermal treatment consists 12-24 hour at 140-200 DEG C again, prepares Graphene-wolframic acid silver composite material.This composite has controlled pattern, bar-shaped wolframic acid silver wrap up by the Graphene of flexibility, Compound Degree is good; This material not only has certain adsorption effect to organic dyestuff; it is also better to the photocatalytic degradation effect of organic dyestuff under visible light illumination; be a kind of desirable compound visible-light photocatalysis material, have broad application prospects in the field such as environmental protection, functional composite material.
Description
Technical field
The present invention relates to a kind of Graphene-wolframic acid silver composite photocatalyst material and preparation method thereof, belong to composite and photocatalysis technology field.
Background technology
As the basis of industrial development, material is the important symbol of measurement national overall national strength and living standards of the people always, and in order to adapt to the various requirement of New Times development to material, the Development Scheme of various new function material also continues to bring out.Be in the China in industrialization and urbanization high speed development stage, be but faced with the two large problems of energy shortage and environment deterioration, this drastically influence the sustainable development of human society.In theory, obtain cheapness and the solar energy of sustainable use from occurring in nature, reducing the various organic pollution of preparing hydrogen energy cost Sum decomposition is the reliable approach solved the problem.Solar energy, due to distinctive superiority such as its storage capacity are large, security is high, energy consumption is low, environmentally friendly, makes it in solution energy crisis and environmental pollution improvement, have good application prospect.Therefore, utilize photocatalysis technology oxidation Decomposition organic pollution, in curbing environmental pollution, there is profound significance.
Photocatalysis technology a kind ofly utilizes luminous energy as the energy to realize the technology of catalysis.The photocatalysis characteristic of semiconductor is confirmed by much research, but from catalytic efficiency, also there is the problem of this technology extensive use of many restrictions.The quantum efficiency how improving photochemical catalyst with make this technology economically can accept by people to be one of the research focus of current international photocatalysis field.The specific area of the compound again suppressing photo-generate electron-hole right and raising catalyst improves two kinds of effective methods of catalyst photocatalytic activity at present.The former is mainly by the impact of photochemical catalyst electronic structure, and latter is relevant with the pattern of photochemical catalyst.Doping vario-property is carried out to photochemical catalyst, effectively can suppress photo-generate electron-hole compound, increase photo-generate electron-hole interface migration rate again, and prepare pattern uniqueness, specific area that the powder of nano-scale greatly can increase photochemical catalyst, make its oxidation efficiency higher, at room temperature the Some Organic Pollutants in water, air and soil can be completely oxidized to the harmless products such as nontoxic carbon dioxide and water, there is no secondary pollution.
Graphene is mono-layer graphite crystal, and it is the basic structural unit building other dimension carbonaceous materials (as zero dimension fullerene, one dimension CNT, three-dimensional graphite).Graphene has excellent electricity, calorifics and mechanical property, is expected to obtain extensive use in fields such as high-performance nano electronic device, composite, field emmision material, gas sensor and stored energies.Due to the two-dimensional structure of its uniqueness, Graphene has contained the abundant and physical phenomenon of novelty, and the research for quantum-mechanical phenomenon provides desirable platform, have important researching value.In addition, Graphene has again larger specific area, has good adsorption capacity to pollutant, and the good light permeability of Graphene is also for photocatalysis provides good condition simultaneously.In recent years, Graphene has a wide range of applications preparing compound catalyze material field.
Due to the existence of Graphene, the light induced electron of wolframic acid silver can be caught, to suppress their compound, improve quantum efficiency.Meanwhile, can effectively expand light absorbing wave-length coverage, improve the utilization rate of visible ray., effectively can promote the oxidation Decomposition of wolframic acid silver to pollutant.
The core of photocatalysis technology is the design and development of catalysis material.Recently, low-dimensional metal tungstates nano material is synthesized as BaWO
4nanometer rods, CdWO
4nanometer rods, BiWO
6powder causes the great interest of scientist, and come from them has great application prospect in a lot of field, as luminescence generated by light, optical fiber, scintillator material, humidity sensor and catalyst etc.Prepared all exigent temperature of method of tungstates material and harsh reaction condition in the past, as in the solid phase reaction of 1000 DEG C and sol-gel process, product morphology of its synthesis is mainly powder, nano particle and micron block.Wolframic acid silver prior synthesizing method passes through WO
3/ Ag
2o system directly obtains under severe reaction conditions.Chinese invention patent CN 101792183B discloses the ultrasonic-sluggish precipitation of a kind of employing and prepares the ultra-fine silver tungstate antibacterial powder that particle diameter is 2 ~ 3 microns, a kind of method adopting microwave heating method to prepare nanometer solid diamond wolframic acid silver that patent CN 102583550A reports, this preparation method exists that process complexity, particle size are comparatively large, pattern is not all first-class not enough, and these materials are applied at electro-conductive glass and antibacterial FIELD OF THE INVENTIONThe at present.But about the report of wolframic acid Silver nanorod synthesis is little, and wolframic acid silver does not find at the report of photocatalysis field application.
Literature survey finds, with graphene oxide, silver nitrate and sodium tungstate for raw material, adopts hydro-thermal method to prepare visible light-responded Graphene-wolframic acid silver composite photocatalyst material and is not reported so far.
The present invention prepares a kind of Graphene-wolframic acid silver composite material, different from general graphene composite material, in this Graphene-wolframic acid silver composite material, wolframic acid Silver nanorod is not just simply attached to the surface of graphene film, but be wrapped in by graphene film, so both can prevent the oxidation of wolframic acid silver, the specific area of photochemical catalyst can be increased again, be expected the desired light catalysis material becoming degradation of contaminant.
Summary of the invention
For overcoming above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of simple possible, the visible light-responded Graphene that with low cost, structural constituent is controlled-wolframic acid silver composite photocatalyst material and preparation method thereof.
The invention provides a kind of Graphene-wolframic acid silver composite photocatalyst material, described composite photocatalyst material is composited by Graphene and wolframic acid silver, and wolframic acid silver is club shaped structure, and wrap up by Graphene; There is good absorption in the ultraviolet-visible light district that Graphene-wolframic acid silver composite material is 200-800 nm at wavelength, and absorbance is between 0.2-1.2; Have good adsorption-photocatalytic degradation effect to organic dyestuff rhodamine B, under dark condition to the adsorption rate of organic dyestuff close to 20%, radiation of visible light after 2 hours degradation rate be 70%, to the adsorption-photocatalytic degradation rate of organic dyestuff rhodamine B more than 90%.
The present invention also provides the preparation method of a kind of Graphene-wolframic acid silver composite photocatalyst material, prepares in accordance with the following steps:
(1) be dissolved in deionized water by graphene oxide, ultrasonic 3-5 hour, obtains dispersion liquid.
(2) in step (1) gained graphene oxide dispersion, add silver nitrate, dropwise add the sodium tungstate aqueous solution after stirring, obtain mixed solution.
(3) be transferred in polytetrafluoroethylliner liner by step (2) gained mixed solution, inner bag is placed in stainless steel outer sleeve, and after sealing, after reacting 12-24 hour at 140-200 DEG C, reactor naturally cools to room temperature.
(4) by the product that step (3) obtains, centrifugation, then uses distilled water and absolute ethanol washing, vacuum drying respectively, obtains Graphene-wolframic acid silver composite photocatalyst material.
Wherein in the dispersion liquid described in step (1), graphene oxide concentration is 0.025wt%-1wt%.
Wherein the salpeter solution of the mixed solution described in step (2) adjusts pH to 1.5-3.0; In mixed solution, the concentration of silver nitrate is 0.067-0.375 mol/L, and the concentration of sodium tungstate is 0.117-0.350 mol/L.
advantage and effect
The invention provides a kind of Graphene-wolframic acid silver composite photocatalyst material and preparation method thereof, this material environmental protection, preparation technology is simple, and raw material is easy to get.Compared with tradition single wolframic acid silver photochemical catalyst, this composite photo-catalyst, the collaborative advantage of wolframic acid silver and Graphene can be played, promote that photogenerated charge is separated, widens the photoresponse scope of Ag tungstate catalyst, improves the catalytic stability of wolframic acid silver, and be conducive to the recycling of wolframic acid silver, reduce cost.Graphene-wolframic acid silver the visible light catalyst of preparation can effectively adsorb and photocatalytically degradating organic dye and hazardous contaminant, can not cause secondary pollution.In the field such as environmental protection, functional composite material, there is important using value.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of Graphene-wolframic acid silver composite photocatalyst material.
Fig. 2 is the X-ray diffraction spectrogram of Graphene-wolframic acid silver composite photocatalyst material.
Fig. 3 is the solid-state UV-visible absorption spectra figure of Graphene-wolframic acid silver composite photocatalyst material.
Fig. 4 is Graphene-wolframic acid silver composite photocatalyst material under dark and radiation of visible light, to the absorption-degradation effect curve map of organic dyestuff rhodamine B.
Detailed description of the invention
The present embodiment implements under premised on technical solution of the present invention; give detailed embodiment; following non-limiting example is used for explaining and the present invention is described; instead of limit the invention; in the protection domain of spirit of the present invention and claim; the any amendment make the present invention and change, all belong to protection scope of the present invention.
embodiment 1:
5 mg graphene oxides are added in 20 mL deionized waters, within ultrasonic 3 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 8 mmol, carry out magnetic agitation, and the aqueous solution 20 mL dropwise dripped in solution containing 14 mmol sodium tungstates, then be 1.5 by salpeter solution adjust ph.Finally, above-mentioned mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, react 24 hours at 140 DEG C, after product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 2:
10 mg graphene oxides are added in 20 mL deionized waters, within ultrasonic 5 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 15 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 14 mmol, then be 1.5 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, react 20 hours at 160 DEG C; After product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 3:
20 mg graphene oxides are added in 20 mL deionized waters, within ultrasonic 3 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 4 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 7 mmol, then be 2.0 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 24 hours at 140 DEG C; After product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 4:
50 mg graphene oxides are added in 30 mL deionized waters, within ultrasonic 3 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 8 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 14 mmol, then be 2.0 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 20 hours at 160 DEG C, after the product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 5:
100 mg graphene oxides are added in 30 mL deionized waters, within ultrasonic 5 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 10 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 14 mmol, then be 2.0 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 16 hours at 180 DEG C, after the product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
The scanning electron microscope diagram of Fig. 1 Graphene prepared by embodiment 5-wolframic acid silver composite material, from figure, we can find out that wolframic acid silver is club shaped structure, and on Graphene, distribution is in order; The x-ray diffraction pattern of the Graphene-wolframic acid silver composite material of Fig. 2 prepared by this embodiment 5, the diffraction maximum occurred in figure can well be attributed to wolframic acid silver, because graphene oxide addition is less, in-situ reducing is not only measured few after becoming Graphene, and diffraction maximum relative to crystallization wolframic acid silver diffraction maximum too weak, so do not observe the characteristic diffraction peak of Graphene in XRD figure.Solid-state UV-visible absorption spectra the figure of the Graphene-wolframic acid silver composite material of Fig. 3 prepared by this embodiment 5, as can be seen from figure we, the visibility region that Graphene-wolframic acid silver composite material is 200-800 nm at wavelength has very strong absorption, and absorbance is between 0.2-1.2.
embodiment 6:
200 mg graphene oxides are added in 40 mL deionized waters, within ultrasonic 5 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 4 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 7 mmol, then be 2.5 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 16 hours at 180 DEG C; After product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 7:
200 mg graphene oxides are added in 40 mL deionized waters, within ultrasonic 3 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 8 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 14 mmol, then be 2.5 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 12 hours at 200 DEG C, after the product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 8:
500 mg graphene oxides are added in 50 mL deionized waters, within ultrasonic 5 hours, obtain graphene oxide dispersion, then in the dispersion liquid of above-mentioned graphene oxide, add the silver nitrate of 15 mmol, magnetic stirrer stirs, and in solution, dropwise drip the sodium tungstate aqueous solution 20 mL of 14 mmol, then be 3.0 by salpeter solution adjust ph.Finally above-mentioned mixed liquor is transferred to the hydrothermal reaction kettle of 100 mL, react 12 hours at 200 DEG C, after the product high speed centrifugation after hydro-thermal reaction is separated, with deionized water, washes of absolute alcohol, after repeated centrifugation washing for several times, be placed in vacuum drying oven dry.
embodiment 9:
Graphene prepared by the present invention-wolframic acid silver composite photocatalyst material applies to the photocatalysis experiment of organic dyestuff rhodamine B, detailed process and step as follows: the Graphene of 100 mg-wolframic acid silver composite material is scattered in the rhodamine B solution of 100 mL5 ppm, the dispersion liquid mixed continues to stir until reach adsorption equilibrium, then the dispersion liquid mixed is transferred in xenon lamp catalytic reaction instrument, after light-catalyzed reaction starts, extracting the postradiation mixed solution of 4 mL every 20 minutes with syringe transfers in the centrifuge tube of mark, light-catalyzed reaction is after 2 hours, by the sample centrifugation in all centrifuge tubes, centrifugal rear obtained supernatant liquor is transferred in quartz colorimetric utensil further, ultraviolet-visible spectrophotometer measures the absorbance under different catalysis time, thus under obtaining each time period composite photo-catalyst to rhodamine B photocatalytic degradation effect.
The Graphene of Fig. 4 prepared by embodiment 5-wolframic acid silver composite photocatalyst material under dark and visible light conditions to the absorption of rhodamine B and photocatalytic degradation figure, as can be seen from figure we, ultrasonic 10 minutes and stir within 30 minutes, reach the dark condition of adsorption equilibrium under, nano composite material to the adsorption ratio of organic dyestuff rhodamine B close to 20%; After opening visible light source irradiation, along with the growth of irradiation time, rhodamine B is constantly degraded, the degradation rate of illumination rhodamine B after 2 hours more than 70%, thus can find out that the Graphene-total adsorption-photocatalytic degradation rate of wolframic acid silver composite photocatalyst material to organic dyestuff rhodamine B prepared by embodiment 5 reaches about 90%.
Claims (4)
1. a Graphene-wolframic acid silver composite photocatalyst material, it is characterized in that, described composite photocatalyst material is composited by Graphene and wolframic acid silver, and wolframic acid silver is club shaped structure, and wrap up by Graphene
;the ultraviolet-visible light district absorbance that this composite is 200-800 nm at wavelength is 0.2-1.2.
2. a preparation method for Graphene-wolframic acid silver composite photocatalyst material, is characterized in that, carry out according to following steps:
(1) be dissolved in deionized water by graphene oxide, ultrasonic 3-5 hour, obtains dispersion liquid;
(2) in step (1) gained graphene oxide dispersion, add silver nitrate, dropwise add the sodium tungstate aqueous solution after stirring, obtain mixed solution;
(3) be transferred in polytetrafluoroethylliner liner by step (2) gained mixed solution, inner bag is placed in stainless steel outer sleeve, and after sealing, after reacting 12-24 hour at 140-200 DEG C, reactor naturally cools to room temperature;
(4) by the product that step (3) obtains, centrifugation, then uses distilled water and absolute ethanol washing, vacuum drying respectively, obtains Graphene-wolframic acid silver composite photocatalyst material;
Mixed solution described in step (2) salpeter solution adjusts pH to 1.5-3.0; In mixed solution, the concentration of silver nitrate is 0.067-0.375 mol/L, and the concentration of sodium tungstate is 0.117-0.350 mol/L.
3. the preparation method of a kind of Graphene according to claim 2-wolframic acid silver composite photocatalyst material, it is characterized in that, in the dispersion liquid described in step (1), graphene oxide concentration is 0.025wt%-1wt%.
4. the preparation method of a kind of Graphene according to claim 2-wolframic acid silver composite photocatalyst material, is characterized in that, prepared Graphene-wolframic acid silver composite photocatalyst material is applied to the adsorption-photocatalytic degradation to organic dyestuff.
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| CN104071798B (en) * | 2014-07-03 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | A kind of ultra-thin montmorillonite-based nano sheet and its preparation method and application |
| CA3040705A1 (en) | 2014-08-20 | 2016-02-25 | Arturo Solis Herrera | Uses of melanin in water |
| CN106268804B (en) * | 2016-07-21 | 2018-08-17 | 吉林师范大学 | One step hydrothermal technique prepares Ag2O/Ag2WO4The method of nanometer rods |
| CN106268805B (en) * | 2016-08-17 | 2019-03-26 | 哈尔滨理工大学 | A kind of silver-wolframic acid silver nanowires and preparation method thereof |
| CN106335926A (en) * | 2016-08-17 | 2017-01-18 | 哈尔滨理工大学 | Silver tungstate nanowire and preparation method thereof |
| CN109692700B (en) * | 2018-11-30 | 2021-09-07 | 华纺股份有限公司 | Fibrous load type g-C3N4/Ag2WO4The photocatalytic material and the preparation method thereof |
| CN113398949A (en) * | 2021-08-16 | 2021-09-17 | 广西大学 | Magnetic reduction graphene oxide/silver tungstate composite photocatalyst and preparation method and application thereof |
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