Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of separation method of chloropyridine mixture

A separation method, the technology of chloropyridine, which is applied in the chemical industry and chemical fields, can solve the problems of poor product purification quality, harsh equipment requirements, and large solvent usage, so as to reduce purification costs, reduce equipment requirements, and stabilize product quality. Effect

Active Publication Date: 2017-12-08
LIER CHEM CO LTD
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the invention of the present invention is: when adopting the existing method to purify the crude product of 2,3,5,6-tetrachloropyridine, the ubiquitous high energy consumption, harsh equipment requirements, large solvent usage, more three wastes, and product purification For the problem of poor quality, provide a method for separating chloropyridine mixtures, especially the separation method for mixtures of 2,3,5,6-tetrachloropyridine and pentachloropyridine

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
  • A kind of separation method of chloropyridine mixture
  • A kind of separation method of chloropyridine mixture
  • A kind of separation method of chloropyridine mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The mixture of 2,3,5,6-tetrachloropyridine and pentachloropyridine is used as component one, wherein the mixture of 2,3,5,6-tetrachloropyridine and 2,3,4,5,6-pentachloropyridine The mass ratio is 98:2. Add 100g of component one and 350g of ethanol to a 1L reaction bottle, stir and dissolve at room temperature, then add dropwise an aqueous solution of sodium sulfide (the aqueous solution of sodium sulfide contains 0.32g of sodium sulfide and 2g of water) into the reaction bottle, after the addition is complete, keep the temperature for reaction 3h. After the reaction is completed, the reaction liquid is subjected to vacuum distillation to remove the organic solvent, and then the distilled reaction liquid is filtered and washed with water to obtain a solid and a mother liquid respectively. The quality of solid is 97g, and wherein 2,3,5,6-tetrachloropyridine content is 99.7% (that is the purity of 2,3,5,6-tetrachloropyridine is 99.7wt%; Contains 2,3,5 , The content of 6-...

Embodiment 2

[0035]The mixture of 2,3,5,6-tetrachloropyridine and pentachloropyridine is used as component one, wherein the mixture of 2,3,5,6-tetrachloropyridine and 2,3,4,5,6-pentachloropyridine The mass ratio is 80:20. Add 100g of component one and 400g of isopropanol to a 1L reaction flask, heat up to 80°C for dissolution, then add dropwise an aqueous solution of sodium sulfide (the aqueous solution of sodium sulfide is formed by mixing 6.5g of sodium sulfide and 35g of water) into the reaction flask, After the dropwise addition, the reaction was incubated for 3 hours. After the reaction is finished, the reaction liquid is subjected to vacuum distillation to remove the organic solvent, and then the distilled reaction liquid is filtered and washed with water to obtain 2,3,5,6-tetrachloropyridine solids and 2,3,5,6- Mother liquor of tetrachloropyridine-4-sulfur sodium salt. The quality of solid is 78.3g, wherein the content of 2,3,5,6-tetrachloropyridine is 99.5%; the content of 2,3,5,...

Embodiment 3

[0037] The mixture of 2,3,5,6-tetrachloropyridine and pentachloropyridine is used as component one, wherein the mixture of 2,3,5,6-tetrachloropyridine and 2,3,4,5,6-pentachloropyridine The mass ratio is 85:15. Add 100g component one and 350g toluene in 1L reaction bottle, be warmed up to 60 ℃ and dissolve, then add dropwise sodium sulfide aqueous solution (this sodium sulfide aqueous solution contains 4.8g sodium sulfide and 28g water) in reaction bottle, after dropwise addition, Keep warm until the reaction is complete. The reaction liquid was distilled under reduced pressure to remove toluene, and then the distilled reaction liquid was filtered and washed with water to obtain 2,3,5,6-tetrachloropyridine solids and 2,3,5,6-tetrachloropyridine-containing Mother liquor of 4-sulfur sodium salt. The mass of the solid was 83g, and the content of 2,3,5,6-tetrachloropyridine was 99.8%; the content of 2,3,5,6-tetrachloropyridine-4-sulfur sodium salt in the mother liquor was 98.5%. ...

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 separating a chloropyridine mixture, and the purpose of the invention is to solve the problems of high energy consumption, critical equipment requirement, large solvent usage amount, more 'three wastes (waste gas, waste water and industrial residue)' and bad product purification quality commonly existed in purification of 2,3,5,6-tetrachloropyridine by using a prior art A metal sulfide and 2,3,4,5,6-pentachloropyridine are reacted for generating 2,3,5,6-tetrachloropyridine-4-sulfosalt, by using a characteristic that 2,3,5,6-tetrachloropyridine is hard to dissolve in water and 2,3,5,6-tetrachloropyridine-4-sulfosalt is easy to dissolve in water, a high efficiency separation of 2,3,5,6-tetrachloropyridine and 2,3,5,6-tetrachloropyridine-4-sulfosalt is realized, and two useful fine chemical intermediates are obtained.

Description

technical field [0001] The invention relates to the fields of chemistry and chemical industry, especially the field of fine chemical industry, and relates to a method for preparing pesticide and pharmaceutical intermediates, in particular to a method for separating chloropyridine mixtures. Background technique [0002] 2,3,5,6-Tetrachloropyridine is an important pharmaceutical and pesticide intermediate, which can be used to synthesize insecticide chlorpyrifos, herbicide triclopyr, etc., and has broad application prospects. At present, the synthesis methods of 2,3,5,6-tetrachloropyridine mainly include the chlorination method, the dechlorination method of pentachloropyridine, and the molecular closing and ring-forming method. Among them, when 2,3,5,6-tetrachloropyridine is synthesized by pentachloropyridine dechlorination method, a large amount of three wastes (ie waste water, waste gas, waste residue) will be produced, and the utilization rate of atoms is low, which has bee...

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 Patents(China)
IPC IPC(8): C07D213/61C07D213/70
CPCC07D213/61C07D213/70
Inventor 任杰范谦晏三军刘强杨辉李建伟
Owner LIER CHEM CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com