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A kind of method for preparing high-purity ethylene sulfide

A high-purity technology of ethylene sulfide, which is applied in the field of preparation of high-purity ethylene sulfide, can solve the problems of high risk of flushing materials, easy safety accidents, and difficulty in effective condensation and recovery of ethylene sulfide, so as to improve the purity , high yield, and the effect of reducing the generation of impurities

Active Publication Date: 2021-04-16
保定加合精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the temperature rises rapidly, the risk of flushing is high, and it is difficult to effectively condense and recover ethylene sulfide, which is prone to safety accidents

Method used

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  • A kind of method for preparing high-purity ethylene sulfide
  • A kind of method for preparing high-purity ethylene sulfide
  • A kind of method for preparing high-purity ethylene sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 220 kg of ethylene carbonate (0.52 times the total amount of ethylene carbonate) in the reaction tank, heat to 55 ° C to melt, stir, add 375 kg of sodium thiocyanate, directly open the steam to heat up to 85 ° C, after the fraction is removed, the The coil condenser and the cyclone separator separated and collected fractions, and at the same time, 200 kg of ethylene carbonate remaining at a temperature of 75°C was added dropwise, and the dropping process controlled the temperature at 100°C. Continue to heat up to 138°C after the addition of sulfide, and stop the reaction until no fraction can be evaporated. The chemical reaction and operation of this step were stable, and it took 2 hours to obtain 270.8 kg of ethylene sulfide, the gas phase detection purity was 99.6%, and the yield was 97.5%.

[0028] Transfer 270.8kg of the ethylene sulfide fraction to a 1000L autoclave, add 330kg of diethylamine, and stir in a closed manner, raise the temperature to 125°C, and kee...

Embodiment 2

[0031] This embodiment is a small test carried out in the laboratory, the main purpose is to test the technical effect of the two-step feeding.

[0032] Add 200g of ethylene carbonate (0.49 times the total amount of ethylene carbonate) into the four-necked bottle, heat to 50°C to melt, stir, add 375g of sodium thiocyanate, heat the oil bath to 95°C, and start to drop the distillate The remaining temperature is 208g of ethylene carbonate at 65°C, and the dropwise addition process controls the temperature at 110°C. Continue to heat up to 136°C after the addition of sulfide, and stop the reaction until no distillate is evaporated. The reaction in this step lasted for 1 hour, and 270.1 g of ethylene sulfide was obtained, the gas phase detection purity was 99.3%, and the yield was 97.2%.

[0033]Transfer 270 g of the ethylene sulfide fraction to a 1-liter autoclave, add 329 g of diethylamine, and stir in an airtight manner, heat up to 128° C., and keep the pressure at 0.4 MPa for ...

Embodiment 3

[0035] This embodiment is a small test carried out in the laboratory, the main purpose is to verify the reliability of the technical effect of the two-step feeding.

[0036] Add 260g of ethylene carbonate to the four-necked bottle, heat to 55°C to melt, stir, add 443g of potassium thiocyanate, heat up the oil bath to 100°C, and start to drop the remaining 160g of ethylene carbonate at 75°C after the distillate , The dropping process controlled the temperature at 105°C. Continue to heat up to 129°C after the addition of sulfide, and stop the reaction until no fraction can be evaporated. The reaction in this step lasted 1.2 hours, and 267.2 g of ethylene sulfide was obtained, the gas phase detection purity was 99.2%, and the yield was 97.5%.

[0037] Transfer 267.1 g of the ethylene sulfide fraction to a 1-liter autoclave, add 325 g of diethylamine, and stir in an airtight manner, raise the temperature to 120° C., and keep the pressure at 0.5 MPa for 1 hour to complete the reac...

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Abstract

The invention provides a method for preparing high-purity ethylene sulfide, comprising the steps of: (1) firstly put in a part of ethylene carbonate preheated to liquefaction according to 0.2 to 0.7 times of the total amount of ethylene carbonate, stir, and control the temperature at 40 to 40 70°C, then add thiocyanate, and rapidly raise the temperature to 75-105°C; (2) Use a condensation system combined with a gas-liquid separator to collect the thiamine produced by the reaction, and start to drop the remaining temperature at 45-105°C. For ethylene carbonate at 85°C, the temperature is controlled between 80°C and 110°C during the dropwise addition process, and the temperature continues to rise to 130°C to 140°C after the dropwise addition, until no distillate is evaporated, and the reaction is ended. The method of the invention avoids the risk of punching materials, has short reaction time, and produces few impurities; the yield of the obtained product thimble is as high as 97%, and the gas-phase detection purity of the product reaches 99%.

Description

technical field [0001] The invention relates to the technical field of production of pharmaceutical intermediates, in particular to a method for preparing high-purity thimble. Background technique [0002] Diethylaminoethanethiol is an important intermediate for the synthesis of veterinary drug tiamulin. There are many synthetic methods of diethylaminoethanethiol reported in the literature, but there are two main industrial production processes at present: the first is diethylaminoethanethiol After chlorination, ethanol reacts with thiourea to generate S-substituted isothiourea salt, which is hydrolyzed with a strong base to obtain diethylaminoethanethiol; the second is first formed by the reaction of ethylene carbonate and thiocyanate Sulfur, and then diethylamine and sulphide react to generate diethylaminoethanethiol. The first process has high costs, long routes, heavy pollution, and poor operating conditions, and has been gradually eliminated; the second process is simp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D331/02
CPCC07D331/02
Inventor 余伟刘美龙张颖丽
Owner 保定加合精细化工有限公司
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