A kind of preparation method of 1,1,1,3-tetrachloropropane

Abstract

The invention discloses a preparation method of 1,1,1,3-tetrachloropropane. Carbon tetrachloride and an auxiliary agent are mixed, preheated and forced to circulate for a period of time, and then reacted with ethylene in an intensified reactor for forced circulation. The crude product of 1,1,1,3-tetrachloropropane was obtained, which was finally separated by vacuum distillation to obtain 1,1,1,3-tetrachloropropane. The method for preparing 1,1,1,3-tetrachloropropane provided by the present invention has simple process, low energy consumption, and easy control of the reaction process. 75% to 95% of the residual liquid in the second rectification column can be recycled, with high material utilization rate, less waste generation, and high purity of the target product. At the same time, the use of ammonia-nitrogen-free and phosphorus-free catalysts solves the problem of nitrogen and phosphorus. The pollution of the three wastes is highly efficient and environmentally friendly.

Description

Technical field [0001] The present invention relates to the preparation method of 1,1,1,3-tetrachloropropane, and more particularly to a method of preparing 1,1,1,3-tetrachloropropane based on carbon chloride and ethylene as a raw material. Background technique [0002] 1,1,1,3-tetrachloropropane, referred to as HCC-250FB, is an important fine chemical, which can be used as a lacquer, a degreaser, and an organic synthetic raw material, for example for the preparation of 1-chloro-3, 3,3-trifluoropropane, 3,3,3-trifluoropropylene or HCC-240dB. [0003] Currently, there have been a variety of methods for preparing 1,1,1,3-tetrachloropropane, including the preparation of ethylene and tetrachloride as a raw material. For example, T.asahara et al. Found that ethylene and tetrachloride were catalyzed with triethylate-hexahydroformation of phosphite, and the process of 1,1,1,3-tetrachloropropane can be prepared. U.S. Patent US 4,43607 has been improved to the preparation method of T.asah...

AI Technical Summary

Problems solved by technology

In U.S. Patent US2004225166, a kind of technology that adopts iron and tributyl phosphate as catalyst to prepare 1,1,1,3-tetrachloropropane is reported, adopting this technology is easy to produce phosphorus-containing waste water, pollutes environment, in addition, solid iron powder is in It cannot be effectively dispersed in the raw materials during the reaction process, so it cannot be added quantitatively, which will easily lead to excessive local catalysts during the reaction process and cause polymerization reactions, resulting in an increase in high polymers

Therefore, the traditional 1,1,1,3-tetrachloropropane synthesis process uses iron powder, ferric chloride and phosphate ester system catalysts to telomerize carbon tetrachloride and vinyl chloride to prepare, but the use of phosphorus-containing catalysts is easy to produce phosphorus-containing The three wastes cause great environmental pollution and difficult post-treatment; in addition, the iron powder used is easy to agglomerate on the surface of the reactor after the reaction, making it difficult to clean up, and the fine iron powder is dispersed in the organic high-boiler, resulting in high consumption and separation Difficult to reuse

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