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Method for preparing 2,6-dichloropyridine by pyridine liquid-phase photochlorination

A technology of dichloropyridine and pyridine chloride solution, applied in the directions of organic chemical methods, chemical instruments and methods, separation methods, etc., can solve the problems of large amount of three wastes, blockage of tail gas pipelines, etc., and achieve the effect of low cost and low energy consumption

Active Publication Date: 2019-01-04
ZHEJIANG AVILIVE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Design purpose: In order to avoid the deficiencies in the background technology, design a pyridine liquid phase that uses trifluoromethyl chlorobenzene as the solvent for the reaction of pyridine and chlorine to achieve the purity of the prepared 2,6-dichloropyridine product ≥ 99.0% The method for preparing 2,6-dichloropyridine by photochlorination overcomes the disadvantages of the large amount of three wastes produced in the preparation method of the background technology and the clogging of tail gas pipes by materials, reduces the discharge of three wastes, reduces production costs, is easier for industrial production, and achieves a purity of ≥99.0 Low pollution, low energy consumption and low cost for the preparation of %2,6-dichloropyridine products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: A method for preparing 2,6-dichloropyridine by liquid-phase photochlorination of pyridine, using pyridine and chlorine as starting materials, using trifluoromethyl chlorobenzene as solvent, at a temperature of 150°C to 210°C and Under the irradiation of ultraviolet light, the chlorination reaction of pyridine and chlorine is carried out continuously, and the pyridine chlorination liquid obtained by cooling the chlorination reaction product and the solvent is:

[0013] Using pyridine and chlorine gas as starting materials, trifluoromethyl chlorobenzene as solvent, continuous feed in the temperature range of 150°C to 210°C under the irradiation of ultraviolet light for liquid phase chlorination reaction, the obtained pyridine chlorination liquid .

[0014] In this embodiment, the weight ratio of pyridine to solvent is 1:0.2-4. At the beginning of the chlorination reaction, a certain amount of solvent is pre-added in the reaction chlorination reactor, heated to...

Embodiment 2

[0017] Embodiment 2: On the basis of Example 1, using pyridine and chlorine as starting materials, taking trifluoromethyl chlorobenzene after heating as solvent, pyridine and chlorine are made under the irradiation of 150 ℃ ~ 210 ℃ temperature and ultraviolet light The chlorination reaction is carried out continuously, and the chlorination reaction product and the solvent are cooled to obtain a pyridine chloride solution. After the chlorination solution is roughly steamed, tar and high boilers are separated, and the distillate is pyridine chloride containing a solvent.

[0018] Preparation of 2,6-dichloropyridine by liquid-phase photochlorination of pyridine (coarsely steamed material) test data

[0019] Reaction temperature °C

Embodiment 3

[0020] Embodiment 3: On the basis of Examples 1 and 2, using pyridine and chlorine as starting raw materials, taking trifluoromethyl chlorobenzene as solvent, pyridine and chlorine are made under the irradiation of 150 ℃ ~ 210 ℃ temperature and ultraviolet light The chlorination reaction is carried out continuously, the pyridine chlorination liquid obtained by cooling the chlorination reaction product and the solvent, the chlorination liquid is subjected to rough steaming, and the tar and high boiling matter are separated, and the distillate obtained is the pyridine chloride containing the solvent. After deducting the solvent, the pyridine The 2,6-dichloropyridine content in the chloride is ≥65%, and the pyridine chloride containing the solvent is purified by rectification to obtain a 2,6-dichloropyridine product with a purity ≥99.0%.

[0021] Experimental test data of preparation of 2,6-dichloropyridine (distillation separation) by liquid-phase photochlorination of pyridine

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Abstract

The invention relates to a method for preparing 2,6-dichloropyridine with product purity greater than or equal to 99.0% by using chlorotrifluoromethylbenzene as a solvent for a reaction between pyridine and chlorine. The preparing process comprises the steps as follows: by using the pyridine and the chlorine as initial raw materials and using the chlorotrifluoromethylbenzene as the solvent, continuously performing a chlorination reaction on the pyridine and the chlorine under the irradiation of ultraviolet light; and cooling a chlorination reaction product and the solvent to obtain pyridine chloride solution. The method has the advantages that 1, a precedent of directly preparing the 2,6-dichloropyridine in a high selectivity mode by a liquid-phase photochlorination reaction is set, and not only is the 2,6-dichloropyridine product with purity greater than or equal to 99.0% obtained, but also the method is easy for industrial production; and 2, not only is recycling of the separation solvent in the preparing process of the 2,6-dichloropyridine product with purity greater than or equal to 99.0% implemented, but also the aims of low pollution, low energy consumption and low cost in the preparing process are fulfilled.

Description

technical field [0001] The invention relates to a method for preparing 2,6-dichloropyridine with a product purity ≥ 99.0% by using trifluoromethyl chlorobenzene as a solvent for the reaction between pyridine and chlorine gas. Background technique [0002] The existing main synthesis methods of 2,6-dichloropyridine are: vapor-phase photochlorination of pyridine aqueous solution, the main product obtained is a mixture of 2-chloropyridine and 2,6-dichloropyridine, and the ratio of 2,6-dichloropyridine Generally, it is 5% to 50%. The chlorinated materials need to be separated and purified through a series of steps such as alkali neutralization, rough steaming and rectification, which will generate a large amount of waste water and waste salt, and the disposal cost of the three wastes is high. [0003] In the direct heating chlorination method of pyridine without ultraviolet light, the yield of 2,6-dichloropyridine is less than 30%, the coking rate is about 45%, a large amount of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61B01D3/143B01J19/123B01J2219/00033B01J2219/00051B01J2219/0869B01J2219/0884C07B39/00
Inventor 李惠跃金克强朱加权
Owner ZHEJIANG AVILIVE CHEM CO LTD