CN102380379B - Ag/ZnO-AC photochemical catalyst and preparation method thereof - Google Patents
Ag/ZnO-AC photochemical catalyst and preparation method thereof Download PDFInfo
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- CN102380379B CN102380379B CN201110278450.3A CN201110278450A CN102380379B CN 102380379 B CN102380379 B CN 102380379B CN 201110278450 A CN201110278450 A CN 201110278450A CN 102380379 B CN102380379 B CN 102380379B
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Abstract
The invention relates to an Ag/ZnO-AC photochemical catalyst and a preparation method thereof. The photochemical catalyst is a composite photochemical catalyst which utilizes activated carbon as a skeleton and carries Ag/ZnO nano-particles. The mass ratio of activated carbon to Ag/ZnO nano-particles is 1:100-10:100, and the mass ratio of Ag in Ag/ZnO nano-particles to ZnO therein is 0.6:1-0.75:1. On the one hand, the quantity of dye adsorbed to the catalyst is increased due to the fact that the superficial area of activated carbon in composite is larger and adsorption capacity of activated carbon is higher, and on the other hand, electron-hole separation can be realized effectively by the aid of Ag serving as an electron acceptor to restrain electron-hole recombination so that degradation of dye is promoted. Compared with pure ZnO, Ag/ZnO and ZnO-AC, the Ag/ZnO-AC composite photochemical catalyst has the advantages that photocatalysis thereof is improved greatly.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method thereof, particularly a kind of Ag/ZnO-AC photochemical catalyst and preparation method thereof.
Background technology
With the organic pollution in conductor photocatalysis degrading waste water, become the focus of current people's research.There are some researches show, semiconductor catalyst many organic pollutions of can degrading under ultra violet lamp, such as washing agent, dyestuff, agricultural chemicals, volatile organic compound etc.Up to the present, TiO
2be considered to one of best semiconductor light-catalyst.But there are some researches show ZnO having shown special value aspect some pollutants of degraded, such as the sewage of bleached pulp factory, phenol and 2-phenylphenol etc.And, also there are some researches prove that ZnO has and TiO
2identical light degradation mechanism.
But owing to can not effectively utilizing ultraviolet light or visible ray, adsorption capacity is lower, and electron-hole is compound etc., and factor has caused the application of semiconductor catalyst to be restricted.In recent years, have been reported a semiconductor catalyst and material with carbon element, as CNT
12, C
60 13, active carbon
14in conjunction with carrying out less these restrictions and improving the catalytic activity of photochemical catalyst.But, due to CNT and C
60expensive and the complex disposal process of price comparison, the two is not all widely used.Active carbon has larger specific area and meso-hole structure, can adsorb a large amount of dye molecules.And active carbon is easily prepared and be cheap, these all make it aspect photocatalysis, have potential application.Noble metal loading, on ZnO surface, be also an important method that improves ZnO photocatalytic activity in addition, such as Pt
21, Pd
22, Ag
23deng.These noble metals play the effect that electronics is accepted and shifted in compound, catch photo-generated carrier, thereby improve electronic transfer process and photocatalytic activity.Silver has certain help to improving the photocatalytic activity of semiconductor light-catalyst.
Summary of the invention
One of object of the present invention is to provide a kind of Ag/ZnO-AC photochemical catalyst.
Two of object of the present invention is to provide the preparation method of this photochemical catalyst.
For achieving the above object, the present invention adopts following technical scheme.
An Ag/ZnO-AC photochemical catalyst, is characterized in that this photochemical catalyst is to take activated carbon as skeleton, and load has Ag/ZnO nano particle and the composite photocatalyst that forms; Wherein the mass ratio of activated carbon and Ag/ZnO nano particle is: 1:100～10:100; In described Ag/ZnO nano particle, the mass ratio of Ag and ZnO is: 0.6: 1～0.75:1.
Above-mentioned activated carbon has: granular pattern activated carbon or powder-type activated carbon.
The particle diameter of above-mentioned Ag/ZnO nano particle is: 20nm～30nm.
A method of preparing above-mentioned Ag/ZnO-AC photochemical catalyst, is characterized in that the concrete steps of the method are:
A. the preparation of nano-ZnO: by soluble zinc salt and (NH
3)
2cO
3by 1:1～1:2, be dissolved in deionized water, reaction 1h～2h, filtration washing, dry; At 300 ℃-900 ℃, calcine 2h～2.5h;
B. the preparation of nanometer Ag/ZnO: be that 0.1mol/L～0.01mol/L silver soluble salting liquid is heated to boiling by concentration, adding concentration is the citric acid three sodium solution of 1wt%～2 wt%, and wherein the mol ratio of soluble silver salt and trisodium citrate is 0.25:1～0.3:1; Continue boiling 15～20min, naturally cooling, obtain Ag colloidal sol;
C. in the Ag colloidal sol of step b gained, add step b gained ZnO, be warming up to 50 ℃～55 ℃, add NaCl as demulsifier, stir 2～3h, filter, washing, dry, obtain Ag/ZnO nano particle; Wherein the mass ratio of Ag, ZnO and NaCl is: 0.75:1:5～0.6:1:5;
The preparation of d.Ag/ZnO-AC: in the mixed solution that the water-soluble and absolute ethyl alcohol of active carbon is formed, ultrasonic dispersions 1h, then adds the Ag/ZnO nano particle of step c gained, stirring and adsorbing 2h, filtration washing, is dried, and obtains Ag/ZnO-AC photochemical catalyst; Wherein the mass ratio of active carbon and Ag/ZnO nano particle is: 1:100～10:100.
That because the larger adsorption capacity of surface area ratio of active carbon is very strong, the dyestuff that makes to be adsorbed on catalyst increases because in compound on the one hand.On the other hand, Ag is as electronics recipient, thereby effectively separate electronic-hole suppresses its compound degraded that promotes dyestuff.Therefore Ag/ZnO-AC composite photo-catalyst of the present invention and pure ZnO, Ag/ZnO compares with ZnO-AC, and its photocatalytic activity improves a lot.
Accompanying drawing explanation
Fig. 1 (a) active carbon, (b) Ag/ZnO, the scanning electron microscope diagram of (c, d) Ag/ZnO-AC;
Fig. 2 ZnO (a), Ag/ZnO (b), ZnO-AC (c), the X-ray diffractogram of and Ag/ZnO-AC (d);
Fig. 3 (a) ZnO, (b) Ag/ZnO, (c) ZnO-AC, (d) Ag/ZnO-AC ultraviolet-diffuse reflection absorption spectrum;
Fig. 4 is (a) ZnO under ultra violet lamp, (b) Ag/ZnO, (c) ZnO-AC, (d) degradation effect of Ag/ZnO-AC;
Fig. 5 is Ag/ZnO-AC=40mg, [MO]=20mg/L, t=60mmin, the impact of initial p H methyl orange degradation under ultra violet lamp;
Fig. 6 is Ag/ZnO-AC=40mg, pH=7, the impact of initial concentration on methyl orange degradation under ultra violet lamp;
Fig. 7 is Ag/ZnO-AC=40mg, pH=7, [MO]=10mg/L, the impact of ZnO calcining heat under ultra violet lamp.
The specific embodiment
embodiment mono-:
1.1reagent and instrument
AgNO
3(A.P., Chemical Reagent Co., Ltd., Sinopharm Group), C
6h
5na
3o (Solution on Chemical Reagents in Shanghai Co., Ltd of Chinese Medicine group), NaCl (A.R., Chemical Reagent Co., Ltd., Sinopharm Group); active carbon (A.R., Chemical Reagent Co., Ltd., Sinopharm Group), ethanol (A.R.; Chemical Reagent Co., Ltd., Sinopharm Group), ZnNO
3(A.P., Chemical Reagent Co., Ltd., Sinopharm Group), (NH
4)
2cO
3(A.P., Chemical Reagent Co., Ltd., Sinopharm Group).Experimental water is deionized water.Key instrument has CR21G II high speed freezing centrifuge (Japanese Hitachi company), U-3010 type ultraviolet-visible spectrophotometer (Japanese Hitachi company), JSM-2010F type x-ray powder diffraction instrument (Jeol Ltd.), JSM-6700F high resolution scanning electron microscope (Jeol Ltd.), photocatalysis apparatus.
The preparation of nano-ZnO: add appropriate ZnNO in beaker
3, be dissolved in appropriate deionized water, under agitation add equimolar (NH
3)
2cO
3, reaction 2h, filtration washing, dry; In Muffle furnace, at 400 ℃, calcine 2h.
The preparation of 1.3 nanometer Ag/ZnO: AgNO3 solution 10ml 0.01mol/L is heated to boiling, adds 10ml 1wt% citric acid three sodium solution, continue boiling 15min, naturally cooling, obtain Ag colloidal sol.In Ag colloidal sol, add through heat treated 1g ZnO, be warming up to 50 ℃, add 5g NaCl as demulsifier, stirring and adsorbing 2h, filters, and washing is dry.
The preparation of 1.4 Ag/ZnO-AC: 100mg active carbon is dissolved in the mixed solution of appropriate 20ml water and 10ml absolute ethyl alcohol composition, ultrasonic dispersion 1h, then adds Ag/ZnO 1
g, stirring and adsorbing 2h, filtration washing, dry.
Photocatalytic Degradation On Methyl Orange Solution experiment
Photocatalytic degradation experiment is carried out in catalytic unit, catalyst is directly added in methyl orange (MO) solution (being crocus), light source is the uviol lamp of 500W, magnetic agitation photocatalytic degradation, every 10min sampling and testing, after centrifugation, get the upper strata stillness of night, at the maximum absorption wavelength 464nm place of MO, carry out the mensuration of absorbance.Degradation effect represents with degradation efficiency:
2.1the sign of sample: sample active carbon, the scanning electron microscope diagram of Ag/ZnO and Ag/ZnO-AC as shown in Figure 1.Fig. 1 c, d shows that ZnO nano particle successfully loads on the surface of Graphene, forms stable ZnO/GS compound, and more even in Graphene surface distributed.But ZnO is all distributed in its surface with individual particle, that also has plenty of cluster is distributed in GS surface.Can infer thus, the size of ZnO load capacity can have influence on the pattern of compound, and then has influence on the catalytic performance of composite catalyst.So the size of ZnO load capacity is also one of key factor that after us, investigation catalyst activity will be considered.Fig. 2 is sample ZnO, Ag/ZnO, the X-ray diffractogram of ZnO-AC and Ag/ZnO-AC.The diffraction maximum occurring in the pure ZnO of sample with can be corresponding with ZnO (JCPDS 36-1451), Ag/ZnO, ZnO-AC with in Ag/ZnO-AC, all there is the diffraction maximum identical with ZnO.Ag/ZnO and Ag/ZnO-AC ° have occurred that diffraction maximum, this diffraction maximum are the diffraction maximums of Ag in 2 θ=38.1, and this is corresponding with the diffraction maximum of the Ag (JCPDS card No. 80-0074) of standard.But at Fig. 2 c, but do not occur the diffraction maximum of active carbon in d, this may be to have very little relation with the content of active carbon.Sample Ag/ZnO-AC, ZnO-AC, the diffuse reflection absorption spectrum of Ag/ZnO and ZnO is as shown in Figure 3.Compare with ZnO, Ag/ZnO-AC, ZnO-AC, the scope of the absorption band of Ag/ZnO is red shift to some extent all, but the degree of Ag/ZnO-AC is maximum.Because the red shift of Ag/ZnO-AC band, makes catalyst can effectively utilize more visible ray, so Ag/ZnO-AC has shown best photocatalytic activity.
Photocatalysis experiment: ZnO, Ag/ZnO, ZnO-AC, the photocatalytic activity of Ag/ZnO-AC completes by Photodegradation of Methyl Orange under UV-irradiation, and result is as shown in Figure 7.As seen from the figure, with respect to ZnO, Ag/ZnO, ZnO-AC, the photocatalysis efficiency of Ag/ZnO-AC compound improves a lot.After 150min, methyl orange solution is all degradeds almost.But, ZnO, Ag/ZnO, ZnO-AC catalyst has only degraded respectively 61%, 67%, 70%.Photocatalysis result fully shows, in Ag/ZnO-AC photochemical catalyst, Ag and active carbon have all played important function.
The photocatalytic activity of Ag/ZnO-AC improves a lot relatively, mainly contains following two reasons.Be exactly because the larger adsorption capacity of the surface area ratio due to active carbon is very strong on the one hand, so have the surface that more dye molecule is attracted to catalyst, for light degradation provides the catalytic environment of high concentration, thereby improved photocatalysis efficiency.Another reason is exactly in composite catalyst, and Ag has also played a vital effect.At Ag/ZnO-AC, Ag nano particle has played the effect that electronics is accepted, and therefore effectively separated fairy maiden and hole, suppressed the compound of electron hole, thereby makes more valence electron can participate in the efficiency that has improved degraded in the degradation process of dyestuff.By experimental result, can be learnt, the photocatalytic activity of Ag/ZnO-AC is all higher than ZnO-AC and Ag/ZnO, illustrates in composite catalyst, and active carbon and Ag have improved the catalytic activity of ZnO jointly.
The impact of methyl orange solution PH on degradation rate
The initial p H of methyl orange solution on the impact of degradation rate as shown in Figure 5.As shown in Figure 6, the initial p H of solution is very large on the impact of degradation rate.Particularly, under alkalescence and acid condition, with respect to the degradation rate under neutrallty condition, be improved, and find that the effect of the photocatalytic degradation under acid condition is best.Can infer thus, light-catalyzed reaction does not occur over just catalyst surface, and occurs in around catalyst surface.
The impact of methyl orange initial concentration on degradation rate
The scope of the methyl orange initial concentration of investigating is 10-30mg/L, and result as shown in Figure 6.Have result known, initial concentration is larger, and photocatalytic degradation efficiency is less, in other fuel of light degradation, has also found similar result.Initial concentration has following reason to the impact of catalytic efficiency: be along with the change of initial concentration is large on the one hand, have more methyl orange concentration and be adsorbed on methyl orange surface, this will affect the degraded of catalyst.The change of initial concentration is large on the other hand, has also hindered proton and has entered into methyl orange solution.Therefore,, along with the change of initial concentration is large, photochemical catalyst rate can decrease.
The impact of calcining heat on degradation rate
In the preparation process of ZnO, the calcining heat of ZnO also has impact to the catalytic efficiency of Ag/ZnO-AC.Therefore, investigate the impact on degradation rate within the scope of 300 ℃-900 ℃ of ZnO calcining heat.As shown in Figure 7, calcining heat has very significantly impact to the degradation rate of catalyst.Along with the impact of calcining heat, degradation rate reduces on the contrary.The reason that causes this phenomenon may be the increase along with calcining heat, and the size of ZnO particle increases, thereby causes the minimizing on ZnO surface, has finally caused the photocatalysis efficiency of Ag/ZnO-AC to reduce.
On the basis of synthetic Ag/ZnO, by absorption method on active carbon load Ag/ZnO, successfully prepared Ag/ZnO-AC composite photo-catalyst.By degraded methyl orange solution, show that the photocatalytic activity of the ZnO catalyst after compound improves a lot.And the PH of initial methyl orange solution has also been investigated in this experiment, the calcining heat of initial concentration and ZnO is on the impact of degradation rate and discuss.Can infer thus, this work will improve new field of ZnO catalytic activity blaze, thereby promotes to solve various environmental problems.
Claims (3)
1. an Ag/ZnO-AC photochemical catalyst, is characterized in that this photochemical catalyst is to take activated carbon as skeleton, and load has Ag/ZnO nano particle and the composite photocatalyst that forms; Wherein the mass ratio of activated carbon and Ag/ZnO nano particle is: 1:100～10:100; In described Ag/ZnO nano particle, the mass ratio of Ag and ZnO is: 0.6: 1～0.75:1, this photochemical catalyst followed these steps to prepare:
A. the preparation of nano-ZnO: by soluble zinc salt and (NH
4)
2cO
3by 1:1～1:2, be dissolved in deionized water, reaction 1h～2h, filtration washing, dry; At 300 ℃-900 ℃, calcine 2h～2.5h;
B. the preparation of nanometer Ag/ZnO: be that 0.1mol/L～0.01mol/L silver soluble salting liquid is heated to boiling by concentration, adding concentration is the citric acid three sodium solution of 1wt%～2 wt%, and wherein the mol ratio of soluble silver salt and trisodium citrate is 0.25:1～0.3:1; Continue boiling 15～20min, naturally cooling, obtain Ag colloidal sol;
C. in the Ag colloidal sol of step b gained, add step a gained ZnO, be warming up to 50 ℃～55 ℃, add NaCl as demulsifier, stir 2～3h, filter, washing, dry, obtain Ag/ZnO nano particle; Wherein the mass ratio of Ag, ZnO and NaCl is: 0.75:1:5～0.6:1:5;
The preparation of d.Ag/ZnO-AC: in the mixed solution that the water-soluble and absolute ethyl alcohol of activated carbon is formed, ultrasonic dispersions 1h, then adds the Ag/ZnO nano particle of step c gained, stirring and adsorbing 2h, filtration washing, is dried, and obtains Ag/ZnO-AC photochemical catalyst; Wherein the mass ratio of activated carbon and Ag/ZnO nano particle is: 1:100～10:100.
2. Ag/ZnO-AC photochemical catalyst according to claim 1, is characterized in that described activated carbon has: granular pattern activated carbon or powder-type activated carbon.
3. Ag/ZnO-AC photochemical catalyst according to claim 1, is characterized in that the particle diameter of described Ag/ZnO nano particle is: 20nm～30nm.
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