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Prepn of 1,1,1,3,3,3-hexachloropropane

A technology of hexachloropropane and carbon tetrachloride, applied in 1 field, can solve the problems of low reaction yield, many by-products, long reaction time, etc., and achieve the effect of shortening the reaction time and increasing the yield

Inactive Publication Date: 2003-05-14
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

We react according to the optimal conditions of this patented technology. The reaction time is 16 hours, the reaction conversion rate is close to 100%, there are many by-products, and the reaction selectivity is lower than 80%. When the reaction time is 4 hours, the reaction yield is lower than 65%.
[0008] In summary, in the preparation method of 1,1,1,3,3,3-hexachloropropane, the ubiquitous reaction time is long, and the problem of low reaction yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 600ml titanium alloy belt stirring autoclave, 110 grams of acetonitrile, 0.14 grams of copper chloride, 1 gram of cuprous chloride, 0.059 grams of isopropylamine, 1.79 grams of diethylene glycol dimethyl ether, and 317.5 grams of carbon tetrachloride were added simultaneously. Join in the reaction kettle, replace the oxygen in the kettle with nitrogen, then add 100 grams of vinylidene chloride to carry out addition reaction, the reaction temperature is 120 ° C, the reaction time is 4 hours, after the reaction, the crude product is distilled under reduced pressure to remove the solvent, and the solvent is recycled. , continue to distill under reduced pressure to obtain hexachloropropane, and the yield of hexachloropropane is 76% in terms of vinylidene chloride.

Embodiment 2

[0018] In a 600ml pure titanium belt stirring autoclave, 55 grams of acetonitrile, 3.4 grams of cupric chloride, 0.5 grams of cuprous chloride, 2.9 grams of isopropylamine, 179.5 grams of diethylene glycol dimethyl ether, and 396.9 grams of carbon tetrachloride were added simultaneously. Join in the reaction kettle, replace the oxygen in the kettle with nitrogen, then add 100 grams of vinylidene chloride to carry out the addition reaction, the reaction temperature is 150 ° C, and the reaction time is 6 hours. After the reaction, the crude product is distilled under reduced pressure to remove the solvent and the solvent is recycled. , continue to distill under reduced pressure to obtain hexachloropropane, and the yield of hexachloropropane is 85% in terms of vinylidene chloride.

Embodiment 3

[0020] In a 600ml titanium alloy belt stirring autoclave, 126.8 grams of acetonitrile, 5.4 grams of copper chloride, 2.0 grams of cuprous chloride, 6.0 grams of isopropylamine, 20.7 grams of diethylene glycol dimethyl ether, and 476.3 grams of carbon tetrachloride were added simultaneously. Join in the reaction kettle, replace the oxygen in the kettle with nitrogen, then add 100 grams of vinylidene chloride to carry out the addition reaction, the reaction temperature is 130 ° C, the reaction time is 4.5 hours, and the crude product after the reaction is decompressed and distilled to remove the solvent, and the solvent is recycled. , continue to distill under reduced pressure to obtain hexachloropropane, and the yield of hexachloropropane is 80% in terms of vinylidene chloride.

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PUM

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Abstract

The present invention discloses a preparation process of 1,1,1,3,3,3-hexachloropropane. Carbon tetrachloride, vinylidene chloride, solvent and catalyst are mixed and is subjected to addition reactionto produce, 1,1,1,3,3,3-hexachloropropane. In acetonitrile solvent, the molar ratio between carbon tetrachloride and vinylindene chloride is 2-5, and the reaction temperature is 120-150 deg.c. It is characterized by the catalyst including main catalyst copper chloride and cuprous chloride and cocatalyst isopropyl amine; the solvent including main solvent acetonitrile and cosolvent diethanediol dimethyl ether; and the reaction time of 4-6 hr. The present invention has short reaction time and high reaction yield.

Description

technical field [0001] The present invention relates to a preparation method of 1,1,1,3,3,3-hexachloropropane. Background technique [0002] 1,1,1,3,3,3-Hexachloropropane is a raw material for the synthesis of 1,1,1,3,3,3-hexafluoropropane. The main purpose of 1,1,1,3,3,3-hexafluoropropane is to replace Hallon1211 fire extinguishing agent. It has good fire extinguishing performance and zero ODP value. It is a green and environmentally friendly product. Therefore, 1,1,1,3,3,3-Hexachloropropane synthesis methods are increasingly showing importance. [0003] There are many reports about the synthesis method of 1,1,1,3,3,3-hexachloropropane abroad, and the method for the addition of vinylidene chloride and carbon tetrachloride is one of the paths, which consumes tetrachloride. attention has been paid to carbon materials. [0004] The synthetic method of 1,1,1,3,3,3-hexachloropropane is that vinylidene chloride and carbon tetrachloride carry out an addition r...

Claims

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Application Information

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IPC IPC(8): C07C17/278C07C19/01
Inventor 蒋琦
Owner JUHUA GRP
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