CN104722293A - Visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and preparation method thereof - Google Patents

Visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and preparation method thereof Download PDF

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CN104722293A
CN104722293A CN201510054272.4A CN201510054272A CN104722293A CN 104722293 A CN104722293 A CN 104722293A CN 201510054272 A CN201510054272 A CN 201510054272A CN 104722293 A CN104722293 A CN 104722293A
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visible light
bi2wo6
bi2o3
heterojunction photocatalyst
responded
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张凤君
王天野
钟爽
肖国生
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Jilin University
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Jilin University
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Abstract

The invention relates to a visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and a preparation method thereof. The visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst is prepared from the following components in parts by weight: sodium oleate, an ethanediol solution, bismuth nitrate, sodium tungstate and a carrier. The preparation method is simple and the operation is simple and convenient; preparation conditions are moderate and are free from toxin and secondary pollution is not caused in a preparation process; the batch production can be realized; the prepared visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst has a high visible light absorption capability, has strong light absorption property and strong organic matter light degradation capability in a visible light region, and has a good application prospect of degrading RhB under the visible light; and particularly, the degradation rate of rhodamine B can be up to 99.5% under the condition of illuminating for 90 minutes under visible light with the wavelength more than nm. The prepared composite photocatalyst is convenient to recycle and reuse, and the difficulty that the recycling is difficult when a photocatalysis technology is actually applied in environment purification can be solved.

Description

A kind of visible light-responded support type Bi 2wO 6/ Bi 2o 3heterojunction photocatalyst and preparation method
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method, especially visible light-responded support type Bi 2wO 6/ Bi 2o 3heterojunction photocatalyst, particularly Bi 2wO 6/ Bi 2o 3/ graphene composite photocatalyst and Bi 2wO 6/ Bi 2o 3/ scoria composite photo-catalyst and preparation method, and the application of their rhodamine B degradations under visible light illumination.
Background technology
Bismuth tungstate is considered to one of semiconductor catalyst in bismuth-based oxide with best visible light catalysis activity, receives the extensive concern of scholars in recent years.But the restriction of the quick compound right due to photo-generate electron-hole and the factor such as visible light-responded scope is narrower, inhibits the visible light catalysis activity of single bismuth tungstate catalyst.Therefore, to single Bi 2wO 6carry out modifying and modification remains to improve its photocatalytic activity under visible light the main flow direction that bismuth series catalysts studies.
Construct Bi 2wO 6hetero-junctions, is considered to the effective ways improving its photocatalytic activity.Utilization can make the semiconductor Existential Space electrical potential difference of crystal boundary close contact with overlap effect, its internal electric field can impel photo-generated carrier to move to another kind of semiconductor energy level from a kind of semiconductor energy level as driving force, thus widens Bi 2wO 6visible absorption scope, suppress the right combined efficiency of photo-generate electron-hole, reach the effect strengthening photocatalytic activity.Due to Bi 2wO 6typical n-type semiconductor, and Bi 2o 3typical p-type semiconductor, can to Bi 2wO 6and Bi 2o 3carry out semiconductors coupling, construct typical p-n heterojunction type semiconductor catalyst.In recent years, people start to pay close attention to synthesis Bi 2wO 6/ Bi 2o 3the best approach of hetero-junctions, makes it have higher visible light-responded and stronger visible light catalysis activity, and has carried out large quantifier elimination to it, such as, synthesized Bi by microwave hydrothermal method, a step solution combustion method and two step solwution methods 2wO 6/ Bi 2o 3, also someone utilizes polystyrene particle to synthesize Bi as template by hydro-thermal-roasting method 2wO 6/ Bi 2o 3hollow microsphere.But these synthetic method relative complex reported, are applicable to laboratory synthesis preparation more, be not suitable for actual industrial production to synthetic method high yield, easy requirement.
Meanwhile, the problem of solidification of catalysis material is also one of maximum bottleneck in catalyst environment purification applications.In preparation nanometer luminescent material, wish that reducing particle size increasing specific surface area obtains better photocatalytic activity on the one hand; Granule is in open heterogeneous reaction system on the other hand, such as, in the liquid and gas reaction of Open Dynamic environmental system, must consider the recovery problem of catalyst.The separation that nano particle catalysis material is directly applied in liquid phase suspension system small particles is a complicated job, during energy charge, and particle is easily reunited, thus reduce the photocatalytic activity of catalysis material, thus the practical application of photocatalysis technology in depollution of environment field is reduced.Therefore, be a problem urgently to be resolved hurrily by catalysis material immobilization in photocatalysis depollution of environment scale application.
Summary of the invention
Object of the present invention is just for above-mentioned the deficiencies in the prior art, provides a kind of visible light-responded support type Bi 2wO 6/ Bi 2o 3heterojunction photocatalyst;
Another object of the present invention is to provide a kind of visible light-responded support type Bi 2wO 6/ Bi 2o 3heterojunction photocatalyst preparation method;
Another object of the present invention is the application of rhodamine B degradation under visible light illumination.
The object of the invention is to be achieved through the following technical solutions:
A visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, its component has following raw materials according to make by mass fraction:
Described carrier is scoria or Graphene, wherein scoria 4.0g-6.0g, Graphene 0.04g-0.06g.
A preparation method for visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, comprises the following steps:
Under A room temperature, 1.0g-1.5g enuatrol is dissolved in 30ml-50ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g-2.1g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.5g-0.8g sodium tungstate and is dissolved in 20ml-30ml ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 0.04g-0.06g Graphene or 4.0g-6.0g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
Can be used in the rhodamine B degraded of nm level wavelength under visible light illumination.
Beneficial effect: preparation method of the present invention is simple, easy and simple to handle, preparation condition moderate notoxic, preparation process non-secondary pollution, be applicable to batch production; Support type Bi prepared by the present invention 2wO 6/ Bi 2o 3heterojunction composite photocatalyst has high visible absorption ability, strong in visible region light absorption, light degradation organic matter ability, the RhB that degrades under visible light has good application prospect, specifically, under wavelength > nm visible ray, irradiate the degradation rate of rhodamine B under 90min minute condition reach 99.5%.Composite photo-catalyst prepared by the present invention is convenient to recovery and reuse, solves the difficult problem that photocatalysis technology reclaims difficulty in depollution of environment practical application.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 preparation Bi 2wO 6/ Bi 2o 3hetero-junctions catalyst and Bi 2wO 6xRD figure;
Fig. 2 is Bi 2wO 6/ Bi 2o 3hetero-junctions catalyst and Bi 2wO 6sEM figure, (a) Bi 2wO 6/ Bi 2o 3, (b) Bi 2wO 6;
Fig. 3 is Bi 2wO 6/ Bi 2o 3hetero-junctions catalyst and Bi 2wO 6uV-Vis diffuse reflection spectroscopy;
Fig. 4 is Bi 2wO 6/ Bi 2o 3hetero-junctions catalyst is to RhB photocatalytic degradation efficiency comparison diagram;
Fig. 5 is Bi 2wO 6/ Bi 2o 3the ultraviolet-visible spectrum of hetero-junctions catalyst degradation RhB;
Fig. 6 is Bi 2wO 6/ Bi 2o 3the XRD figure of/scoria composite catalyst;
Fig. 7 is Bi 2wO 6/ Bi 2o 3the SEM collection of illustrative plates of/scoria composite catalyst, (a)-(c) scoria, scoria after (d)-(h) load;
Fig. 8 is Bi 2wO 6/ Bi 2o 3/ scoria composite catalyst is to RhB photocatalytic degradation efficiency comparison diagram;
Fig. 9 is Bi 2wO 6/ Bi 2o 3the ultraviolet-visible light spectrogram of/scoria composite catalyst degraded RhB;
Figure 10 is Bi 2wO 6/ Bi 2o 3the XRD figure of/graphene composite catalyst;
Figure 11 is Bi 2wO 6/ Bi 2o 3the SEM figure spectrogram of/graphene composite catalyst;
Figure 12 is Bi 2wO 6/ Bi 2o 3the UV-Vis diffuse reflection spectroscopy figure of/graphene composite catalyst
Figure 13 is Bi 2wO 6/ Bi 2o 3/ graphene composite catalyst is to RhB photocatalytic degradation efficiency comparison diagram
Figure 14 is Bi 2wO 6/ Bi 2o 3the ultraviolet-visible spectrogram of/graphene composite catalyst degraded RhB
Detailed description of the invention
Below in conjunction with accompanying drawing and example, the invention will be further described, but the present invention is not limited only to this.
A visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, its component has following raw materials according to make by mass fraction:
Described carrier is scoria or Graphene, wherein scoria 4.0g-6.0g, Graphene 0.04g-0.06g.
A preparation method for visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, comprises the following steps:
Under A room temperature, 1.0g-1.5g enuatrol is dissolved in 30ml-50ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g-2.1g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.5g-0.8g sodium tungstate and is dissolved in 20ml-30ml ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 0.04g-0.06g Graphene or 4.0g-6.0g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
Can be used in the rhodamine B degraded of nm level wavelength under visible light illumination.
Embodiment 1
Bi 2wO 6/ Bi 2o 3the preparation method of heterojunction photocatalyst
Under A room temperature, 1.22g enuatrol is dissolved in 40.00Ml ethylene glycol solution and makes mixed liquor;
B adds 1.94g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.66g sodium tungstate and is dissolved in 30.00mL ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 5g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
As Fig. 1, the Bi of preparation 2wO 6/ Bi 2o 3the XRD diffraction maximum of hetero-junctions catalyst divides not only corresponding rhombic Bi 2wO 6(JCPDS No.39-0256) PDF standard card, simultaneously also with Emission in Cubic Bi 2o 3(JCPDS 76-2478) PDF standard card is corresponding;
As can be seen from Figure 2, the Bi of preparation 2wO 6/ Bi 2o 3hetero-junctions catalyst is Nano microsphere shape, have evenly, less particle diameter;
As can be seen from Figure 3, the Bi of preparation 2wO 6/ Bi 2o 3heterojunction photocatalyst has better visible light-responded, and in 20min, degradation rate reaches 99.6%.
Embodiment 2
Bi 2wO 6/ Bi 2o 3the preparation method of heterojunction photocatalyst
Under A room temperature, 1.0g enuatrol is dissolved in 40.00Ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.60g sodium tungstate and is dissolved in 20.00mL ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 5.5g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
Embodiment 3
Bi 2wO 6/ Bi 2o 3the preparation method of heterojunction photocatalyst
Under A room temperature, 1.5g enuatrol is dissolved in 50.00Ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.80g sodium tungstate and is dissolved in 30.00mL ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 6.0g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
Embodiment 4
Bi 2wO 6/ Bi 2o 3the preparation method of heterojunction photocatalyst
Under A room temperature, 1.22g enuatrol is dissolved in 40.00Ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.66g sodium tungstate and is dissolved in 20.00mL ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 0.05g Graphene, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, can prepare visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, in 90min, degradation rate reaches 98.91%.
Embodiment 5
Bi 2wO 6/ Bi 2o 3the preparation method of heterojunction photocatalyst
Under A room temperature, 1.5g enuatrol is dissolved in 40.00Ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.70g sodium tungstate and is dissolved in 30.00mL ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 0.06g Graphene, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.

Claims (5)

1. a visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, it is characterized in that, its component is made up by mass fraction of following raw materials according:
Enuatrol 1.0g ~ 1.5g
Ethylene glycol solution 20ml ~ 80ml
Bismuth nitrate 1.90g ~ 2.1g
Sodium tungstate 0.5g ~ 0.8g
Carrier 0.04g-6.0g.
2., according to visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst according to claim 1, it is characterized in that, described carrier is scoria or Graphene, wherein scoria 4.0g-6.0g, Graphene 0.04g-0.06g.
3. a preparation method for visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst, is characterized in that, comprise the following steps:
Under A room temperature, 1.0g-1.5g enuatrol is dissolved in 30ml-50ml ethylene glycol solution and makes mixed liquor;
B adds 1.90g-2.1g bismuth nitrate in mixed liquor, is uniformly mixed solution to clear;
C gets 0.5g-0.8g sodium tungstate and is dissolved in 20ml-30ml ethylene glycol solution, is then joined in step B mixed solution, continues stirring until CL;
D adds 0.04g-0.06g Graphene or 4.0g-6.0g scoria, continues to be stirred to mix;
E, the solution dislocation autoclave that will mix, add that charge is autoclave volume 80%, under 180 DEG C of conditions, heat 20h;
After F, autoclave Temperature fall to room temperature, take out the mixture of solid and solvent, wash residual organic carbon with ethanol and distilled water;
G, at 60 DEG C of temperature, dry 12h, visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst can be prepared.
4. according to visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst according to claim 1, it is characterized in that, can be used in the rhodamine B degraded of nm level wavelength under visible light illumination.
5. according to visible light-responded support type Bi2WO6/Bi2O3 heterojunction photocatalyst according to claim 1, it is characterized in that, 1 part of described enuatrol is (1.22g) 1.0g-1.5g, 4 parts of ethylene glycol solutions are (10.0mL), 0.8 mL-1.2 mL, 1 part of bismuth nitrate (1.94g) is 1.90g-2.0g, and 1 part of sodium tungstate is 0.66g, and 1 part of carrier is 0.04g-6.0g.
CN201510054272.4A 2015-02-02 2015-02-02 Visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and preparation method thereof Pending CN104722293A (en)

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CN106955699A (en) * 2016-01-11 2017-07-18 中国科学院上海硅酸盐研究所 A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof
CN107537466A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method of photochemical catalyst
CN107537467A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method of bismuth tungstate base heterojunction photochemical catalyst
CN107537468A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide
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CN108977975A (en) * 2018-07-25 2018-12-11 南京意西欧环境科技有限公司 It is a kind of can the low cost of recycled in its entirety administer black-odor river with pedaline and lawn and preparation method thereof
CN109078633A (en) * 2018-08-24 2018-12-25 西南交通大学 A kind of W doping Bi2O3The preparation method of nanostructure
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CN113198453A (en) * 2021-05-20 2021-08-03 陕西科技大学 Lamellar Bi2O2SiO3-Si2Bi24O40Heterogeneous composite photocatalyst and preparation method thereof
CN113231099A (en) * 2021-05-21 2021-08-10 吉林大学 Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst

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CN106955699A (en) * 2016-01-11 2017-07-18 中国科学院上海硅酸盐研究所 A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof
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CN107537468A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide
CN107537469A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method of bismuth tungstate Quito member heterojunction photocatalyst
CN107537466A (en) * 2016-06-27 2018-01-05 张家港市杨舍丝印工艺厂 A kind of preparation method of photochemical catalyst
CN106807361A (en) * 2017-02-28 2017-06-09 重庆工商大学 A kind of unformed bismuth tungstate bismuth oxide ternary organic composite photochemical catalyst of bismuth and preparation method
CN106807361B (en) * 2017-02-28 2019-02-15 重庆工商大学 A kind of unformed bismuth tungstate of bismuth-- bismuth oxide ternary organic composite photochemical catalyst and preparation method
CN110508272A (en) * 2018-05-22 2019-11-29 南京理工大学 The preparation method of the compound zero gap heterojunction photocatalyst of bismuth oxide/bismuth molybdate
CN110508272B (en) * 2018-05-22 2022-04-19 南京理工大学 Preparation method of bismuth oxide/bismuth molybdate composite zero-gap heterojunction photocatalyst
CN108977975A (en) * 2018-07-25 2018-12-11 南京意西欧环境科技有限公司 It is a kind of can the low cost of recycled in its entirety administer black-odor river with pedaline and lawn and preparation method thereof
CN109078633A (en) * 2018-08-24 2018-12-25 西南交通大学 A kind of W doping Bi2O3The preparation method of nanostructure
CN113198453A (en) * 2021-05-20 2021-08-03 陕西科技大学 Lamellar Bi2O2SiO3-Si2Bi24O40Heterogeneous composite photocatalyst and preparation method thereof
CN113198453B (en) * 2021-05-20 2022-09-23 陕西科技大学 Lamellar Bi 2 O 2 SiO 3 -Si 2 Bi 24 O 40 Heterogeneous composite photocatalyst and preparation method thereof
CN113231099A (en) * 2021-05-21 2021-08-10 吉林大学 Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst

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