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

Method for producing 2-chloropyridine and 2,6-chloropyridine through organic solvent method

A technology for organic solvent and dichloropyridine, which is applied in the production of 2-chloropyridine and 2 fields by organic solvent method, can solve the problems of low economic benefit, by-products, difficult source of 2-hydroxypyridine, etc., achieves high economic value and is easy to use. separation effect

Inactive Publication Date: 2014-02-05
山东谦诚工贸科技有限公司
View PDF4 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The source of 2-hydroxypyridine is difficult, and phosgene needs to be introduced, so the operability is not good, and it is not conducive to environmental protection
[0013] The raw materials are easy to obtain, but there are protective gases such as nitrogen and carbon dioxide and catalysts, high process requirements, by-products, low single-pass yield, etc., and low economic benefits

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
  • Method for producing 2-chloropyridine and 2,6-chloropyridine through organic solvent method
  • Method for producing 2-chloropyridine and 2,6-chloropyridine through organic solvent method
  • Method for producing 2-chloropyridine and 2,6-chloropyridine through organic solvent method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Mix pyridine and carbon tetrachloride at a mass ratio of 1.5:1 to prepare 20Kg of pyridine solution, and vaporize the pyridine solution to obtain a vapor; mix the vapor and chlorine at a mass ratio of 1:1 Finally, the feed rate of 4Kg / h is sent to the kettle-type quartz reactor to make it react under the irradiation of ultraviolet lamps. The reaction pressure is controlled at -0.5 to -1.0KPa, the reaction temperature is controlled at 190-200 ° C, and the reaction is completed. After cooling, the reaction solution was obtained; the reaction solution was distilled to remove carbon tetrachloride, and then rectified under reduced pressure under the condition of -0.08 to -0.085MPa, and the fractions with a temperature range of 110-113°C were collected to obtain colorless 2-chloropyridine 3.1 Kg (purity 99.2%), collect fractions in the range of 142-146°C, white 2,6-dichloropyridine 16.8Kg (purity 99.0%), total yield 92.7%.

Embodiment 2

[0031] Mix pyridine and carbon tetrachloride at a mass ratio of 0.5:1 to prepare 20Kg of pyridine solution, and vaporize the pyridine solution to obtain a vapor; mix the vapor and chlorine at a mass ratio of 3:1 Finally, the feed rate of 7Kg / h is sent to the kettle-type quartz reactor to make it react under the irradiation of ultraviolet lamps. The reaction pressure is controlled at -0.5 to -1.0KPa, the reaction temperature is controlled at 180-210°C, and the reaction is completed. After cooling, the reaction solution was obtained; the reaction solution was distilled to remove carbon tetrachloride, and then rectified under reduced pressure under the condition of -0.08 to -0.085MPa, and the fractions with a temperature range of 110-113°C were collected to obtain colorless 2-chloropyridine 8.0 Kg (purity 99.6%), the fractions in the range of 142-146°C were collected to obtain 0.7Kg of white 2,6-dichloropyridine (purity 99.8%), and the total yield was 90.0%.

Embodiment 3

[0033] Mix pyridine and carbon tetrachloride at a mass ratio of 0.5:1 to prepare 20Kg of pyridine solution, and vaporize the pyridine solution to obtain a vapor; mix the vapor and chlorine at a mass ratio of 2.5:1 Finally, the feed rate of 7Kg / h is sent to the kettle-type quartz reactor to make it react under the irradiation of ultraviolet lamps. The reaction pressure is controlled at -0.5 to -1.0KPa, the reaction temperature is controlled at 180-210°C, and the reaction is completed. After cooling, the reaction liquid was obtained; the reaction liquid was distilled to remove carbon tetrachloride, and then rectified under reduced pressure under the condition of -0.08 to -0.085 MPa, and the fractions with a temperature range of 110-113 ° C were collected to obtain colorless 2-chloropyridine 7.1 Kg (purity 99.6%), the fractions in the range of 142-146°C were collected to obtain 2.7Kg of white 2,6-dichloropyridine (purity 99.8%), and the total yield was 97.3%.

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

No PUM Login to View More

Abstract

The invention discloses a method for producing 2-chloropyridine and 2,6-chloropyridine through an organic solvent method. The method comprises the following steps: mixing pyridine and carbon tetrachloride to form a pyridine solution according to a mass ratio of (0.2-2): 1, and vaporizing the pyridine solution to obtain a vaporized product; mixing the vaporized product and chlorine according to a mass ratio of (1-3): 1 and introducing the mixture into a reactor, so that the mixture reacts under the condition of 150-250 DEG C, and cooling to prepare a reaction solution after the reaction is ended; distilling the reaction solution to remove the carbon tetrachloride, performing rectification under reduced pressure under the condition of -0.08 to -0.085MPa, collecting fractions of which the temperature ranges from 110 DEG C to 113 DEG C to obtain the 2-chloropyridine, and collecting fractions of which the temperature ranges from 142 DEG C to 146 DEG C, thus obtaining the 2,6-chloropyridine. According to the method, protective gases such as nitrogen and carbon dioxide are not needed, a precious metal catalyst is not added, the pyridine is not needed to be directly chlorinated under high-pressure conditions, the yield is 90-98 percent, and the main byproduct 2,6-chloropyridine is an important chemical material, is easy to separate and has a relatively high economic value.

Description

technical field [0001] The invention relates to a method for producing 2-chloropyridine and 2,6-dichloropyridine by an organic solvent method. Background technique [0002] Pyridine is an important organic chemical raw material. Pyridine and its derivatives are widely used in medicine and pesticides due to their high efficiency, spectrum and low residue characteristics. Pyridine chloride is an important drug intermediate. 2-Chloropyridine is used in the production of shampoo and is widely used in the field of daily chemicals; The raw material of the medicine. 2. 6-Dichloropyridine has a great potential for development. Synthesis of drug intermediates is used as a fungicide, synthesis of Pirozadil is used to lower blood lipids and anti-platelet aggregation drugs; synthesis of muskpyridine, etc. [0003] The synthesis of 2-chloropyridine began in 1891. With the continuous improvement of experimental conditions and the gradual improvement of chemical theory, many new synthesi...

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
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 单永华孟庆浩
Owner 山东谦诚工贸科技有限公司
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