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A kind of preparation technology of ethylene sulfide

A technology for the preparation of ethylene sulfide, which is applied in the field of preparation technology of ethylene sulfide, can solve the problems of unstable properties of ethylene sulfide, reaction efficiency of side reactions, and high odor and toxicity, so as to improve synthesis efficiency and prolong The residence time, the effect of lengthening the condensation process

Active Publication Date: 2016-09-07
张丽学
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Chinese patent ZL200810080197.9 discloses a preparation method of diethylaminoethanethiol, which uses ethylene carbonate and anhydrous thiocyanate to react to generate thioethylene, cyanate and carbon dioxide, and the generated gas and carbon dioxide are directly Emission, due to the low boiling point of sulfide at about 55°C, and the stench and toxicity, at 80°C to 100°C, sulfide is easily discharged into the atmosphere together with carbon dioxide to cause environmental pollution, and sulfide Unstable in nature, it is easy to open the ring and undergo polymerization reaction in the presence of nucleophile. The polymerization equation of thioethylene is However, water has a certain nucleophilicity, and the presence of water and air in the reaction environment will cause side reactions to occur and the reaction efficiency is low.

Method used

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  • A kind of preparation technology of ethylene sulfide
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Effect test

Embodiment 1

[0036] Add 89g of potassium thiocyanate into the closed reactor, heat the reactor to 180°C under a vacuum of -0.099MPa, start the stirrer for mechanical stirring after the potassium thiocyanate melts, and continue to raise the temperature of the reactor to 220°C After the potassium thiocyanate is completely melted, the water is distilled off for 1.0 hour, and then the reactor is cooled to below 40°C. After the potassium thiocyanate is solidified, nitrogen gas is filled into the reactor to a micro-pressure level of 0-0.3kpa, and 62g of carbonic acid is added. Vinyl ester, heat up slowly, the reactor is heated up to 80°C within 15 minutes, the mixture in the reactor starts to react and ethylene sulfide evaporates, maintain the reactor at 80°C for 1 hour, continue to heat the reactor to 100°C, When the reactor temperature reaches 130°C, the distillation ends, and 41.3g of ethylene sulfide is obtained by condensation at -5°C using a refrigerant containing ethylene glycol, and 0.2g ...

Embodiment 2

[0038] Add 75g of potassium thiocyanate into the closed reactor, heat the reactor to 170°C under a vacuum of -0.099MPa, start the stirrer for mechanical stirring after the potassium thiocyanate melts, and continue to raise the temperature of the reactor to 210°C After the potassium thiocyanate is completely melted, the water is distilled off for 0.8 hours, and then the reactor is cooled to below 40°C. After the potassium thiocyanate is solidified, the reactor is filled with nitrogen to a micro-pressure level of 0-0.3kpa, and 62g of carbonic acid is added. Vinyl ester, slowly raise the temperature, the reactor will heat up to 75°C within 15 minutes, the mixture in the reactor will start to react, and ethylene sulfide will evaporate, keep the reaction at 75°C for 1 hour, continue to heat the reactor and raise the temperature to 100°C, when the reaction Distillation ends when the temperature of the device reaches 125°C, and 41.2g of ethylene sulfide is obtained by condensation at ...

Embodiment 3

[0040] Add 71.5g of potassium thiocyanate into the closed reactor, heat the reactor to 160°C under a vacuum of -0.099MPa, start the stirrer for mechanical stirring after the potassium thiocyanate melts, and continue to raise the temperature of the reactor to 200 ℃, after the potassium thiocyanate is completely melted, the water is distilled off for 0.5 hours, and then the reactor is cooled to below 40 ℃. After the potassium thiocyanate is solidified, nitrogen gas is filled into the reactor to a micro-pressure level of 0-0.3kpa, and 62g Ethylene carbonate, heat up slowly, the reactor will be heated to 70°C within 15 minutes, the mixture in the reactor will start to react and ethylene sulfide will evaporate, keep the reaction at 70°C for 1 hour, continue to heat the reactor to 95°C, when When the temperature of the reactor reaches 120°C, the distillation ends, and 40.7g of ethylene sulfide is obtained by condensing at -5°C with a refrigerant containing ethylene glycol, and 0.2g o...

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Abstract

The invention discloses a preparation process of ethylene sulfide. The preparation process comprises the following steps: heating potassium thiocyanate at a vacuum condition for dehydrating; continuously charging nitrogen to protect the reaction until a reaction system is at a micro-pressure; subsequently adding ethylene carbonate to perform a synthetic reaction; condensing to obtain liquid ethylene sulfide. The reaction system is also provided with an ethylene sulfide tail gas adsorbing device and an air drying device so as to prevent polymerization reaction of ethylene sulfide, so that the preparation process of ethylene sulfide is little in side reaction, high in reaction yield and small in environmental pollution.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a preparation process of sulfide. Background technique [0002] Chinese patent ZL200810080197.9 discloses a preparation method of diethylaminoethanethiol, which uses ethylene carbonate and anhydrous thiocyanate to react to generate thioethylene, cyanate and carbon dioxide, and the generated gas and carbon dioxide are directly Emission, due to the low boiling point of sulfide at about 55°C, and the stench and toxicity, at 80°C to 100°C, sulfide is easily discharged into the atmosphere together with carbon dioxide to cause environmental pollution, and sulfide Unstable in nature, it is easy to open the ring and undergo polymerization reaction in the presence of nucleophile. The polymerization equation of sulfide is However, water has a certain nucleophilicity, and the presence of water and air in the reaction environment will lead to the occurrence of side react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D331/02
CPCC07D331/02
Inventor 张丽学
Owner 张丽学