A kind of preparation method of stannous sulfide

A technology of stannous sulfide and tin powder, applied in chemical instruments and methods, tin compounds, inorganic chemistry, etc., can solve the problems of difficult cleaning and removal, large investment, and high equipment requirements

Active Publication Date: 2020-07-07
云南锡业集团(控股)有限责任公司研发中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Tin sulfide products can be synthesized by various methods. For example, patent application 201710802843.7 discloses a method, which uses tin-containing materials and sulfur for sulfide reaction to convert them into sulfide, and then vacuum distillation to remove impurities to obtain high-purity sulfide Tin; the method of patent application 201210404428.3 is to first react tin with concentrated hydrochloric acid and then react with sodium sulfide to prepare stannous sulfide. Soluble stannous salt is prepared into a solution, hydrochloric acid is added dropwise to sulfur salt to generate hydrogen sulfide gas, and the generated gas is introduced into the stannous salt solution to react to synthesize stannous sulfide, which is then washed to remove impurities, dried and purified to obtain a purity of 95.77%~99.54 % stannous sulfide products; the existing part of the dry process to prepare stannous sulfide raw materials has strong adaptability, and the resulting product has high purity, but the equipment requirements are high and the investment is large; the wet process is easy to introduce other impurity ions in the preparation process , it is difficult to wash and remove, which affects the purity of the product. Some wet processes involve toxic gases, and there is a certain risk in personnel operation, and there is a common problem of waste liquid treatment in the later stage of wet preparation of stannous sulfide.

Method used

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  • A kind of preparation method of stannous sulfide
  • A kind of preparation method of stannous sulfide
  • A kind of preparation method of stannous sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Weigh 119 grams of 200 mesh 2N metal tin powder and 32 grams of sublimated sulfur powder in the mixer according to the molar ratio of tin powder (99%, particle size <150μm) to sublimation sulfur powder of 1:1. Mix for 1h;

[0029] (2) Raise the temperature of the reaction furnace to 650°C, and replace the air in the furnace with nitrogen for 30 minutes;

[0030] (3) Put the mixed powder in the figure 1 In the hopper, the tin and sulfur powder react rapidly in a nitrogen atmosphere at 650 °C to form stannous sulfide, and are fed into the reaction furnace at a constant speed through the feeding controller. After the feeding is completed, the temperature in the furnace is maintained at 650 °C. 2h, make the excess sulfur evaporate and enter the condenser to condense and collect;

[0031] (4) Natural cooling of stannous sulfide in the furnace after impurity removal;

[0032] (5) After the furnace temperature is cooled to room temperature, open the furnace cover to tak...

Embodiment 2

[0034] (1) According to the molar ratio of tin powder (99.9%, particle size < 150μm) and sublimation sulfur powder as 1:1.5, weigh 119 grams of 200-mesh 3N metal tin powder and 48 grams of sublimated sulfur powder in the mixer. Mix for 1h;

[0035] (2) Raise the temperature of the reaction furnace to 750℃, and replace the air in the furnace with nitrogen for 30min;

[0036] (3) Put the mixed powder in the figure 1 In the hopper, it is added to the reaction furnace at a constant speed through the feeding controller, and the powder and sulfur powder react rapidly in a nitrogen atmosphere at 750 ° C to form stannous sulfide; After the sulfur evaporates, it enters the condenser to condense and collect;

[0037] (4) Natural cooling of stannous sulfide in the furnace after impurity removal;

[0038] (5) After the furnace temperature is cooled to room temperature, open the furnace cover to take out the sample, and the preparation of the stannous sulfide sample is completed; the pu...

Embodiment 3

[0040] (1) According to the molar ratio of tin powder (99.99%, particle size < 150μm) and sublimation sulfur powder of 1:2, weigh 119 grams of 200-mesh 4N metal tin powder and 64 grams of sublimated sulfur powder in the mixer. Mix for 1h;

[0041] (2) Raise the temperature of the reaction furnace to 800℃, and replace the air in the furnace with argon for 30min;

[0042] (3) Put the mixed powder in the figure 1 In the hopper, and fed into the reaction furnace at a constant speed through the feeding controller, the tin powder and the sulfur powder reacted rapidly in an argon atmosphere at 800 ° C to form stannous sulfide. After the feeding, the furnace temperature was maintained at 800 ° C for 2 hours. After the excess sulfur is evaporated, it enters the condenser to condense and collect;

[0043] (4) Naturally cool stannous sulfide in the furnace after removing elemental sulfur;

[0044] (5) After the furnace temperature is cooled to room temperature, open the furnace cover ...

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Abstract

The invention discloses a preparation method of stannous sulfide. The preparation method comprises the following steps: uniformly mixing metallic tin powder with sublimate powdered sulfur, adding mixed powder into an atmosphere reaction furnace with the temperature of 650 DEG C-1000 DEG C and performing a quick reaction on tin and sulfur to obtain liquid tin sulfide; controlling the furnace temperature at 650 DEG C-1000 DEG C, continuously preserving the temperature for 0.5-4h, distilling to remove redundant sulfur in the tin sulfide product and cooling to obtain the high-purity stannous sulfide. The method is simple in process, low in cost, high in synthesis speed of the product, high in product yield and high in purity; less waste residues and waste gas are generated, and the productionprocess is green and environmentally-friendly, therefore, the method has a relatively good industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of stannous sulfide, and belongs to the field of new material preparation. Background technique [0002] Stannous sulfide is an important multifunctional material with the advantages of safety and non-toxicity, and is used for various purposes. Antimony sulfide in automobile friction materials can reduce the decomposition rate of organic binders, maintain stable friction performance, and reduce noise and vibration during friction braking. It is a solid lubricant with excellent performance, but antimony has a carcinogenic effect. Many countries have begun to restrict or prohibit the use of stannous sulfide, which is safe and non-toxic, and is used as a substitute for antimony sulfide. Stannous sulfide is used in the light absorption layer of solar cells. Because of its direct band gap of 1.2ev~1.52ev and indirect bandgap of 1.0ev~1.1ev, it has high photoelectric conversion efficiency for sunlight, which is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/00
Inventor 郭绍雄陈高芳彭巨擘张家涛普友福鲍庆煌罗晓斌
Owner 云南锡业集团(控股)有限责任公司研发中心
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