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Preparation method of diphenyl sulfide

A technology of diphenyl sulfide and chlorobenzene, which is applied in the field of preparing diphenyl sulfide, can solve the problems of large amount of solvent used, high recovery cost, high price of iodobenzene, etc., and achieves reasonable synthesis process, low cost and environmental friendliness Effect

Active Publication Date: 2015-01-28
兰州诚胜化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The treatment of the three wastes is very difficult, and the amount of solvent used is large, and the recycling cost is not small
The raw material iodobenzene of the third method is more expensive, and the yield is too poor, resulting in relatively large production costs and difficulty in forming production capacity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a 500ml four-neck flask equipped with a vacuum system, stirring, dropping funnel, distillation head, condenser, and thermometer, add 240.0g of sodium sulfide, and slowly heat to 200°C at -0.098MPa. Remove the distillation system, slowly add solvent NMP100ml, after stirring for 20 minutes, transfer the sodium sulfide solution to a 500ml autoclave while it is hot, and then add 225g of chlorobenzene dropwise within 2 hours under stirring; Replace the air twice with nitrogen, continue to keep stirring at 190-200°C for 5 hours; then filter off the solids, evaporate NMP in vacuum, cool slowly to 80°C, add 300ml of water and stir for 10 minutes, let stand for 30 minutes, separate the water layer and the oil layer Distillation was carried out to collect fractions at 125-135°C (0.5kPa) to obtain 154g of diphenyl sulfide, with a yield of 81.1% and a purity of 98.1%.

Embodiment 2

[0035] In a 500ml four-neck flask equipped with a vacuum system, stirring, dropping funnel, distillation head, condenser, and thermometer, add 240.0g of sodium sulfide, and slowly heat to 200°C at -0.098MPa. Remove the distillation system, slowly add solvent DMF80ml dropwise, after stirring for 20 minutes, transfer the sodium sulfide solution to a 500ml autoclave while hot, then add 225g of chlorobenzene dropwise within 1.8 hours under stirring; Replace the air twice with nitrogen, continue to keep stirring at 190-200°C for 5 hours; then filter off the solids, evaporate DMF in vacuum, cool slowly to 80°C, add 300ml of water and stir for 10 minutes, let stand for 30 minutes, separate the water layer and the oil layer Distillation was carried out to collect fractions at 125-135°C (0.5kPa) to obtain 153.6g of diphenyl sulfide with a yield of 81.22% and a purity of 98.5%.

Embodiment 3

[0037] In a 500ml four-neck flask equipped with a vacuum system, stirring, dropping funnel, distillation head, condenser, and thermometer, add 240.0g of sodium sulfide, and slowly heat to 210°C at -0.098MPa. Remove the distillation system, slowly add solvent NMP100ml, after stirring for 10 minutes, transfer the sodium sulfide solution to a 500ml autoclave while it is hot, then add 222g of chlorobenzene dropwise within 2.0 hours under stirring, cover, and replace the air with nitrogen twice , then slowly heated up to 240°C with stirring, kept stirring for 2.0 hours; filtered off the solids, evaporated to remove NMP in vacuum, slowly cooled to 80°C, added 300ml of water and stirred for 10 minutes, stood still for 30 minutes, separated the water layer, and collected the oil layer by distillation 158g of diphenyl sulfide was obtained in the distillate at 125-135°C (0.5kPa), with a yield of 83.3% and a purity of 98.2%.

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Abstract

The invention discloses a preparation method of diphenyl sulfide. The method is as below: adding a certain amount of sodium sulfide in a reaction container; keeping the negative pressure at less than or equal to -0.098 MPa, and slowly heating to 190-220 DEG C; dropwise adding a solvent with insulation, stirring, transferring the sodium sulfide solution while hot to an autoclave, then dropwise adding chlorobenzene while stirring in 1.5-2.5 h, covering the lid, and displacing the air with nitrogen two times; slowly heating to 190 to 240 DEG C while stirring, preserving the temperature and stirring for reaction; slowly cooling, filtering solid, recovering the solvent, purifying and distilling to obtain diphenyl sulfide. The novel method of the invention uses chlorobenzene and sodium sulfide as raw materials to prepare diphenyl sulfide by using. Compared with the prior art in the market, the method has the advantages of low raw material cost, safe and convenient operation, environment-friendliness, less three wastes and high yield, and is suitable for industrial production; and the product quality is in line with international standards.

Description

technical field [0001] The invention relates to a new method for preparing diphenyl sulfide, which belongs to the field of organic chemistry. Background technique [0002] Diphenyl sulfide is used as an intermediate for pesticides, medicines, and dyes. This product is also a catalyst for the synthesis of 2,4-dichlorophenol, pesticide herbicides (benben, 2,4-D), insecticide ibifos (EPBP), veterinary drug Dukesan, etc.; it is used in the synthesis of thiobis Dichlorophenol etc. [0003] There are mainly three preparation methods for diphenyl sulfide in the market: 1. First mix benzene and aluminum trichloride, cool to a certain temperature, and add a solution of sulfur chloride and benzene dropwise under stirring. At the beginning of the reaction, hydrogen chloride and a small amount of hydrogen sulfide are released, and a yellow viscous aluminum trichloride complex is precipitated. After the reaction is completed, diphenyl sulfide is obtained through a series of post-treat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C323/09
Inventor 王耀良刘必焕
Owner 兰州诚胜化工科技有限公司
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