Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF9 Cites 7 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com