Industrial production method of 2-chloro-5-trichloromethyl pyridine

A technology of trichloromethylpyridine and chloromethylpyridine, which is applied in the industrial production field of 2-chloro-5-trichloromethylpyridine, and can solve the problems of long reaction time of catalyst, high reaction yield, influence on equipment productivity and the like , to avoid the darkening of the material color, increase the liquid phase chlorination temperature, and achieve the effect of fast reaction speed

Active Publication Date: 2016-03-30
连云港埃森化学有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a high reaction yield and less impurities. The disadvantage is that the reaction time without catalyst is long, which affects the equipment capacity.

Method used

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  • Industrial production method of 2-chloro-5-trichloromethyl pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 200kg of 2-chloro-5-chloromethylpyridine and 150kg of 4-chlorobenzotrifluoride to a 500L glass-lined reactor. After the reactor is heated to 120°C, chlorine gas is introduced, and ultraviolet light is turned on to initiate the reaction. Keep the reaction temperature at 120°C , after reacting for 30 hours, sample GC analysis, when 2-chloro-5-trichloromethylpyridine content ≥ 90.0%, stop chlorine gas feed; feed N 2 Until the tail gas is neutral, the temperature of the reaction kettle is lowered to 80°C, and put into the rectification kettle; under the conditions of a pressure of 2kpa, a temperature of the kettle of 110°C, a temperature of the top of the rectification tower of 64°C, and a reflux ratio of 6:1, the solvent is recovered, and the Under the conditions of 600Pa pressure, 160℃ kettle temperature, 114℃ rectification tower top temperature and 6:1 reflux ratio, 214kg of 2-chloro-5-trichloromethylpyridine was collected, with a content of 99.21%, and a melting poin...

Embodiment 2

[0029] Add 200kg of 2-chloro-5-chloromethylpyridine and 150kg of 3,4-dichlorobenzotrifluoride to a 500L glass-lined reactor. After the reactor is heated to 120°C, chlorine gas is introduced, and ultraviolet light is turned on to initiate the reaction. Reaction temperature to 160°C, keep 160°C for 12 hours, sample GC analysis, when the content of 2-chloro-5-trichloromethylpyridine is ≥90.0%, stop the introduction of chlorine gas; 2 Until the tail gas is neutral, the temperature of the reaction kettle is lowered to 80°C, and put into the rectification kettle; under the conditions of 2kpa pressure, 110°C kettle temperature, 87°C rectification column top temperature, and a reflux ratio of 6:1, the solvent is recovered, and the Under the conditions of 600Pa pressure, 160°C kettle temperature, 114°C rectification tower top temperature, and 6:1 reflux ratio, 243kg of 2-chloro-5-trichloromethylpyridine was collected with a content of 99.21% and a melting point of 53-55°C. The total yi...

Embodiment 3

[0031] Operate with embodiment 1, reaction temperature 80 ℃, reaction time 120hr. 202kg of 2-chloro-5-trichloromethylpyridine was obtained, with a content of 99.03% and a melting point of 53-55°C. The total yield is 70.9%.

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Abstract

The invention discloses an industrial production method of 2-chloro-5-trichloromethyl pyridine, belonging to the technical field of pesticide chemical. The industrial production method of 2-chloro-5-trichloromethyl pyridine comprises the following steps: with 2-chloro-5-chloromethyl pyridine as a start raw material, introducing gaseous chlorine into the solvents such as trifluoromethyl monochlorobenzene, trifluoromethyl dichlorobenzene and trifluoromethyl trichlorobenzene at 80-205 DEG C; initiating a chlorination reaction through ultraviolet irradiation to obtain a crude product of 2-chloro-5-trichloromethyl pyridine directly by one-step chlorination, wherein the content of 2-chloro-5-trichloromethyl pyridine in the crude product is higher than or equal to 90%; and purifying the crude product by a rectifying process to obtain a product of 2-chloro-5-trichloromethyl pyridine, wherein the purity is higher than or equal to 99.0%. The method disclosed by the invention overcomes the shortcomings of the existing production method such as long reaction time, low reaction selectivity, high polymer generation and low yield; and without a catalyst, the reaction selectivity and yield are increased, the reaction is accelerated, and the industrial production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of pesticide chemical industry, in particular to an industrial production method of 2-chloro-5-trichloromethylpyridine. Background technique [0002] 2-Chloro-5-trichloromethylpyridine is an intermediate in the synthesis of 2-chloro-5-trifluoromethylpyridine and 2,3-dichloro-5-trifluoromethylpyridine, and it is also An important intermediate of Zonglong, it has a broad market prospect. 2-Chloro-5-trifluoromethylpyridine is the key intermediate for the synthesis of fluazifop-pyl, and 2,3-dichloro-5-trifluoromethylpyridine is The key intermediate of amide. [0003] The preparation of 2-chloro-5-trichloromethylpyridine generally has the following methods: method one (CN201310261224.3, CN201210505004.6, CN201010521968.0, CN00122987.7) uses 2-chloro-5-methylpyridine as Raw materials, using azobisisobutyronitrile, phosphorus trichloride, ammonium persulfate and benzoyl peroxide and photoinitiator, using dichlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 李惠跃金克强吴雨明赵羽冲金浩峰
Owner 连云港埃森化学有限公司
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