One-step synthesis of ethyl isocyanate

A technology of ethyl isocyanate and trichloromethyl carbonate, applied in the field of chemistry, can solve the problems of pollution, high cost, dangerous degree of light-passing process and the like

Active Publication Date: 2012-09-12
平原倍斯特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In order to overcome the deficiencies in the prior art, the present invention aims to provide a method for synthesizing ethyl isocyanate in one step to solve the problem that phosgene is used in the above-mentioned conventional synthesis method, and the light-passing process in the production process has a high degree of danger, serious pollution, and high cost. , poor quality and other issues

Method used

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  • One-step synthesis of ethyl isocyanate
  • One-step synthesis of ethyl isocyanate
  • One-step synthesis of ethyl isocyanate

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Embodiment Construction

[0024] 1. Catalyst preparation: Mix commercially available alkylammonium salts and benzylammonium groups at a ratio of 1:4.2, reflux in ether solvent for 1 hour at the boiling point, cool down, centrifuge, dry, and pulverize for later use.

[0025] 2. Synthesis of the target product:

[0026] 180kg of ethylamine hydrochloride and mixed xylene were thrown into the reaction kettle and refluxed at 138°C to separate the water until the water content was ≤200ppm.

[0027] Cool down to below 40°C, add 8kg of catalyst and 260kg of trichloromethylcarbonate to rise through the program, keep warm to 135-137°C, add the xylene solution of trichloromethylcarbonate dropwise at 28kg / h at this temperature, the central control Analyze until the reaction is complete.

[0028] 3. Separation of the target product: Put the synthesis solution in a rectification kettle (number of plates: 40) and raise the temperature to reflux, completely remove the acid gas, and receive the target product at 60°C,...

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Abstract

The invention relates to one-step synthesis of ethyl isocyanate, which belongs to the chemical technical field. The method abandons a process of phosgene feeding in routine techniques, and uses xylene as a solvent.150-200 kg ethylamine hydrochloride is dissolved in 400-600 L xylene; the xylene solution containing 200-300 kg trichloromethyl carbonate is added into a reaction vessel in a dropwise manner with the presence of 5-10 kg of a catalyst; and the following steps are carried out: preparation of a catalyst, synthesis of a target product, separation of the target product, synthesis of ethyl isocyanate, and preparation of the product after separation. The method in the invention abandons the process of phosgene feeding in the routine techniques, and uses xylene as the solvent. The method effectively solves the problems of high risk, severe pollution, high cost and poor quality and the like in the process of phosgene feeding in the productive process in the routine techniques that use phosgene.

Description

technical field [0001] The invention belongs to the technical field of chemistry and relates to a synthesis technology of ethyl isocyanate (ethyl isocyanate). Background technique [0002] The general formula is [0003] [0004] Ethyl isocyanate belongs to a kind of pharmaceutical intermediate, its main use is to produce alfentanil; to manufacture heat-resistant polyurethane elastomer (used in sealing strips, etc.); [0005] Antiallergic drugs: 4-piperidinemethylpurine; derivative medical antihistamines; 2-heterocycloalkylimidazopyridine; [0006] Analgesics: N-phenyl-N-(4-piperidinyl)amine derivatives; [0007] Antibacterial drugs: cephalosporins containing sulfonyl imidazolidinone substituents, etc. [0008] At present, the synthesis method of ethyl isocyanate is mainly the phosgene method, directly passing excessive phosgene into the xylene solution of ethylamine hydrochloride, finally detecting the end point, catching light, and distilling to obtain the finished p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/04C07C263/10
Inventor 武淑勇
Owner 平原倍斯特化工有限公司
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