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Process for the continuous preparation of 1,1,1,2,3-pentachloropropane

A technology of pentachloropropane and trichloropropene, applied in the direction of halogen addition preparation, etc., can solve the problems of high solubility and complicated treatment, and achieve the effects of promoting mass transfer, high reaction efficiency and low reaction temperature

Active Publication Date: 2017-07-07
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses ferric chloride as a Lewis acid catalyst, which easily leads to the substitution reaction of chlorine. In addition, due to the high solubility of ferric chloride in halogenated hydrocarbons, the post-reaction treatment is more complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1,1,1,3-Tetrachloropropane was dehydrochlorinated under the action of 30% sodium hydroxide aqueous solution at 80°C to obtain a trichloropropene mixture, in which the ratio of HCC-1240zf to HCC-1240za was 58.5:41.5. A glass tube with a length of 30 cm and a diameter of 2.4 cm is used as a tubular reactor, and a ceramic ring filler is placed inside, and the above-mentioned trichloropropene raw material is injected into the reactor with a metering pump at 4.5 mL / min, and the chlorine flow rate is controlled at the same time. 3.3g / min, the reaction is carried out at normal temperature and pressure, the reaction residence time is 0.5 hours, the reaction product is analyzed by gas chromatography, the average conversion rate of trichloropropene reaches 99.1%, 1,1,1,2,3-pentachloro The average selectivity to propane was 98.5%.

Embodiment 2

[0028] The ratio of HCC-1240zf to HCC-1240za in the trichloropropene mixture was adjusted to 35.3:64.7, and the rest of the preparation process was the same as in Example 1. The reaction products were analyzed by gas chromatography. The average conversion rate of trichloropropene was 98.3%, and the average selectivity of 1,1,1,2,3-pentachloropropane was 98.1%.

Embodiment 3

[0030] Trichloropropene is completely with HCC-1240zf as raw material, passes into tubular reactor by the method for embodiment 1, analyzes the reaction product with gas chromatography, and the average conversion rate of trichloropropene reaches 100%, 1,1,1,2, The average selectivity of 3-pentachloropropane was 98.3%.

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Abstract

The invention discloses a continuous preparation method of 1,1,1,2,3-pentachloropropane. Firstly, trichloropropene and chlorine gas undergo a gas-liquid phase chlorination reaction to generate 1,1,1,2,3-pentachloropropane. The crude chloropropane is purified by rectification to obtain 1,1,1,2,3-pentachloropropane. The technology provided by the invention does not need to use a catalyst, does not need to be illuminated, has a simple operation process, and has high gas-liquid two-phase mass transfer efficiency of raw materials.

Description

technical field [0001] The present invention relates to a continuous process for the preparation of 1,1,1,2,3-pentachloropropane. Background technique [0002] 1,1,1,2,3-Pentachloropropane (HCC-240db) can be prepared by reacting trichloropropene obtained by dehydrochlorination of 1,1,1,3-tetrachloropropane with chlorine gas. [0003] In the prior art, the preparation process of HCC-240db is described as follows: [0004] (1) Japanese Patent Laid-Open 2010-248104 and World Patent WO2010123148 ​​reported the preparation method of HCC-240db, using 1,1,1,3-tetrachloropropane as raw material and dehydrochlorination with alkali to obtain a mixture of trichloropropene, the product HCC-240db can be obtained by passing chlorine gas under UV light irradiation without separation. The selectivity of HCC-240db reaches 93%, and the conversion rate of olefins reaches 97%. High-purity HCC-240db can be obtained by fractional distillation under reduced pressure. The chlorination reaction of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/01C07C17/04
Inventor 刘毓林张勇耀徐卫国杨箭
Owner SINOCHEM LANTIAN
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