CN104646032A - Method for preparing SnS2/ZnFe2O4 graphene compound photocatalyst through hydrothermal method - Google Patents

Method for preparing SnS2/ZnFe2O4 graphene compound photocatalyst through hydrothermal method Download PDF

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Publication number
CN104646032A
CN104646032A CN201510065857.6A CN201510065857A CN104646032A CN 104646032 A CN104646032 A CN 104646032A CN 201510065857 A CN201510065857 A CN 201510065857A CN 104646032 A CN104646032 A CN 104646032A
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graphene
sns
znfe
composite photocatalyst
hydro
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CN201510065857.6A
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Inventor
邓芳
裴旭乐
罗旭彪
李文涛
罗胜联
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Nanchang Hangkong University
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Nanchang Hangkong University
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Abstract

The invention discloses a method for preparing a high-performance SnS2/ZnFe2O4 graphene compound photocatalyst through a hydrothermal method. The method comprises the following steps: firstly, graphene oxide is synthesized by adopting a modified Hummers method, the graphene oxide is reduced with 80% hydrazine hydrate, and then the reduced graphene oxide is prepared through freezing and drying; the prepared graphene, zinc nitrate, iron nitrate, stannic chloride and thioacetamide are added into deionized water and are mixed uniformly, the pH of the solution is adjusted to be alkali with alkali liquor, then the solution is transferred into a reaction still, water thermal reaction is carried out for 14-24 hours at 160-220 DEG C, and then suction filtering, washing and drying are carried out to prepare the SnS2/ZnFe2O4 graphene compound photocatalyst. The method has the outstanding advantages of simplicity and practicability, high productivity and low cost, and has very good photocatalytic degradation performance.

Description

Hydro-thermal method prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst
Technical field
The present invention relates to the SnS that a kind of hydro-thermal method prepares high catalytic performance 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, belongs to composite photo-catalyst preparing technical field.
Background technology
Water is lifespring, does not have water, does not just have life.But along with industry and economic fast development, people lack the consciousness of environmental protection, add the factors such as the restriction of sewage disposal technology level and result in discharged volume of industrial waste water and sharply increase, the pollution problem of water environment is day by day serious.These waste component are complicated, and character is changeable, not only containing common are organic pollutants, simultaneously containing some heavy metal ion.If these waste water do not process, be directly discharged in environment, water environment and ecological environment caused to the destruction of unrepairable, and harm humans is healthy.So seek efficient, green wastewater treating technology is extremely urgent.Art in recent years, photocatalysis oxidation technique arouses widespread concern in water pollution control.
Zinc ferrite (ZnFe 2o 4) be the soft magnetic material of function admirable, there is good opto-electronic conversion performance simultaneously, but photocatalysis effect not ideal.Therefore, ZnFe is improved 2o 4photocatalysis performance have great significance.
SnS 2be a kind of very important layered semiconductor material, have a wide range of applications in photocatalytically degradating organic dye, but due to energy gap large, the right separating rate of light induced electron and hole is slow, and recombination rate is high, causes SnS 2application in visible-range receives certain restriction.It is modified, is better applied to environmental protection and is necessary.
Graphene (RG0) is as a kind of novel carbon structure material, charge carrier containing high fluidity, surface area is large, have good conduction and heat conductivility, many catalysis materials, with it after compound, all show excellent photocatalysis performance simultaneously, overcome energy gap large, the shortcomings such as specific area is little, promote the generation of catalytic reaction, improve photocatalysis efficiency.Comprehensively above-mentioned, by Graphene and SnS 2, ZnFe 2o 4carry out compound, photocatalysis efficiency will be improved further, better for wastewater treatment.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, propose the SnS that a kind of hydro-thermal method prepares high catalytic performance 2/ ZnFe 2o 4the method of/graphene composite photocatalyst.This method prepares SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst productive rate is high, and has extraordinary photocatalysis performance.
The object of the invention is to be achieved through the following technical solutions, this preparation method comprises the steps: the Hummers method synthesis graphene oxide first adopting modification, then use the hydrazine hydrate reduction graphene oxide of 80%, then carry out freeze drying and prepare redox graphene (RGO).By the Graphene prepared, zinc nitrate, ferric nitrate, stannic chloride and thioacetamide join in deionized water, stir, and regulate pH to be alkalescence, then solution are transferred to reactor, 160 ~ 220 ounder C, hydro-thermal reaction 14 ~ 24 hours, then carries out suction filtration, washing, drying, prepares SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst.
Described Graphene take graphite powder as raw material.
Described alkali lye is NaOH or ammonia spirit.
Described pH value of solution scope is 8 ~ 13.
Described SnS 2and ZnF 2o 4mol ratio is 50:1 ~ 25:2.
Described Graphene and SnS 2mass ratio be 1:100 ~ 3:20.
The present invention prepares SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst advantage:
(1) the present invention has the advantage that preparation method is simple, energy consumption is low, cost is low.
(2) SnS for preparing of the present invention 2/ ZnFe 2o 4/ graphene composite photocatalyst has good photocatalysis performance under visible light.
(3) SnS for preparing of the present invention 2/ ZnFe 2o 4/ graphene composite photocatalyst has larger specific area, and energy gap is narrow, can effectively make electron-hole be separated, under visible light can efficient degradation organic pollution and reducing heavy metal ion.
Accompanying drawing explanation
Fig. 1 is SnS prepared by embodiments of the invention 6 2/ ZnFe 2o 4snS prepared by (a) and embodiment 1 2/ ZnFe 2o 4nitrogen adsorption-the desorption isotherm of/graphene composite photocatalyst (b), as seen from the figure, SnS 2/ ZnFe 2o 4and SnS 2/ ZnFe 2o 4the adsorption-desorption isothermal of/graphene composite photocatalyst all belongs to the IV type in IUPAC classification, H3 hysteresis loop.SnS 2/ ZnFe 2o 4the specific area of/graphene composite photocatalyst is 54.5 m 2/ g, SnS 2/ ZnFe 2o 4specific area is 51.5 m 2/ g, SnS 2/ ZnFe 2o 4the specific area of/graphene composite photocatalyst is a bit larger tham SnS 2/ ZnFe 2o 4.
Fig. 2 is SnS prepared by embodiments of the invention 6 2/ ZnFe 2o 4snS prepared by (a) and embodiment 1 2/ ZnFe 2o 4the diffuse reflection figure of/graphene composite photocatalyst (b).As seen from the figure, SnS 2/ ZnFe 2o 4the energy gap of/graphene composite photocatalyst is than SnS 2/ ZnFe 2o 4little.
Fig. 3 is SnS prepared by embodiments of the invention 6 2/ ZnFe 2o 4snS prepared by (a) and embodiment 1 2/ ZnFe 2o 4/ graphene composite photocatalyst (b) to the photocatalytic degradation curve of methyl orange, as seen from the figure, SnS 2/ ZnFe 2o 4the Photocatalytic activity of/graphene composite photocatalyst to methyl orange is greater than SnS 2/ ZnFe 2o 4.
Detailed description of the invention
Below implement to be intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) take graphite powder as raw material, adopt Hummers method synthesis graphene oxide (GO), then reduce with the hydrazine hydrate of 80%, obtain redox graphene.
(2) by the Zn (NO of 0.01mol 3) 26H 2o and 0.02molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=13 with NaOH.
(3) in beaker A, add the stannic chloride of 0.002mol and the thioacetamide of 0.004mol, add the Graphene prepared in advance simultaneously, Graphene addition is SnS 2the 1wt% of quality.
(4) solution in beaker A has been transferred in polytetrafluoroethyllining lining reactor 160 oreact 14 hours under C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares orange-yellow SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst.
Embodiment 2
(1) take graphite powder as raw material, adopt Hummers method synthesis graphene oxide (GO), then reduce with the hydrazine hydrate of 80%, obtain redox graphene.
(2) by the Zn (NO of 0.01mol 3) 26H 2o and 0.02molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=8 with NaOH.
(3) in beaker A, add the stannic chloride of 0.002mol and the thioacetamide of 0.004mol, add the Graphene prepared in advance simultaneously, the corresponding SnS of amount of Graphene 2mass ratio is 15wt%.
(4) to have been transferred to by the solution in beaker A in polytetrafluoroethyllining lining reactor and reacted 24 hours at 220 DEG C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares orange-yellow SnS 2/ ZnFe 2o 4/ Graphene orange composite photo-catalyst.
Embodiment 3
(1) take graphite powder as raw material, adopt Hummers method synthesis graphene oxide (GO), then reduce with the hydrazine hydrate of 80%, obtain redox graphene.
(2) by the Zn (NO of 0.01mol 3) 26H 2o and 0.125molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=13 with NaOH.
(3) in beaker A, add the stannic chloride of 0.002mol and the thioacetamide of 0.004mol, add the Graphene prepared in advance simultaneously, the corresponding SnS of amount of Graphene 2mass ratio is 7wt%.
(4) to have been transferred to by the solution in beaker A in polytetrafluoroethyllining lining reactor and reacted 24 hours at 180 DEG C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares orange-yellow SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst.
Embodiment 4
(1) take graphite powder as raw material, adopt Hummers method synthesis graphene oxide (GO), then reduce with the hydrazine hydrate of 80%, obtain redox graphene.
(2) by the Zn (NO of 0.01mol 3) 26H 2o and 0.125molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=13 with ammoniacal liquor.
(3) in beaker A, add the stannic chloride of 0.002mol and the thioacetamide of 0.004mol, add the Graphene prepared in advance simultaneously, the corresponding SnS of amount of Graphene 2mass ratio is 15wt%.
(4) to have been transferred to by the solution in beaker A in polytetrafluoroethyllining lining reactor and reacted 24 hours at 180 DEG C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares orange-yellow SnS 2/ ZnFe 2o 4the orange-yellow composite photo-catalyst of/Graphene.
Embodiment 5
(1) take graphite powder as raw material, adopt Hummers method synthesis graphene oxide (GO), then reduce with the hydrazine hydrate of 80%, obtain redox graphene.
(2) by the Zn (NO of 0.01mol 3) 26H 2o and 0.02molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=10 with NaOH.
(3) in beaker A, add the stannic chloride of 0.002mol and the thioacetamide of 0.004mol, add the Graphene prepared in advance simultaneously, the corresponding SnS of amount of Graphene 2mass ratio is 15wt%.
(4) to have been transferred to by the solution in beaker A in polytetrafluoroethyllining lining reactor and reacted 24 hours at 180 DEG C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares orange-yellow SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst.
Embodiment 6
(1) by the Zn (NO of 0.01mol 3) 26H 2o and 0.02molFe (NO 3) 39H 2o is dissolved in the beaker A of the deionized water of 50ml, stirs, and regulates pH=13 with NaOH.
(2) stannic chloride of 0.002mol and the thioacetamide of 0.004mol are added in the beaker A of 50ml deionized water and stir.
(3) to have been transferred to by the solution in beaker A in polytetrafluoroethyllining lining reactor and reacted 24 hours at 180 DEG C, then use deionized water and absolute ethanol washing three times, after dry 12 hours, grinding, prepares yellow SnS 2/ ZnFe 2o 4photochemical catalyst.

Claims (6)

1. a hydro-thermal method prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that, first adopts the Hummers method synthesis graphene oxide of modification, then the hydrazine hydrate reduction graphene oxide of 80% is used, then carry out freeze drying and prepare redox graphene, then the redox graphene that will prepare, zinc nitrate, ferric nitrate, stannic chloride and thioacetamide join in deionized water, stir, and regulate pH value of solution to be alkalescence with alkali lye, then solution is transferred to reactor, 160 ~ 220 ounder C, hydro-thermal reaction 14 ~ 24 hours, then carries out suction filtration, washing, drying, prepares SnS 2/ ZnFe 2o 4/ graphene composite photocatalyst.
2. hydro-thermal method according to claim 1 prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that: described Graphene take graphite powder as raw material.
3. hydro-thermal method according to claim 1 prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that: described alkali lye is NaOH or ammonia spirit.
4. hydro-thermal method according to claim 1 prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that: described pH value of solution scope is 8 ~ 13.
5. hydro-thermal method according to claim 1 prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that: ZnF 2o 4and SnS 2mol ratio be 1:50 ~ 2:25.
6. hydro-thermal method according to claim 1 prepares SnS 2/ ZnFe 2o 4the method of/graphene composite photocatalyst, is characterized in that: Graphene and SnS 2mass ratio be 1:100 ~ 3:20.
CN201510065857.6A 2015-02-07 2015-02-07 Method for preparing SnS2/ZnFe2O4 graphene compound photocatalyst through hydrothermal method Pending CN104646032A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112844414A (en) * 2021-01-29 2021-05-28 昆明理工大学 Popcorn-shaped ZnFe2O4Preparation method of/CdS/GO heterojunction photocatalyst
CN113042062A (en) * 2021-03-05 2021-06-29 景德镇陶瓷大学 Zinc ferrite-tin oxide composite material, preparation thereof and application thereof in photocatalysis

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CN102151567A (en) * 2011-02-25 2011-08-17 哈尔滨工业大学 Catalyst for oxidation and decomposition of organic pollutants in water with ozone and method thereof for catalyzing sewage treatment with ozone
CN102522543A (en) * 2011-12-15 2012-06-27 清华大学 Method for preparing nanometer compound of tin disulfide-graphene

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CN102142549A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene nano sheet and SnS2 composite nano material and synthesis method thereof
CN102151567A (en) * 2011-02-25 2011-08-17 哈尔滨工业大学 Catalyst for oxidation and decomposition of organic pollutants in water with ozone and method thereof for catalyzing sewage treatment with ozone
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112844414A (en) * 2021-01-29 2021-05-28 昆明理工大学 Popcorn-shaped ZnFe2O4Preparation method of/CdS/GO heterojunction photocatalyst
CN113042062A (en) * 2021-03-05 2021-06-29 景德镇陶瓷大学 Zinc ferrite-tin oxide composite material, preparation thereof and application thereof in photocatalysis

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