CN102380379A - 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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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
Become the focus of current people's research with the conductor photocatalysis degrading organic contaminant in wastewater.There are some researches show, semiconductor catalyst many organic pollutions of under ultra violet lamp, can degrading, 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 have research proof ZnO to have and TiO
2Identical light degradation mechanism.
But owing to can not effectively utilize ultraviolet light or visible light, adsorption capacity is lower, and factors such as electronics-hole-recombination have caused the application of semiconductor catalyst to be restricted.In recent years, existing report is semiconductor catalyst and material with carbon element, like CNT
12, C
60 13, active carbon
14In conjunction with the catalytic activity of coming less these restrictions and raising photochemical catalyst.But, because CNT and C
60Expensive and the complex disposal process of price comparison, the two all is not widely used.Active carbon has bigger specific area and meso-hole structure, can adsorb a large amount of dye molecules.And active carbon is prone to preparation and cheap, and these all make it that potential application is arranged aspect photocatalysis.Also an important method that improves the ZnO photocatalytic activity on the ZnO surface in addition, such as Pt noble metal loading
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 the photocatalytic activity that improves semiconductor light-catalyst.
Summary of the invention
One of the object of the invention is to provide a kind of Ag/ZnO-AC photochemical catalyst.
Two of the object of the invention is to provide the preparation method of this photochemical catalyst.
For achieving the above object, the present invention adopts following technical scheme.
A kind of Ag/ZnO-AC photochemical catalyst is characterized in that this photochemical catalyst is is skeleton with the activated carbon, and load has the 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; The mass ratio of Ag and ZnO is in the described Ag/ZnO nano particle: 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 kind of method for preparing above-mentioned Ag/ZnO-AC photochemical catalyst is characterized in that the concrete steps of this method are:
A. the preparation of nano-ZnO: with soluble zinc salt and (NH
3)
2CO
3Be dissolved in the deionized water reaction 1h～2h, filtration washing, drying by 1:1～1:2; Calcine 2h～2.5h down at 300 ℃-900 ℃;
B. the preparation of nanometer Ag/ZnO: with concentration is that 0.1mol/L～0.01mol/L silver soluble salting liquid is heated to boiling; 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, cooling naturally gets 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, stir 2～3h, filter as demulsifier, washing, drying obtains the 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 water-soluble mixed solution of forming with absolute ethyl alcohol of active carbon, ultrasonic dispersions 1h adds the Ag/ZnO nano particle of step c gained then, stirring and adsorbing 2h, and filtration washing, drying must the Ag/ZnO-AC photochemical catalyst; Wherein the mass ratio of active carbon and Ag/ZnO nano particle is: 1:100～10:100.
Be because in compound on the one hand,, make the dyestuff that is adsorbed on the catalyst increase because the big adsorption capacity of the surface area ratio of active carbon is very strong.On the other hand, Ag is as the electronics recipient, thereby effectively separate electronic-hole suppresses its compound degraded that promotes dyestuff.So 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.
Description of drawings
Fig. 1 (a) active carbon, (b) Ag/ZnO, (c, d) scanning electron microscope diagram of 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 the 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 influence of initial p H methyl orange degradation under ultra violet lamp;
Fig. 6 is Ag/ZnO-AC=40mg, pH=7, and initial concentration is to the influence of methyl orange degradation under ultra violet lamp;
Fig. 7 is Ag/ZnO-AC=40mg, pH=7, [MO]=10mg/L, the influence of ZnO calcining heat under ultra violet lamp.
The specific embodiment
Embodiment one:
1.1Reagent and instrument
AgNO
3(A.P., Chemical Reagent Co., Ltd., Sinopharm Group), C
6H
5Na
3O (Shanghai chemical reagent 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 a 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: in beaker, add an amount of ZnNO
3, be dissolved in the proper amount of deionized water, under agitation add equimolar (NH
3)
2CO
3, reaction 2h, filtration washing, drying; In Muffle furnace, calcine 2h down for 400 ℃.
1.3 the preparation of nanometer Ag/ZnO: AgNO3 solution 10ml 0.01mol/L is heated to boiling, adds 10ml 1wt% citric acid three sodium solution, continue boiling 15min, cooling naturally gets 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, washing, drying.
1.4 the preparation of Ag/ZnO-AC: the 100mg active carbon is dissolved in the mixed solution of an amount of 20ml water and 10ml absolute ethyl alcohol composition, ultrasonic dispersion 1h adds Ag/ZnO 1 then
g, stirring and adsorbing 2h, filtration washing, drying.
The experiment of photocatalytic degradation methyl orange solution
The photocatalytic degradation experiment is carried out in catalytic unit; Catalyst directly is added in methyl orange (MO) solution (being crocus), and light source is the uviol lamp of 500W, the magnetic agitation photocatalytic degradation; Every at a distance from the 10min sampling and testing; After the centrifugation, get the upper strata stillness of night, carry out the mensuration of absorbance at the maximum absorption wavelength 464nm place of MO.Degradation effect is represented with degradation efficiency:
2.1The sign of sample: the sample active carbon, the scanning electron microscope diagram of Ag/ZnO and Ag/ZnO-AC is as shown in Figure 1.Fig. 1 c, d show the surface that loads on Graphene of ZnO nano particle success, form stable ZnO/GS compound, and more even in the Graphene surface distributed.But ZnO all is distributed in its surface with individual particle, and that also has plenty of cluster is distributed in the GS surface.Can infer that thus the size of ZnO load capacity can have influence on the pattern of compound, and then have influence on the catalytic performance of composite catalyst.So the size of ZnO load capacity also is one of key factor that investigation catalyst activity will be considered after us.Fig. 2 is sample ZnO, Ag/ZnO, the X-ray diffractogram of ZnO-AC and Ag/ZnO-AC.The diffraction maximum that occurs among the pure ZnO of sample with can both be corresponding with ZnO (JCPDS 36-1451), the diffraction maximum identical with ZnO all appearred among the Ag/ZnO, ZnO-AC and Ag/ZnO-AC.Ag/ZnO and Ag/ZnO-AC ° diffraction maximum occurred in 2 θ=38.1, and this diffraction maximum is the diffraction maximum of Ag, and this diffraction maximum with the Ag (JCPDS card No. 80-0074) of standard is corresponding.But at Fig. 2 c, but do not occur the diffraction maximum of active carbon among the d, this possibly be that content with active carbon has relation very little.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 light, so Ag/ZnO-AC has shown best photocatalytic activity.
Photocatalysis experiment: ZnO, Ag/ZnO, ZnO-AC, the photocatalytic activity of Ag/ZnO-AC is accomplished through light degradation methyl orange under UV-irradiation, and the result is as shown in Figure 7.Can know by figure, with respect to ZnO, Ag/ZnO, ZnO-AC, the photocatalysis efficiency of Ag/ZnO-AC compound improves a lot.After the 150min, methyl orange solution is all degradeds almost.But, ZnO, Ag/ZnO, ZnO-AC catalyst have only degraded 61%, 67%, 70% respectively.Photocatalysis is the result fully show, Ag and active carbon have all played important function in the Ag/ZnO-AC photochemical catalyst.
The photocatalytic activity of Ag/ZnO-AC improves a lot relatively, mainly contains following two reasons.Be exactly owing to,,, thereby improved photocatalysis efficiency on the one hand for light degradation provides the catalytic environment of high concentration so have the surface that more dye molecule is attracted to catalyst because the big adsorption capacity of the surface area ratio of active carbon is very strong.Another reason is exactly in composite catalyst, and Ag has also played a crucial effects.At Ag/ZnO-AC, the Ag nano particle has played the effect that electronics is accepted, and has therefore effectively separated fairy maiden and hole, has suppressed the compound of electron hole, thereby makes more valence electron can participate in the efficient that has improved degraded in the degradation process of dyestuff.Can be learnt that by experimental result the photocatalytic activity of Ag/ZnO-AC is all higher than ZnO-AC and Ag/ZnO, explains in composite catalyst, active carbon and Ag have improved the catalytic activity of ZnO jointly.
Methyl orange solution PH is to the influence of degradation rate
The initial p H of methyl orange solution is as shown in Figure 5 to the influence of degradation rate.Can know that by Fig. 6 the initial p H of solution is very big to the influence of degradation rate.Particularly under alkalescence and acid condition, raising is arranged, and find that the effect of the photocatalytic degradation under acid condition is best with respect to the degradation rate under the neutrallty condition.Can infer that thus light-catalyzed reaction does not occur over just catalyst surface, and occurs in around the catalyst surface.
The methyl orange initial concentration is to the influence of degradation rate
The scope of the methyl orange initial concentration of investigating is 10-30mg/L, and the result is as shown in Figure 6.Have the result to know, initial concentration is big more, and photocatalytic degradation efficient is more little, in other fuel of light degradation, has also found similar result.Initial concentration has following reason to the influence of catalytic efficiency: be along with the change of initial concentration is big on the one hand, have more methyl orange concentration and be adsorbed on the methyl orange surface that this will influence the degraded of catalyst.The change of initial concentration is big on the other hand, has also hindered proton and has entered into methyl orange solution.Therefore, along with the change of initial concentration is big, the photochemical catalyst rate can decrease.
Calcining heat is to the influence of degradation rate
In the preparation process of ZnO, the calcining heat of ZnO is also influential to the catalytic efficiency of Ag/ZnO-AC.Therefore, investigate the influence to degradation rate in 300 ℃ of-900 ℃ of scopes of ZnO calcining heat.Can know that by Fig. 7 calcining heat has very significantly influence to the degradation rate of catalyst.Along with the influence of calcining heat, degradation rate reduces on the contrary.The reason that causes this phenomenon possibly 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, through absorption method on active carbon load Ag/ZnO, successful preparation the Ag/ZnO-AC composite photo-catalyst.Through the 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, and the calcining heat of initial concentration and ZnO is to the influence of degradation rate and discuss.Can infer that thus this work will opened up a new field aspect the raising ZnO catalytic activity, thereby promotes to solve various environmental problems.
Claims (4)
1. an Ag/ZnO-AC photochemical catalyst is characterized in that this photochemical catalyst is is skeleton with the activated carbon, and load has the 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; The mass ratio of Ag and ZnO is in the described Ag/ZnO nano particle: 0.6: 1～0.75:1.
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.
4. method for preparing according to claim 1,2 or 3 described Ag/ZnO-AC photochemical catalysts is characterized in that the concrete steps of this method are:
A. the preparation of nano-ZnO: with soluble zinc salt and (NH
3)
2CO
3Be dissolved in the deionized water reaction 1h～2h, filtration washing, drying by 1:1～1:2; Calcine 2h～2.5h down at 300 ℃-900 ℃;
B. the preparation of nanometer Ag/ZnO: with concentration is that 0.1mol/L～0.01mol/L silver soluble salting liquid is heated to boiling; 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, cooling naturally gets 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, stir 2～3h, filter as demulsifier, washing, drying obtains the 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 water-soluble mixed solution of forming with absolute ethyl alcohol of active carbon, ultrasonic dispersions 1h adds the Ag/ZnO nano particle of step c gained then, stirring and adsorbing 2h, and filtration washing, drying must the Ag/ZnO-AC photochemical catalyst; Wherein the mass ratio of active carbon and Ag/ZnO nano particle is: 1:100～10:100.
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| CN104525119A (en) * | 2015-01-05 | 2015-04-22 | 福建农林大学 | G-C3N4/ZnO/activated carbon functional charcoal adsorption material and preparation method thereof |
| CN104841454A (en) * | 2015-04-22 | 2015-08-19 | 南京理工大学 | Preparation method of Pd-Fe2O3/GO composite material |
| CN104857946A (en) * | 2015-05-12 | 2015-08-26 | 上海大学 | Method for using zinc electroplating sludge to prepare azo dyes photocatalyst |
| CN105032418A (en) * | 2015-08-18 | 2015-11-11 | 河南师范大学 | Preparation method of Ag/ZnO-carbon sphere ternary shell-core heterojunction photocatalysts with different microtopographies |
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| CN1962054A (en) * | 2006-11-30 | 2007-05-16 | 华南理工大学 | Method for preparing Ag sensitized zinc oxide photocatalyst with visible light activity |
| CN101711000A (en) * | 2009-11-17 | 2010-05-19 | 天津大学 | Coding scheme based on acquisition of three primary colors with widest sensible color gamut |
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2011
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Patent Citations (2)
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| CN1962054A (en) * | 2006-11-30 | 2007-05-16 | 华南理工大学 | Method for preparing Ag sensitized zinc oxide photocatalyst with visible light activity |
| CN101711000A (en) * | 2009-11-17 | 2010-05-19 | 天津大学 | Coding scheme based on acquisition of three primary colors with widest sensible color gamut |
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| CN104525119A (en) * | 2015-01-05 | 2015-04-22 | 福建农林大学 | G-C3N4/ZnO/activated carbon functional charcoal adsorption material and preparation method thereof |
| CN104525119B (en) * | 2015-01-05 | 2016-09-07 | 福建农林大学 | A kind of g-C3n4functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof |
| CN104841454A (en) * | 2015-04-22 | 2015-08-19 | 南京理工大学 | Preparation method of Pd-Fe2O3/GO composite material |
| CN104857946A (en) * | 2015-05-12 | 2015-08-26 | 上海大学 | Method for using zinc electroplating sludge to prepare azo dyes photocatalyst |
| CN105032418A (en) * | 2015-08-18 | 2015-11-11 | 河南师范大学 | Preparation method of Ag/ZnO-carbon sphere ternary shell-core heterojunction photocatalysts with different microtopographies |
| CN105032418B (en) * | 2015-08-18 | 2017-11-21 | 河南师范大学 | The preparation method of diverse microcosmic appearance Ag/ZnO carbon ball ternary shell dyskaryosis knot photochemical catalysts |
| CN105709689A (en) * | 2016-03-04 | 2016-06-29 | 唐山建华科技发展有限责任公司 | Carbon-based functional material and preparation method thereof |
| CN109499563A (en) * | 2017-09-15 | 2019-03-22 | 张家港市沐和新材料技术开发有限公司 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
| CN110227453A (en) * | 2019-04-17 | 2019-09-13 | 江苏省农业科学院 | A kind of preparation method of Ag/ZnO/GO composite visible light catalyst |
| CN110227453B (en) * | 2019-04-17 | 2022-03-25 | 江苏省农业科学院 | Preparation method of AgCl/ZnO/GO composite visible light catalyst |
| US11717810B1 (en) | 2022-03-18 | 2023-08-08 | Najran University | Nanocomposite photocatalyst and method of degrading organic pollutant therewith |
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