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One-pot method for preparing 1,1,1,2,3-pentachloropropane with high selectivity and high yield

A pentachloropropane and tetrachloropropane technology, applied in the field of compound synthesis, can solve the problems of coking and blackening of the reaction solution, catalyst deactivation, and low yield

Active Publication Date: 2021-01-26
JIANGXI TIANYU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, in the existing preparation technology, in the presence of anhydrous iron trichloride Lewis acid catalyst, the dehydrochlorination reaction of polychlorinated hydrocarbons, there are various side reactions such as polymerization and isomerization
Especially when 1,1,1,3-tetrachloropropane is dehydrochlorinated to 1,1,3-trichloropropene, due to the presence of 1,1,3-trichloropropene allyl, in the presence of Lewis acid catalyst , the polymerization reaction is very easy to occur, so that the whole reaction solution is coked and blackened, and the catalyst is deactivated, so that the key intermediate 1,1,1,2,3-pentachloropropane in the preparation of 1,1,2,3-tetrachloropropene The yield becomes lower, resulting in a lower yield of 1,1,2,3-tetrachloropropene

Method used

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  • One-pot method for preparing 1,1,1,2,3-pentachloropropane with high selectivity and high yield
  • One-pot method for preparing 1,1,1,2,3-pentachloropropane with high selectivity and high yield

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 500mL three-necked flask, add 300g of 1,1,1,3-tetrachloropropane with a content of 98% (the total content of water, alcohol, amine and trialkyl phosphate is 0.2%, and the content of carbon tetrachloride is 1.70%) ), 0.45g anhydrous ferric trichloride, put into the water bath of 75 ℃, stirred and reacted for 40 minutes, at this moment, the content of detecting 1,1,3-trichloropropene was 16%, and the reaction solution became light yellow, and the The temperature of the reaction system is reduced to 55°C, and chlorine gas is introduced, and the temperature of the reaction system is slowly raised to 70°C, and the temperature of the reaction system is controlled to be stable at 72°C. Gas chromatography detects 1,1,3-trichloropropene (area normalization method), so that the content of 1,1,3-trichloropropene is kept at 3%, and a small amount of chlorine gas and hydrogen chloride gas produced are absorbed with liquid caustic soda After reacting with chlorine gas for four h...

Embodiment 2

[0039] In a 500mL three-necked flask, add 300g of 98% 1,1,1,3-tetrachloropropane (the total content of water, alcohol, amine and trialkyl phosphate is 0.05%, and the carbon tetrachloride content is 1.77%) ), 0.45g anhydrous ferric chloride, 0.15g iron powder, put into 80 ℃ water bath, stir and react for 30 minutes. It is light yellow, reduce the temperature of the reaction system to 50°C, start to feed chlorine gas, slowly raise the temperature of the reaction system to 65°C, control the temperature of the reaction system to be stable at 75°C, and pass the chlorine gas at a rate of , reaction solution sampling detects 1,1,3-trichloropropene (area normalization method) with gas chromatography so that 1,1,3-trichloropropene content remains on 6%, a small amount of chlorine that emerges and the hydrogen chloride gas that produces Absorbed with liquid alkali, reacted with chlorine gas for 3 hours, took the reaction solution and detected it by gas chromatography, there were unreact...

Embodiment 3

[0041] In a 500mL three-necked flask, add 300g of 98% 1,1,1,3-tetrachloropropane (the total content of water, alcohol, amine and trialkyl phosphate is 0.14%, and the carbon tetrachloride content is 1.73%) ), 3g anhydrous ferric trichloride, put into 70 DEG C of water baths, stir and react for 20 minutes, at this moment, the content of detecting 1,1,3-trichloropropene is 12%, and the reaction solution becomes pale yellow, and the reaction The temperature of the system was lowered to 65°C, and chlorine gas was introduced. The temperature of the reaction system was slowly raised to 75°C. The temperature of the reaction system was controlled to be stable at 75°C. Chromatography detects 1,1,3-trichloropropene (area normalization method,) to keep its content at 1%, a small amount of chlorine gas that emerges and the hydrogen chloride gas produced are absorbed with liquid caustic soda, and after 3.5 hours of chlorine gas reaction, take The reaction solution was detected by gas chroma...

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Abstract

The invention provides a method for preparing 1,1,1,2,3-pentachloropropane with high selectivity and high yield in a one-pot method. The method uses 1,1,1,3-tetrachloropropane as a raw material to remove Hydrogen chloride reaction to obtain 1,1,3-trichloropropene, when the content of 1,1,3-trichloropropene in the system reaches 4-20%, feed chlorine to react, after feeding chlorine, control 1,1, The content of 3-trichloropropene is 1-6%. When the content of 1,1,1,2,3-pentachloropropane generated in the system reaches 90-99%, stop the reaction. The present invention utilizes a one-pot method to prepare 1,1,1,2,3-pentachloropropane, by controlling the content of 1,1,3-trichloropropene in the system after the dehydrochlorination reaction and introducing chlorine gas, and controlling the generated The control of the content of 1,1,1,2,3-pentachloropropane can greatly reduce side reactions and improve the selectivity and yield of preparing 1,1,1,2,3-pentachloropropane.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis and relates to a method for preparing 1,1,1,2,3-pentachloropropane. In particular, it relates to a one-pot method for preparing 1,1,1,2,3-pentachloropropane with high selectivity and high yield. Background technique [0002] Chlorinated hydrocarbon compounds are often used as raw materials for the preparation of refrigerants, blowing agents, biocides and polymers. 1,1,2,3-Tetrachloropropene is one of the main intermediates for the preparation of the chemical herbicide tricamba, and it is also the main intermediate for the new generation of environmentally friendly refrigerant 2,3,3,3-tetrafluoropropene. The latest process for the preparation of 1,1,2,3-tetrachloropropene is obtained by dehydrochlorination of 1,1,1,2,3-pentachloropropane; the preparation of 1,1,1,2,3-pentachloropropene The main method of chloropropane is: use carbon tetrachloride and ethylene as raw materials to first ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/04C07C19/01C07C17/25C07C21/04
CPCC07C17/04C07C17/25C07C19/01C07C21/04
Inventor 尹笃林兰支利田晓宏肖自胜钟文周谢思勉彭鹏庞怀林刘忠德陈梦现周玲余一鸣
Owner JIANGXI TIANYU CHEM CO LTD
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