CN105195155A - Preparation method of sheet-shaped alpha-Fe2O3/ZnO composite photocatalyst - Google Patents

Preparation method of sheet-shaped alpha-Fe2O3/ZnO composite photocatalyst Download PDF

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CN105195155A
CN105195155A CN201510658981.3A CN201510658981A CN105195155A CN 105195155 A CN105195155 A CN 105195155A CN 201510658981 A CN201510658981 A CN 201510658981A CN 105195155 A CN105195155 A CN 105195155A
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catalyst
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谢娟
李美霞
郝勇静
刘志勇
高鹏鹏
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Hebei University of Engineering
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Abstract

The invention relates to a preparation method of a sheet-shaped alpha-Fe2O3/ZnO composite photocatalyst. The preparation method comprises the following steps: step 1: preparing a reaction precursor liquid: under a stirring condition, dripping an alkali solution into a trivalent iron salt liquid; then dripping an zinc salt solution; after dripping, continually stirring until a mixed solution is at a muddy state containing red brown substances, wherein the mol ratio of a trivalent iron salt to an alkali to a zinc salt is (1-10) to 90 to 10; step 2: ageing: immersing a glass container filled with the reaction precursorliquid into a water-bath pot at 80-99 DEG C and ageing until sediment covers the bottom of the container and a reaction solution is clear; and filtering, washing and naturally airing to obtain the alpha-Fe2O3/ZnO composite photocatalyst. The alpha-Fe2O3/ZnO composite photocatalyst powder is prepared by adopting a low-temperature ageing method; and reaction raw materials are easy to obtain, operation steps are simple, reaction conditions are moderate and energy consumption is small, so that the preparation method can be easily popularized in industrialized mass production.

Description

A kind of sheet α-Fe 2o 3the preparation method of/ZnO composite photo-catalyst
Technical field
The present invention relates to a kind of sheet α-Fe 2o 3the preparation method of/ZnO composite photo-catalyst, belongs to photochemical catalyst preparation field.
Background technology
Semiconductor out-phase Photocatalyst is an emerging environmental contaminants purification techniques.In the catalysis material used at present, although TiO 2because redox ability is strong, stable in properties, the advantage such as nontoxic be in the core status of research always, but it still exists the easy compound of light induced electron and hole so far, and quantum efficiency is lower, cannot make full use of the problems such as visible ray.
ZnO has and TiO 2close energy gap and valence-band level position, and both Mechanism of Semiconductor Photocatalytic Degradations are identical, therefore ZnO is also a kind of excellent catalysis material in essence.The research of past ZnO photocatalyst is less, mainly because ZnO compares TiO 2exist and photoetch easily occurs and diffluent deficiency in highly acid and alkaline solution.In recent years, the report of micro-nano ZnO photocatalysis to degrade organic matter increases gradually.In addition the quantum efficiency of ZnO is higher than TiO 2, and production cost is relatively low, so ZnO very likely becomes the TiO that continues 2another application prospect photochemical catalyst widely afterwards.
Current, scientific research personnel to improve the performance of semiconductor light-catalyst, improves photocatalysis efficiency mainly through modes such as metal/non-metal doping, semiconductors coupling and precious metal surface support.Wherein composite photo-catalyst mostly is second-component system, as CdS/TiO 2, SnO 2/ TiO 2, Fe 2o 3/ SnO 2and WO 3-TiO 2deng, they all show the stability and catalytic activity that are better than single semiconductor.But be still in the starting stage by the compound system research promoted for the purpose of ZnO photocatalyst performance, complexing agent used also more is limited to TiO 2, CdS, SnO 2etc. conventional semiconductors.Therefore, the Synthesis and application research continuing to strengthen ZnO composite photo-catalyst is very important.
Although α is-Fe 2o 3energy gap narrower, light abstraction width extend to visible region, and has the good characteristics such as chemical stability is high, acid and alkali-resistance, resistance to photoetch, but up to now, relevant α-Fe 2o 3the research of the preparation of/ZnO compound and photocatalysis performance thereof is also little.(the ZnO/Fe such as domestic Zhou Zhen 2o 3photocatalytic Degradation of Phenol. Yulin Teachers College's journal (natural science), 2011,32 (5): 69-72) adopt infusion process by ZnO load at Fe 2o 3on, prepare the ZnO/Fe of a series of different quality percentage 2o 3composite photo-catalyst, confirms to take incandescent lamp as light source simultaneously, and when phenol is for degraded object, ZnO load capacity is the ZnO/Fe of 3% 2o 3composite photo-catalyst activity is the highest.(the PreparationandphotocatalyticactivityofZnO/Fe such as Liu 2o 3nanotubecomposites.MaterialsScienceandEngineeringB, 2015,194:9-13) apply photochemical precipitation method by Fe 2o 3be deposited on ZnO nanorod surface prepared by hydrothermal reaction at low temperature and obtain ZnO/Fe 2o 3nanotube, the made ZnO/Fe of optimum reaction condition in same time 2o 3the efficiency of nano pipe photochemical catalyst degradation of methylene blue is close to 2 times of ZnO nanorod.(the AqueoussynthesisandenhancedphotocatalyticactivityofZnO/F e such as Achouri 2o 3heterostructures.JournalofPhysicsandChemistryofSolids, 2014,75 (10): 1081-1087) by impelling FeCl 3znO/Fe has been obtained in the mode of nano-ZnO surface hydrolysis 2o 3heterojunction structure, and find that its salicylic activity of degrading under ultraviolet lighting is apparently higher than commercial ZnO.It is different from these three kinds of methods, deng (PhotocatalyzedmineralizationofkraftblackliquoronZnO/Fe 2o 3coupledsemiconductor.EnvironmentalTechnology, 2002,23 (8): 955-959) directly to ZnO and Fe 2o 3powder carries out mechanical mixture and obtains ZnO/Fe 2o 3couple semiconductor, in its photocatalytic degradation black liquid, organic experimental result shows, mineralization rate is with ZnO/Fe 2o 3the increase (0.5 → 0.7) of ratio is constantly risen.Although support type α-Fe 2o 3/ ZnO is compared with the ZnO/Fe obtained through mechanical mixture 2o 3coupling body is more conducive to playing ZnO-Fe 2o 3between cooperative effect, but there is secondary preparation and the higher problem of cost.Therefore, find one both simple economies, can ZnO and Fe be ensured again 2o 3between interactional α-Fe 2o 3/ ZnO composite photo-catalyst preparation method meaning clearly.
Summary of the invention
One is the object of the present invention is to provide to prepare sheet α-Fe 2o 3the method of/ZnO composite photo-catalyst, the method reaction raw materials is few, technique is simple, mild condition, reaction time are short, environmentally safe, is a kind of green synthesis process, easily realizes industrialization.Obtained catalyst prod can under ultraviolet-visible illumination condition effective degradable organic pollutant, can be used for wastewater treatment.
In order to realize foregoing invention object, the technical solution adopted in the present invention is as follows:
The present invention includes following step:
Step one: the preparation of reaction precursor liquid: under agitation, first drips aqueous slkali, then drips zinc solution in ferric salt solution, after dropwising, continues to be stirred to mixed liquor in the muddy state comprising bronzing material;
Wherein the mol ratio of trivalent iron salt, alkali and zinc salt is (1 ~ 10): 90: 10;
Step 2: ageing: the glass container that reaction precursor liquid is housed is immersed ageing to container bottom in the water-bath of 80 ~ 99 DEG C and be covered with precipitation and reactant liquor change clarification, through suction filtration, washing, naturally dry, obtain α-Fe 2o 3/ ZnO composite photo-catalyst.
As to further restriction of the present invention, described in step one of the present invention, trivalent iron salt is selected from ferric nitrate, iron chloride or ferric sulfate; The molar concentration of the described trivalent iron salt aqueous solution is 0.5 ~ 2molL -1.
As to further restriction of the present invention, trivalent iron salt described in step one of the present invention is ferric nitrate; The molar concentration of described iron nitrate aqueous solution is 1molL -1.
As to further restriction of the present invention, described in step one of the present invention, alkali is selected from NaOH, potassium hydroxide or ammoniacal liquor; The molar concentration of described aqueous slkali is 2 ~ 6molL -1.
As to further restriction of the present invention, alkali described in step one of the present invention is NaOH; The molar concentration of described sodium hydrate aqueous solution is 4molL -1.
As to further restriction of the present invention, described in step one of the present invention, zinc salt is selected from zinc nitrate, zinc chloride, zinc acetate or zinc sulfate; The molar concentration of described zinc salt solution is 0.5 ~ 2molL -1.
As to further restriction of the present invention, zinc salt described in step one of the present invention is zinc nitrate; The molar concentration of described zinc nitrate aqueous solution is 1molL -1.
Good effect of the present invention is: the present invention adopts low temperature maturation method one step to prepare α-Fe 2o 3/ ZnO composite photo-catalyst, compared to first preparing α-Fe 2o 3or ZnO synthesizes α-Fe again 2o 3the two-step method of/ZnO compound and directly with pure α-Fe 2o 3, pure ZnO is the mechanical mixing of raw material, not only operating procedure is simple, reaction condition is gentle, energy consumption is little, can also give full play to α-Fe 2o 3and the cooperative effect between ZnO, is conducive to promoting when the large production of industrialization.
The present invention adopts low temperature maturation legal system for α-Fe 2o 3/ ZnO composite photo-catalyst, belongs to a kind of inorganic material synthetic method.Although the solvent used in the method is also water, still exists with the hydrothermal synthesis method of routine and necessarily to distinguish.The hydrothermal synthesis method of general routine prepares α-Fe 2o 3/ ZnO powder needs to use the particular device such as autoclave and Muffle furnace, and cost is higher, and during reaction, temperature is many between 100 ~ 240 DEG C, consumes energy also larger.And method use of the present invention is all simple glass instrument, water-bath used during ageing also non-precious equipment, and reaction temperature is no more than 100 DEG C, therefore relatively more simple, economical.
α-Fe prepared by the present invention 2o 3/ ZnO composite photo-catalyst, utilizes α-Fe on the one hand 2o 3with ZnO energy level difference therebetween, the energy gap of composite semiconductor is reduced, thus expand the scope of absorbing wavelength, improve the utilization rate to visible ray; α-Fe on the other hand 2o 3the electronics be excited in ZnO conduction band is also made to be easy to move to the lower α-Fe of energy level with ZnO energy level difference therebetween 2o 3on conduction band, make electronics and hole be in not jljl mutually in, extend electronics and hole life to a certain extent, reduce their recombination probability, improve the photocatalysis performance of composite semiconductor.In addition, α-Fe 2o 3the good characteristic of acid and alkali-resistance, resistance to photoetch more efficiently can improve resistance to acids and bases and the photostability of ZnO, realizes α-Fe 2o 3the repeatedly recycling of/ZnO composite photo-catalyst.
The present invention has groped α-Fe 2o 3the optimum proportioning of/ZnO composite photo-catalyst, both can utilize α-Fe 2o 3with the energy level difference between ZnO improves the photocatalytic activity of ZnO, can avoid again too much α-Fe 2o 3destroy α-Fe 2o 3dispersion on ZnO and/or because the position of ZnO valence band is lower than α-Fe 2o 3the position of valence band, the photohole that ZnO produces can be transferred to α-Fe 2o 3valence band in go, and make unnecessary α-Fe 2o 3become the complex centre in electronics and hole, so that affect the separative efficiency of photo-generate electron-hole, reduce α-Fe 2o 3the photocatalysis performance of/ZnO compound.
Accompanying drawing explanation
Fig. 1 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the XRD of/ZnO composite photo-catalyst characterizes collection of illustrative plates;
Fig. 2 is the FESEM phenogram of pure ZnO photocatalyst prepared by comparative example;
Fig. 3 is α-Fe prepared by embodiment 1 2o 3the FESEM phenogram of/ZnO composite photo-catalyst;
Fig. 4 is α-Fe prepared by embodiment 2 2o 3the FESEM phenogram of/ZnO composite photo-catalyst;
Fig. 5 is α-Fe prepared by embodiment 3 2o 3the FESEM phenogram of/ZnO composite photo-catalyst;
Fig. 6 is α-Fe prepared by embodiment 4 2o 3the FESEM phenogram of/ZnO composite photo-catalyst;
Fig. 7 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the UV-visDRS of/ZnO composite photo-catalyst characterizes collection of illustrative plates;
Fig. 8 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the time dependent curve of/ZnO composite photo-catalyst photocatalytic degradation pentachlorophenol efficiency;
Fig. 9 is α-Fe prepared by embodiment 3 2o 3/ ZnO composite photo-catalyst reuse situation.
In the accompanying drawings, a is pure ZnO photocatalyst powder prepared by comparative example, and b is α-Fe prepared by embodiment 1 2o 3/ ZnO composite photo-catalyst powder, c is α-Fe prepared by embodiment 2 2o 3/ ZnO composite photo-catalyst powder, d is α-Fe prepared by embodiment 3 2o 3/ ZnO composite photo-catalyst powder, e is α-Fe prepared by embodiment 4 2o 3/ ZnO composite photo-catalyst powder.
Detailed description of the invention
Embodiment 1
Get 1molL -1iron nitrate aqueous solution 2mL, in beaker, under magnetic stirring, first dropwise adds 4molL -1sodium hydrate aqueous solution 45mL, more dropwise add 1molL -1zinc nitrate aqueous solution 20mL (mol ratio of ferric nitrate, NaOH and zinc nitrate is 1: 90: 10).After dropwising, continue to stir 1h.This reaction precursor liquid is transferred in the conical flask of band grinding port plug, immerses and be warming up to ageing 5h in the water-bath of 80 DEG C in advance.Finally by suction filtration, distilled water washing 2 ~ 3 times, naturally dry, obtain α-Fe 2o 3/ ZnO composite catalyst.
Embodiment 2 ~ 6 and comparative example
Embodiment 2 ~ 6 and comparative example identical with the operating procedure of embodiment 1, difference is only the kind of trivalent iron salt used, alkali and zinc salt, concentration, the ratio of three and Aging Temperature, specifically as shown in table 1.
Table 1 embodiment 2 ~ 6 and comparative example
Aging Temperature in table 1 refers to the temperature being transferred to by reaction precursor liquid and being with and also immersing in the water-bath heated up in advance the water-bath of setting when carrying out ageing in the conical flask of grinding port plug.Under higher Aging Temperature, reacting phase is to comparatively fast, and the digestion time therefore needed is corresponding shorter; Under lower Aging Temperature, react relatively slow, the digestion time therefore needed is corresponding longer.When Aging Temperature is for limited 80 ~ 99 DEG C, reaction carry out comparatively thorough, and the used time is shorter, and obtained composite catalyst purity is also higher, so 80 ~ 99 DEG C of preferred Aging Temperature scopes that are the present invention.
Experimental example 1: the XRD of photochemical catalyst characterizes
Fig. 1 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the XRD of/ZnO composite photo-catalyst characterizes collection of illustrative plates.Can find out, 2 θ=24.1 °, 33.1 °, 35.6 °, 40.8 °, 49.4 °, 54.0 °, the diffraction maximum at 63.9 ° of places belongs to α-Fe 2o 3(JCPDSNo.33-0664), other diffraction maximums then all belong to ZnO (JCPDSNo.36-1451).Along with the increase of trivalent iron salt use amount, α-Fe in product 2o 3the intensity of characteristic diffraction peak increases gradually.Do not find other impurity peaks, illustrate that the purity of product is very high.
Experimental example 2: the FESEM of photochemical catalyst characterizes
Fig. 2 to Fig. 6 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the FESEM phenogram of/ZnO composite photo-catalyst.Can find out, pure ZnO particle (comparative example) is similar to spherical in shape or elliposoidal, and size scope is 36 ~ 108nm.α-Fe 2o 3the pattern of existence to ZnO create considerable influence, α-Fe 2o 3/ ZnO composite photo-catalyst particle (embodiment 1 ~ 4) is all in irregular sheet, and average thickness is about 25nm.
Experimental example 3: the UV-visDRS of photochemical catalyst characterizes
Fig. 7 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the UV-visDRS of/ZnO composite photo-catalyst characterizes collection of illustrative plates.Compared with the pure ZnO (comparative example) that only can absorb ultraviolet light, α-Fe 2o 3/ ZnO composite photo-catalyst (embodiment 1 ~ 4) all has response at Uv and visible light district (300 ~ 800nm), and along with α-Fe 2o 3the rising of content, α-Fe 2o 3the red shift degree of/ZnO composite photo-catalyst Absorption edge increases gradually.
Experimental example 4: the ultraviolet-visible photocatalysis performance of photochemical catalyst
100mL pentachlorophenol solution (10mgL is added in beaker -1, pH9 ~ 10) and the photochemical catalyst powder prepared of 0.1g comparative example or embodiment 1 ~ 4, lucifuge strong stirring 30min, makes pentachlorophenol reach adsorption-desorption balance at catalyst surface.Then under magnetic stirring, 500W xenon lamp is adopted to irradiate (light source and liquid level vertical range are 12cm) and start timing.Interval samples, and centrifugation, supernatant liquor, through filtering with microporous membrane, measures it at pentachlorophenol maximum absorption wavelength (λ with ultraviolet-visible spectrophotometer max=220nm) absorbance at place, and the degradation rate (η) of pentachlorophenol is calculated according to following formula:
η＝(A 0-A t)/A 0×100％
In formula: A 0for the absorbance of pentachlorophenol solution before illumination; A tfor the absorbance of pentachlorophenol solution after light application time t.
Fig. 8 is α-Fe prepared by the pure ZnO photocatalyst prepared of comparative example and embodiment 1 ~ 4 2o 3the time dependent curve of/ZnO composite photo-catalyst photocatalytic degradation pentachlorophenol efficiency.Blank assay result shows, and after xenon lamp irradiates 300min, the degradation rate of pentachlorophenol is only 18.30%, and this phenomenon is the selfdecomposition of pentachlorophenol.While xenon lamp irradiates, add catalyst, then the degradation rate of pentachlorophenol significantly improves.The degradation effect of embodiment 1 ~ 4 is all better than the degradation effect of comparative example, and α-Fe 2o 3when being 4: 10 with the mol ratio of ZnO, α-Fe 2o 3/ ZnO composite photo-catalyst (embodiment 3) shows the highest photocatalytic activity, and in 300min, pentachlorophenol is almost completely degraded.
The catalyst powder photocatalytic degradation pentachlorophenol that table 2 is prepared for embodiment 1 ~ 6 and comparative example is to degradation rate data during 300min.Result shows, as α-Fe 2o 3α-Fe in/ZnO compound 2o 3when being 1: 10 ~ 10: 10 with the mol ratio of ZnO, the purer ZnO of degradation effect (comparative example) of compound (embodiment 1 ~ 6) is improved; But α is-Fe 2o 3content not more high better, α-Fe 2o 3with the mol ratio of ZnO more than 4: 10 after, the catalytic efficiency of compound decreases on the contrary.
Catalyst powder photocatalytic degradation pentachlorophenol prepared by table 2 embodiment 1 ~ 6 and comparative example is to degradation rate during 300min
Experimental example 5: photochemical catalyst reuse situation
To used α-Fe 2o 3with the α-Fe that ZnO mol ratio is 4: 10 2o 3/ ZnO compound carries out filtered and recycled, fully washs absorption impurity in its surface, again carry out photocatalysis performance test after naturally drying under the same terms with ethanol.
Fig. 9 is α-Fe prepared by embodiment 3 2o 3/ ZnO composite photo-catalyst reuse situation.Can find out, when this photochemical catalyst reuses the 1st time, activity decrease is obvious, but from the 2nd time, activity decrease trend slows down, and when reusing the 3rd time, the degradation rate of pentachlorophenol still remains on more than 80%.This shows, α-Fe 2o 3/ ZnO composite photo-catalyst has good repeat performance.

Claims (7)

1. a sheet α-Fe 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that it comprises the steps:
Step one: the preparation of reaction precursor liquid: under agitation, first drips aqueous slkali, then drips zinc solution in ferric salt solution, after dropwising, continues to be stirred to mixed liquor in the muddy state comprising bronzing material;
Wherein the mol ratio of trivalent iron salt, alkali and zinc salt is (1 ~ 10): 90: 10;
Step 2: ageing: the glass container that reaction precursor liquid is housed is immersed ageing to container bottom in the water-bath of 80 ~ 99 DEG C and be covered with precipitation and reactant liquor change clarification, through suction filtration, washing, naturally dry, obtain α-Fe 2o 3/ ZnO composite photo-catalyst.
2. a kind of sheet α-Fe according to claim 1 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that trivalent iron salt described in step one is selected from ferric nitrate, iron chloride or ferric sulfate;
The molar concentration of the described trivalent iron salt aqueous solution is 0.5 ~ 2molL -1.
3. a kind of sheet α-Fe according to claim 2 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that trivalent iron salt described in step one is ferric nitrate; The molar concentration of described iron nitrate aqueous solution is 1molL -1.
4. a kind of sheet α-Fe according to claim 1 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that alkali described in step one is selected from NaOH, potassium hydroxide or ammoniacal liquor;
The molar concentration of described aqueous slkali is 2 ~ 6molL -1.
5. a kind of sheet α-Fe according to claim 4 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that alkali described in step one is NaOH; The molar concentration of described sodium hydrate aqueous solution is 4molL -1.
6. a kind of sheet α-Fe according to claim 1 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that zinc salt described in step one is selected from zinc nitrate, zinc chloride, zinc acetate or zinc sulfate;
The molar concentration of described zinc salt solution is 0.5 ~ 2molL -1.
7. a kind of sheet α-Fe according to claim 6 2o 3the preparation method of/ZnO composite photo-catalyst, is characterized in that zinc salt described in step one is zinc nitrate; The molar concentration of described zinc nitrate aqueous solution is 1molL -1.
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CN107626315A (en) * 2017-10-23 2018-01-26 烟台智本知识产权运营管理有限公司 A kind of preparation method of the ZnO photocatalyst of Fe doping
CN108435186A (en) * 2018-04-28 2018-08-24 河北科技大学 A kind of α-Fe2O3- ZnO/ gangue composite photo-catalysts and its preparation method and application
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CN107626315A (en) * 2017-10-23 2018-01-26 烟台智本知识产权运营管理有限公司 A kind of preparation method of the ZnO photocatalyst of Fe doping
CN108435186A (en) * 2018-04-28 2018-08-24 河北科技大学 A kind of α-Fe2O3- ZnO/ gangue composite photo-catalysts and its preparation method and application
CN108636416A (en) * 2018-04-28 2018-10-12 河北科技大学 A kind of ZnO/ gangues composite photo-catalyst and its preparation method and application
CN108686656A (en) * 2018-04-28 2018-10-23 河北科技大学 A kind of α-Fe2O3/ gangue composite photo-catalyst and its preparation method and application
CN108435186B (en) * 2018-04-28 2021-02-05 河北科技大学 alpha-Fe2O3-ZnO/coal gangue composite photocatalyst and preparation method and application thereof
CN108686656B (en) * 2018-04-28 2021-04-13 河北科技大学 alpha-Fe2O3Coal gangue composite photocatalyst and preparation method and application thereof
CN108636416B (en) * 2018-04-28 2021-04-13 河北科技大学 ZnO/coal gangue composite photocatalyst and preparation method and application thereof
CN108671919A (en) * 2018-05-14 2018-10-19 攀枝花学院 Unformed shape photochemical catalyst and preparation method thereof

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Application publication date: 20151230