CN110526281B

CN110526281B - Method for synthesizing tin disulfide

Info

Publication number: CN110526281B
Application number: CN201910791771.XA
Authority: CN
Inventors: 梁初; 潘良斌; 汪炀锋; 黄辉; 张文魁; 甘永平; 夏阳; 张俊
Original assignee: Zhejiang University of Technology ZJUT
Current assignee: Zhejiang University of Technology ZJUT
Priority date: 2019-08-26
Filing date: 2019-08-26
Publication date: 2021-08-24
Anticipated expiration: 2039-08-26
Also published as: CN110526281A

Abstract

The invention discloses a method for synthesizing tin disulfide, which takes anhydrous tin tetrachloride and lithium sulfide as a tin source and a sulfur source respectively and enables the anhydrous tin tetrachloride and the lithium sulfide to react by a direct heating method. After the reaction is finished, filtering, washing and drying the product by deionized water to obtain the tin disulfide. The method has simple process and low energy consumption, and is easy for industrial production.

Description

Method for synthesizing tin disulfide

Technical Field

The invention belongs to the field of materials science, and particularly relates to a method for synthesizing tin disulfide by a heating mode.

Background

Over the past 100 years, a large amount of energy resources on earth have been consumed. The world energy structure is dominated by fossil energy, which remains the energy base for human survival and development for a long period of time. At present, the use of fossil energy mainly comprising coal and petroleum brings global energy environmental problems, which mainly include acid rain, ozone layer destruction, greenhouse gas emission and the like. Nowadays, the problems of fossil energy exhaustion and energy environmental pollution still plague human beings. Renewable energy is the most efficient method to replace conventional fossil energy. Renewable energy sources are broadly classified into wind energy, solar energy, geothermal energy, tidal energy, and the like. Among the above energy sources, solar energy has the most potential to become a mainstream energy source, and under the condition that fossil fuel is decreasing, solar energy has become an important component of energy used by human beings, and is continuously developed.

Tin disulfide (SnS)₂) Is a non-toxic, cheap and typical CdI₂The n-type semiconductor with the layer-shaped structure has a wide band gap of about 2.1eV, and has good optical and electrical properties due to the wider band gap;meanwhile, the Sn and S elements are rich in earth content and are nontoxic. Therefore, the tin disulfide is a promising thin-film solar cell material.

The Chinese invention patent (application No. 201710455988.4) discloses a hydrothermal preparation method of locally oxidized SnS₂The method of the slice adopts tin tetrachloride or tin nitrate and is used as a tin source, an L-cysteine sulfur source and a mixed solution of water and glycol as a solvent, and the partial oxidized SnS is obtained by heating for 5 to 15 hours at the temperature of 160-165 DEG C₂A sheet. The Chinese invention patent (application No. 201711128867.5) discloses a hydrothermal method for preparing SnS rich in S vacancy₂Method of making ultrathin nanosheets from SnCl₄·5H₂O and L-cysteine are respectively used as a tin source and a sulfur source, ethylene glycol is used as a solvent, and the mixture is heated at 160-220 ℃ for 16-48 h to prepare SnS rich in S vacancy₂An ultrathin nanosheet. At present, although an SnS having a specific structure has been available₂But preparation of SnS₂In the preparation of the material, organic solvents or chemical surfactants which are not beneficial to environmental ecology and a hydrothermal method with high energy consumption are almost adopted. Thus developing environment-friendly, simple and low-energy-consumption synthetic SnS₂The approach of materials remains challenging.

Disclosure of Invention

The invention aims to provide a simple, green, environment-friendly and low-energy-consumption method for synthesizing tin disulfide by a heating mode aiming at the defects of the prior art.

The invention utilizes anhydrous stannic chloride and lithium sulfide as a tin source and a sulfur source respectively, and the anhydrous stannic chloride and the lithium sulfide react to synthesize the stannic sulfide in a heating mode.

The invention adopts the following specific technical scheme for solving the technical problems:

a method for synthesizing tin disulfide comprises the following steps:

(1) under vacuum or protective atmosphere, uniformly mixing anhydrous tin tetrachloride and lithium sulfide, and transferring the mixture to a closed reactor;

(2) heating the mixture in the reactor to a certain temperature and reacting at constant temperature for a period of time;

(3) and after the constant-temperature reaction is finished, separating the taken solid product to obtain the tin disulfide.

Preferably, the protective atmosphere in step (1) is a gas or a mixture thereof that does not react with the reactants and products, and includes nitrogen and argon.

Preferably, the molar ratio of the anhydrous tin tetrachloride to the lithium sulfide in the step (1) is 0.5-10: 1.

Preferably, the temperature in the step (2) is 20-200 ℃, and the constant-temperature reaction time is 0.1-24 hours.

Preferably, the separation in step (3) is to heat the solid product to 130 ℃, collect the excess stannic chloride by condensation reflux, dissolve the solid product in water, filter, wash and dry the solid product with deionized water.

Compared with the prior art, the invention has the following beneficial effects: the method has the advantages of simple process, low energy consumption, easy industrial production, environmental protection and no generation of byproducts and waste gas.

Drawings

Figure 1 is an XRD pattern of the tin disulfide synthesized by the reaction of example 1.

Detailed Description

The technical solution of the present invention is further described with reference to the following embodiments, but the scope of the present invention is not limited thereto.

Example 1

Anhydrous tin tetrachloride and lithium sulfide were mixed in a molar ratio of 0.5:1 under vacuum, the mixture was transferred to a reactor, and the mixture was heated to 20 ℃ for isothermal reaction for 24 hours. And after the constant-temperature reaction is finished, taking out a solid product, heating the solid product to 130 ℃, condensing, refluxing and collecting redundant stannic chloride, dissolving the solid product in water, filtering, washing and drying by using deionized water to obtain the stannic sulfide. The XRD pattern is shown in figure 1.

Example 2

Anhydrous tin tetrachloride and lithium sulfide were mixed at a molar ratio of 10:1 under a nitrogen atmosphere, the mixture was transferred to a reactor, and the mixture was heated to 200 ℃ for a constant temperature reaction for 0.1 h. And after the constant-temperature reaction is finished, taking out a solid product, heating the solid product to 130 ℃, condensing, refluxing and collecting redundant stannic chloride, dissolving the solid product in water, filtering, washing and drying by using deionized water to obtain the stannic sulfide.

Example 3

Anhydrous tin tetrachloride and lithium sulfide were mixed at a molar ratio of 5:1 under an argon atmosphere, the mixture was transferred to a reactor, and the mixture was heated to 100 ℃ and reacted at a constant temperature for 12 hours. And after the constant-temperature reaction is finished, taking out a solid product, heating the solid product to 130 ℃, condensing, refluxing and collecting redundant stannic chloride, dissolving the solid product in water, filtering, washing and drying by using deionized water to obtain the stannic sulfide.

Example 4

Anhydrous tin tetrachloride and lithium sulfide were mixed in a molar ratio of 2:1 under vacuum, the mixture was transferred to a reactor, and the mixture was heated to 150 ℃ for 4h at constant temperature. And after the constant-temperature reaction is finished, taking out a solid product, heating the solid product to 130 ℃, condensing, refluxing and collecting redundant stannic chloride, dissolving the solid product in water, filtering, washing and drying by using deionized water to obtain the stannic sulfide.

Example 5

Anhydrous tin tetrachloride and lithium sulfide were mixed at a molar ratio of 6:1 under a mixed atmosphere of nitrogen and argon, the mixture was transferred to a reactor, and the mixture was heated to 80 ℃ and reacted at a constant temperature for 16 hours. And after the constant-temperature reaction is finished, taking out a solid product, heating the solid product to 130 ℃, condensing, refluxing and collecting redundant stannic chloride, dissolving the solid product in water, filtering, washing and drying by using deionized water to obtain the stannic sulfide.

Claims

1. A method for synthesizing tin disulfide by a heating mode is characterized by comprising the following steps:

(3) after the reaction is finished, separating the taken solid product to obtain the tin disulfide;

wherein the temperature in the step (2) is 20-200 ℃, and the heat preservation time is 0.1-24 h.

2. The method for synthesizing tin disulfide by heating as claimed in claim 1, wherein: the protective atmosphere in step (1) is a gas or a mixture of gases which do not react with the reactants and the products, and comprises nitrogen and argon.

3. The method for synthesizing tin disulfide by heating as claimed in claim 1, wherein: the molar ratio of the anhydrous tin tetrachloride to the lithium sulfide in the step (1) is 0.5-10: 1.

4. The method for synthesizing tin disulfide by heating as claimed in claim 1, wherein: and (3) the separation in the step (3) is to heat the solid product to 130 ℃, collect the redundant stannic chloride by condensation and reflux, dissolve the solid product in water, filter, wash and dry the solid product by deionized water.