Preparation method of zinc copper sulfide flower-like micro-sphere super-structure visible-light-driven photocatalyst composed of nanosheets

A flower-shaped microsphere, copper-zinc sulfide technology, applied in the field of photocatalysis, can solve the problems of weak oxidative degradation ability of pollutants, unstable photocatalyst, low solar energy utilization rate, etc., and achieves increased oxidative degradation ability and strong photocorrosion resistance. , the effect of low cost

Inactive Publication Date: 2018-07-13
XIANGTAN UNIV
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  • Claims
  • Application Information

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Problems solved by technology

At present, in the semiconductor catalysts used in heterogeneous photocatalytic reactions, the energy band gap of semiconductors that are sensitive to sunlight and have photocatalytic properties is generally 1.9-3.1eV. If the band gap is too wide, it can only absorb ultraviolet rays in sunlight. Light, and ultraviolet light in sunlight only accounts for 3% to 4% of the total energy of sunlight, so the utilization rate of solar energy is low, such as TiO 2 (3.2eV), ZnO(3.4eV), ZnS(3.6eV) and other photocatalysts; on the contrary, if the band gap is too narrow, the ability to oxidize and degrade pollutants is weak, such as Bi 2 S 3 (1.2~1.7eV), Sb 2 S 3 (1.5~2.2eV), CuS(1.8~2.0eV), CuO(1.7eV), etc.
In addition, metal sulfide semiconductor photocatalysts such as ZnS, CuS, and CdS are unstable in the photocatalytic process and are prone to photocorrosion, which also limits their practical applications. However, their stability can be improved if they are prepared as multi-component metal sulfides. , making it less susceptible to photocorrosion

Method used

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  • Preparation method of zinc copper sulfide flower-like micro-sphere super-structure visible-light-driven photocatalyst composed of nanosheets
  • Preparation method of zinc copper sulfide flower-like micro-sphere super-structure visible-light-driven photocatalyst composed of nanosheets
  • Preparation method of zinc copper sulfide flower-like micro-sphere super-structure visible-light-driven photocatalyst composed of nanosheets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (a) Weigh 0.82g CuCl 2 2H 2 O and 0.35 g ZnSO 4 ·7H 2 O was added to 120mL ethylene glycol respectively (equivalent to adding Zn in every milliliter ethylene glycol 2+ with Cu 2+The amount of total substance is 0.05mmol), stirring and dissolving; Then add 1.83g thiourea (the amount of its substance is Zn 2+ with Cu 2+ 4 times of the amount of total substance), continue to stir until thiourea dissolves completely, obtain mixed solution;

[0023] (b) Add 60 mg of polyvinylpyrrolidone (equivalent to adding 0.5 mg of polyvinylpyrrolidone per milliliter of ethylene glycol) to the mixed solution, and stir evenly; then, stir and reflux at 130° C. for 1 hour;

[0024] (c) After the reaction is completed, naturally cool to room temperature, centrifuge, and wash the obtained precipitate with deionized water and absolute ethanol alternately and ultrasonically for 3 times, and after drying, a flower-shaped microsphere superstructure visible light catalyst composed of nanoshee...

Embodiment 2

[0027] (a) Weigh 1.42g CuSO 4 ·5H 2 O and 0.041g ZnCl 2 were added to 60mL 1,2-propanediol (equivalent to adding Zn 2+ with Cu 2+ The amount of total substance is 0.1mmol), stirring and dissolving; Then add 1.37g thiourea (the amount of its substance is Zn 2+ with Cu 2+ 3 times of the amount of total substance), continue to stir until thiourea dissolves completely, obtain mixed solution;

[0028] (b) Add 180 mg of polyvinylpyrrolidone (equivalent to 3 mg of polyvinylpyrrolidone per milliliter of 1,2-propylene glycol) into the mixed solution, and stir evenly; then, stir and reflux at 150° C. for 2 hours;

[0029] (c) After the reaction is completed, naturally cool to room temperature, centrifuge, and wash the obtained precipitate with deionized water and absolute ethanol alternately and ultrasonically for 3 times, and after drying, a flower-shaped microsphere superstructure visible light catalyst composed of nanosheets is obtained. Zn 0.05 Cu 0.95 S.

Embodiment 3

[0031] (a) Weigh 1.30g Cu(NO 3 ) 2 ·3H 2 O and 0.17g ZnSO 4 ·7H 2 O was added to 100mL ethylene glycol respectively (equivalent to adding Zn in every milliliter ethylene glycol 2+ with Cu 2+ The amount of total substance is 0.06mmol), stirring and dissolving; Then add 0.91g thiourea (the amount of its substance is Zn 2+ with Cu 2+ 2 times of the amount of total substance), continue to stir until thiourea dissolves completely, obtain mixed solution;

[0032] (b) Add 200 mg of polyvinylpyrrolidone (equivalent to 2 mg of polyvinylpyrrolidone per 1 ml of ethylene glycol) into the mixed solution, and stir evenly; then, stir and reflux at 160° C. for 3 hours;

[0033] (c) After the reaction is completed, naturally cool to room temperature, centrifuge, and wash the obtained precipitate with deionized water and absolute ethanol alternately and ultrasonically for 3 times, and after drying, a flower-shaped microsphere superstructure visible light catalyst composed of nanosheets i...

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Abstract

The invention provides a preparation method of a zinc copper sulfide flower-like micro-sphere super-structure visible-light-driven photocatalyst composed of nanosheets. The method comprises the following steps: respectively adding a zinc salt and a copper salt into o-hydroxyl diol, stirring and dissolving, adding thiourea, and continuously stirring until the thiourea is completely dissolved; adding polyvinylpyrrolidone (PVP), and performing stirring reflux at a temperature of 120-160 DEG C for 1-3 hours; naturally cooling to a room temperature, and performing centrifugal separation; washing and drying the obtained precipitate, thereby obtaining the flower-like micro-sphere super-structure visible-light-driven photocatalyst ZnxCu1-xS composed of nanosheets (x is more than or equal to 0.05 and less than or equal to 0.3). The product prepared by the method disclosed by the invention is large in specific surface area, high in photocorrosion resistance and high in visible-light photocatalytic activity, and environmental pollutants can be subjected to photocatalytic degradation by fully utilizing sunlight. The method has the advantages of being simple in production process, safe in production process, easily controllable in reaction parameters and capable of easily realizing large-scale industrialized production.

Description

technical field [0001] The invention belongs to the technical field of photocatalysis, and in particular relates to a Zn nanometer sheet composed of nanosheets prepared by a reflux method. x Cu 1-x S(0.05≤x≤0.3) (copper zinc sulfide) flower-shaped microsphere superstructure visible light catalyst method. Background technique [0002] With the development of social economy, the problem of environmental pollution is becoming more and more serious. The governance and control of environmental pollution is a major issue that human beings face and need to solve urgently in the 21st century. Semiconductor heterogeneous photocatalysis has been favored by people because of its strong oxidative properties, complete mineralization of pollutants, and direct use of sunlight in the removal of various environmental refractory pollutants. At present, in the semiconductor catalysts used in heterogeneous photocatalytic reactions, the energy band gap of semiconductors that are sensitive to s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/04B01J35/08B01J37/03C02F1/30C02F101/36C02F101/38
CPCC02F1/30B01J27/04B01J37/031C02F2101/38C02F2101/40C02F2101/36C02F2101/308C02F2305/10B01J35/23B01J35/51B01J35/39
Inventor 朱启安黎平胡耐根蒋叔立
Owner XIANGTAN UNIV
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