CN106345496B - A kind of compound semiconductor photocatalytic material and preparation method thereof - Google Patents
A kind of compound semiconductor photocatalytic material and preparation method thereof Download PDFInfo
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- CN106345496B CN106345496B CN201510419675.4A CN201510419675A CN106345496B CN 106345496 B CN106345496 B CN 106345496B CN 201510419675 A CN201510419675 A CN 201510419675A CN 106345496 B CN106345496 B CN 106345496B
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- biobr
- bivo
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Abstract
The present invention provides a kind of compound semiconductor photocatalytic materials and preparation method thereof.This method first uses hydro-thermal method to synthesize BiOBr and BiVO4, then use supercritical ultrasonics technology by BiOBr and BiVO again4Mix preparation BiOBr/BiVO4Compound semiconductor photocatalytic material.Method of the invention has many advantages, such as easy to operate, pollution-free, at low cost, can be mass-produced.Prepared composite semiconductor catalysis material has large specific surface area, is uniformly dispersed, the visible light response activity that stability is good, high, while having good degradation property to organic dyestuff rhodamine B.
Description
Technical field
The present invention relates to a kind of compound semiconductor photocatalytic materials and preparation method thereof, belong to new material and environment protection field.
Background technique
With the continuous development of scientific and technological progress and society, environment and energy problem are got worse.Catalysis material can be
Under conditions of illumination, Organic Hazardous Compounds in effective dirty water and air of degrading generate H2O and CO2, reach the function of decontamination environmental protection
Energy.Traditional catalysis material is mainly with TiO2Based on, the forbidden bandwidth of this kind of catalysis material is larger, and can only be in purple
The irradiation of outer light issues third contact of a total solar or lunar eclipse catalytic effect, this undoubtedly limits its application.
Summary of the invention
And bismuth based material has a lesser forbidden bandwidth, and can under the action of visible light degradation of organic substances matter, to real
Border application provides bigger space.Therefore again in addition to titanium based material other than, study more a kind of catalysis material.So
And single bismuth based material can lead to the drop of photocatalytic activity because of the higher recombination rate of photo-generate electron-hole pairs of generation
It is low.In order to improve the activity of catalysis material, two kinds of different semiconductors couplings are selected, form heterojunction structure on its contact surface,
It will be helpful to the separation of photo-generate electron-hole pair, reduce recombination rate, improve photocatalysis efficiency.
BiOBr and BiVO4There is certain photocatalytic activity under visible light.But single BiOBr and BiVO4Due to compared with
The recombination rate of high photo-generate electron-hole pair, photocatalytic activity are very limited.
Summary of the invention
The purpose of the present invention is to provide a kind of compound semiconductor photocatalytic materials.
Another object of the invention is to provide the preparation method of above-mentioned compound semiconductor photocatalytic material.
Above-mentioned purpose of the present invention is achieved by the following technical programs.
Key problem in technology of the invention is that hydro-thermal method synthesizes BiOBr and BiVO4, and by the BiOBr synthesized and BiVO4
In ethanol, ultrasonic treatment is uniform to mixture for mixing, then dries to get uniformly mixed BiOBr/BiVO4It is compound partly to lead
Body catalysis material.
To achieve the above object, the technical solution adopted by the present invention is.
A kind of BiOBr/BiVO is provided4Compound semiconductor photocatalytic material.Using CTAB as bromine source, Bi (NO3)3·5H2O is
Synthesis BiOBr is sent out using hydro-thermal in bismuth source；With NH4VO3It is used as promotor, Bi (NO simultaneously as vanadium source3)3·5H2O is bismuth source, water
Thermal method synthesizes BiVO4；Using ethyl alcohol as medium, BiOBr and BiVO4It is mixed in a certain ratio, after ultrasonication, obtains
BiOBr/BiVO4Compound semiconductor photocatalytic material.
In the synthesis process of the BiOBr, Bi (NO3)3·5H2The mass ratio of O and CTAB is 1:2 ~ 1:3, synthesis temperature
Be 140 DEG C ~ 160 DEG C, the reaction time be 12 ~ for 24 hours.
The BiVO4Synthesis process in, NH4VO3With Bi (NO3)3·5H2The ratio between amount of substance of O is 1:2 ~ 1:4.Instead
Answering temperature is 70 ~ 90oC, the reaction time be 12 ~ for 24 hours.
The present invention prepares the BiOBr/BiVO of different proportion4, it is expressed as BiOBr/BiVO4- xx, ratio 1:0,2:3,1:
1,3:2,0:1 are expressed as BiOBr, BiOBr/BiVO4-60、BiOBr/BiVO4-50、BiOBr/BiVO4-40、BiVO4。
Above-mentioned catalysis material being capable of degradable organic pollutant under visible light.
The present invention has the advantages that
1) preparation process of catalysis material shown in is simple, easily operated, pollution-free；
2) in the catalysis material preparation process described in, select ethyl alcohol as BiOBr and BiVO4Mixes liquid environment,
Be conducive to rapid draing, substance is prevented from caking, has saved the energy；
3) in the catalysis material preparation process described in, BiOBr and BiVO are made by ultrasonication4It is uniformly mixed,
The reunion for reducing substance, improves specific surface area；
4) catalysis material described in, narrowed semiconductor forbidden bandwidth, enhances response of the catalyst to visible light, mentions
High photocatalysis efficiency；
5) catalysis material described in after degradation of contaminant, will not generate secondary pollution, and catalyst easily with solution point
From stability is good, convenient for recycling, has saved cost, can industrialized production.
Detailed description of the invention
Fig. 1 is BiOBr, BiVO4、BiOBr/BiVO4SEM figure and BiOBr/BiVO4TEM figure.
Fig. 2 is BiOBr, BiVO4、BiOBr/BiVO4UV-Vis diffuse spectrogram.
Fig. 3 is BiOBr/BiVO4Composite photocatalyst material is in visible light (300W tungsten halogen lamp, 400nm end filter plate)
Irradiate the effect picture of lower rhodamine B degradation.The result shows that BiOBr/BiVO4The degradation effect of -50 pairs of organic pollutant rhodamine Bs
It is best.
Fig. 4 is BiOBr/BiVO4Composite photocatalyst material recycles 15 degradation figures to rhodamine B.
Specific embodiment
Catalysis material of the invention is described below with reference to specific example, this example is served only for further illustrating,
Rather than limiting the invention.
Embodiment 1:
Prepare BiOBr photochemical catalyst.By a certain amount of Bi (NO3)3·5H2O is dissolved in 10mL straight alcohol, forms solution
Cetyl trimethylammonium bromide (CTAB) is slowly added into A by A, is stirred and is formed precursor B after ultrasonication, (Bi
(NO3)3·5H2The mass ratio of O and CTAB is 1:2 ~ 1:3).B is transferred in the autoclave of 50mL teflon lined, body
Product compactedness 80%.Autoclave is sealed, heating temperature is 140 ~ 160 DEG C, the reaction time 12 ~ for 24 hours.After reaction be centrifuged, wash 2 ~
3 times, dry 8h, obtains BiOBr powder in 60 DEG C of baking ovens.
Embodiment 2:
Prepare BiVO4Photochemical catalyst.NH4VO3It is dissolved in 20mL deionized water, is put into 96 DEG C of insulating box after 20min
Form solution C.Bi(NO3)3•5H2O, which is added in 20mL deionized water, obtains solution D, wherein NH4VO3With Bi(NO3)3•5H2The matter of O
The ratio between amount is 1:2 ~ 1:4, and solution D is slowly dropped in C, forms presoma E.Then E is transferred in flask, regulating thermostatic
Water-bath reacts 12h to 70 ~ 90 DEG C.After centrifugation, washing, it is put into 60 DEG C of insulating boxs dry 5h, obtains BiVO4。
Embodiment 3:
Prepare BiOBr/BiVO4Photochemical catalyst.The BiOBr and BiVO that above-described embodiment 1 and embodiment 2 are obtained4By 2:3
It is added in ethyl alcohol, then ultrasonication 30min, after mixing, is put into 60 DEG C of insulating boxs dry 2h, obtains BiOBr/
BiVO4- 60 composite photo-catalysts.
Embodiment 4
In above-described embodiment 3, in addition to proportion changes 1:1 into, other conditions are constant, and BiOBr/BiVO is made4- 50 is compound
Photochemical catalyst.
Embodiment 5
In above-described embodiment 3, in addition to proportion changes 3:2 into, other conditions are constant, and BiOBr/BiVO is made4- 40 is compound
Photochemical catalyst.
Claims (1)
1. a kind of compound semiconductor photocatalytic material, which is characterized in that the compound semiconductor photocatalytic material is first to synthesize
BiOBr and BiVO out4, then using ethyl alcohol as medium ultrasonication BiOBr and BiVO4Mixture to being uniformly mixed to get
BiOBr/BiVO4Compound semiconductor photocatalytic material, the ultrasonic treatment time are 30min；
The preparation method includes the following steps:
(1) preparation of BiOBr: by Bi (NO3)3·5H2O is added in ethanol in proper amount, stirs evenly, and certain mass ratio is then added
CTAB cetyl trimethylammonium bromide into above-mentioned solution, obtain presoma；Presoma is transferred to polytetrafluoroethylene (PTFE) lining
In autoclave in, after heating reaction a period of time, centrifugation, washing are put into insulating box dry 8h, obtain BiOBr, Bi
(NO3)3·5H2The mass ratio of O and CTAB is 1:2~1:3, and heating temperature is 140~160 DEG C, the reaction time 12~for 24 hours；
(2)BiVO4Preparation: by a certain amount of NH4VO3Dissolution in deionized water, is put into 96 DEG C of insulating box after 20min
Obtain solution A；By the Bi (NO of certain mass ratio3)3·5H2O, which is added in deionized water, obtains substance B；Gained B is slowly dropped to
C is obtained in solution A；Then C is transferred in flask, regulating thermostatic water bath temperature, after reacting a period of time, washing, centrifugation,
It is then placed in 60 DEG C of insulating boxs dry 5h, obtains BiVO4, NH4VO3With Bi (NO3)3·5H2The mass ratio of O is 1:2~1:
4, water bath temperature is 70~90 DEG C, reaction time 12h；
(3)BiOBr/BiVO4Preparation: by BiVO obtained in BiOBr obtained in (1) and (2)4It mixes according to a certain percentage
It is combined, ethanol in proper amount is added, ultrasonic treatment is then placed in 2h in 60 DEG C of insulating boxs, obtains BiOBr/BiVO4It is compound partly to lead
Body catalysis material；
BiOBr and BiVO described in step (3)4Ratio be 1:1.
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| CN109092334B (en) * | 2018-08-23 | 2021-02-12 | 辽宁石油化工大学 | Visible light response BiOBr/CeVO4Preparation of heterojunction and application thereof |
| CN111186857B (en) * | 2020-01-15 | 2022-05-17 | 杭州电子科技大学 | Preparation method of BiOBr nano material |
| CN113522319B (en) * | 2021-07-05 | 2023-07-11 | 北京建筑大学 | Preparation method and application of catalytic material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101791548A (en) * | 2010-04-22 | 2010-08-04 | 华中科技大学 | Visible light catalyst BiVO4 and preparation method thereof |
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| CN101244385A (en) * | 2008-03-20 | 2008-08-20 | 同济大学 | Process for producing high-efficiency photocatalysis material |
| CN104772134B (en) * | 2015-03-31 | 2017-01-18 | 浙江师范大学 | Method for massively preparing mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst |
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Non-Patent Citations (6)
| Title |
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| "BiVO4纳米阵列在量子点太阳电池中的应用";李毅;《第13届中国光伏大会》;20140609;第436页 |
| "Preeminent visible-light photocatalytic activity over BiOBr–BiVO4 heterojunctions";F. P. Cao et al;《cryst. Res. Technol.》;20141205;第49卷;第933-938页 |
| "Surface modification of m-BiVO4 with wide band-gap semiconductor BiOCl to largely improve the visible light induced photocatalytic activity";Jing cao et al;《Applied Surface Science》;20130726;第284卷;第263-269页 |
| "The Enhanced Photocatalytic Properties of BiOCl_BiVO4 p-n Heterojunctions via Plasmon Resonance of Metal Bi";Chenchen Feng et al;《RSC Advances》;20131231;第1-3卷;第1-6页 |
| "新型可见光催化剂BiVO4的制备与研究";刘宏伟;《万方数据知识服务平台》;20120426;全文 |
| "新型可见光催化剂BiVO4的制备方法";刘宏伟;《材料导报》;20111231;第S1卷;第54-58页 |
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