Synthesis technology for N,N-diethylamino group ethanethiol

A technology of diethylaminoethane mercaptan and synthesis process, which is applied in the field of N, can solve the problems of large volatilization loss of raw materials, long reaction time and high cost, and achieves the effects of small excess molar ratio of feeding materials, few kinds of raw materials and low production cost.

Active Publication Date: 2011-08-17
保定加合精细化工有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] This operational route uses sulfide and diethylamine to synthesize N,N-diethylaminoethanethiol by reflux reaction under catalyst conditions. Although this process is environmentally friendly, it can be completely reacted without using a solvent, thereby obtaining high-yield product, but the process has the following defects: the amount of diethylamine is large (the molar ratio of ethylene sulfide and diethylamine is 1:5), the price of the catalyst used is higher, the required reaction time is longer, and the raw materials volatilize Large losses, poor operating environment, high cost, and weak industrial competitiveness

Method used

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  • Synthesis technology for N,N-diethylamino group ethanethiol

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Embodiment 1

[0014] Press 80 kg of sulfide and 100 kg of diethylamine into a 500L autoclave with nitrogen, heat to 80°C with stirring, and seal the reaction. During the reaction, the pressure in the kettle rose up to 0.2MPa. As the reaction progressed, the pressure in the kettle dropped from the highest point. When the pressure in the kettle dropped to 0.02MPa, the reaction ended, and the reaction time was 3 hours. After the reaction was completed, the temperature was lowered to 50° C., and the material was put into a distillation kettle. Firstly, diethylamine was recovered by distillation, and then 170.2 kg of N,N-diethylaminoethanethiol was obtained by distillation under reduced pressure.

[0015] The mass percent content of N,N-diethylaminoethanethiol in this example is 99%. The product yield is 96%.

Embodiment 2

[0017] Press 250 kg of sulfide and 330 kg of diethylamine into a 2000L autoclave with nitrogen, heat to 90°C with stirring, and seal the reaction. During the reaction process, the pressure in the kettle rose to 0.3MPa at the highest. As the reaction progressed, the pressure in the kettle dropped from the highest point. When the pressure in the kettle dropped to 0.02MPa, the reaction ended, and the reaction time was 4 hours. After the reaction is completed, the temperature is lowered to 50° C., and the material is put into a distillation still. Firstly, diethylamine is recovered by distillation, and then 534.7 kg of N,N-diethylaminoethanethiol can be obtained by distillation under reduced pressure.

[0018] The mass percent content of N,N-diethylaminoethanethiol in this embodiment is 99%. The product yield is 96.5%.

Embodiment 3

[0020] Press 250 kg of sulfide and 330 kg of diethylamine into a 2000L autoclave with nitrogen, heat to 100°C with stirring, and seal the reaction. During the reaction, the pressure in the kettle rose up to 0.5MPa. As the reaction progressed, the pressure in the kettle dropped from the highest point. When the pressure in the kettle dropped to 0.02MPa, the reaction ended, and the reaction time was 4 hours. After the reaction is completed, the temperature is lowered to 50° C., and the material is put into a distillation kettle, diethylamine is recovered by distillation, and 530 kg of N,N-diethylaminoethanethiol can be obtained by distillation under reduced pressure.

[0021] The mass percent content of N,N-diethylaminoethanethiol in this embodiment is 99%. The product yield is 95.6%.

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Abstract

The invention discloses a synthesis technology for N,N-diethylamino group ethanethiol. The synthesis technology includes the steps of pressing ethane episulfide and diethylamine into a pressure reaction kettle by nitrogen, heating to the temperature of 80-100 DEG C in a closed state under the condition of stirring, and reacting for 3-5 hours to obtain the N,N-diethylamino group ethanethiol. The synthesis technology is finished in the closed reaction kettle by adopting the technical conditions as above, does not use any dissolvent or catalyst, does not generate by-product, and has the advantages of short technology flow, few material types, short reaction time and small excess of feed mole ratio of diethylamine to ethane episulfide; the mass percent of the prepared product can achieve 99%; and the whole production technology has the characteristics of low production cost, high yield, no exhaust of three wastes (waste gas, waste water, industrial residual), and the synthesis technology belongs to an environment-friendly chemical-industrial synthesis technology.

Description

technical field [0001] The invention relates to the technical field of mercaptans, in particular to a synthesis process of N, N-diethylaminoethanethiol. Background technique [0002] In the prior art (Chinese patent ZL200910300473.2), the disclosed N,N-diethylaminoethanethiol synthesis route is as follows: [0003] [0004] This operational route uses sulfide and diethylamine to synthesize N,N-diethylaminoethanethiol by reflux reaction under catalyst conditions. Although this process is environmentally friendly, it can be completely reacted without using a solvent, thereby obtaining high-yield product, but the process has the following defects: the amount of diethylamine is large (the molar ratio of ethylene sulfide and diethylamine is 1:5), the price of the catalyst used is higher, the required reaction time is longer, and the raw materials volatilize Large losses, poor operating environment, high cost, and weak industrial competitiveness. Contents of the invention ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/25C07C319/06
Inventor 赵云现李超
Owner 保定加合精细化工有限公司
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