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Preparation method of trichloropyridine

A technology for trichloropyridine and chloropyridine, which is applied in the field of preparation of 2,3,6-trichloropyridine, can solve the problems of many wastes, complicated product separation process, residual residues and the like

Active Publication Date: 2014-04-23
盐城恒盛化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to overcome the product separation process complexity existing in the existing triclopyridine preparation method, waste material is many, residual catalyst such as ferric chloride etc. defect in the product, provide a kind of easy to operate industrialized production, less waste material, And the preparation method of the new trichloropyridine that catalyst can be reused

Method used

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Examples

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preparation example Construction

[0016] The invention provides a preparation method of triclopyridine, the method comprising: in the presence of a catalyst, contacting a low-chlorinated pyridine compound with chlorine gas to obtain a product after the contact reaction, wherein the catalyst is ferric chloride, One or more of zinc chloride, magnesium chloride and aluminum chloride, the inert gas is passed through the product after the contact reaction and then distilled.

[0017] According to the present invention, the catalyst is a catalyst commonly used in the art to synthesize triclopyridine through the contact reaction of low-chlorinated pyridine compounds and chlorine gas. Such a catalyst is one or more of the above-mentioned ferric chloride, zinc chloride, magnesium chloride and aluminum chloride; from the aspect of cost performance, it is preferred that the catalyst is ferric chloride. The catalysts described in the present invention are all Lewis acids of metal chlorides, which can form complexes with c...

Embodiment 1

[0035] This example is used to illustrate the preparation method of 2,3,6-trichloropyridine of the present invention.

[0036] Mix 15g of ferric chloride and 350g of 2,6-dichloropyridine, heat to 200°C under a nitrogen atmosphere, and then pass through chlorine gas for 8 hours to obtain a product after the contact reaction, which contains 389g 2,3,6-trichloropyridine, 17.3g of 2,6-dichloropyridine and 15.5g of 2,3,5,6-tetrachloropyridine.

[0037] The product was bubbled with nitrogen at 200°C for 2h, then cooled to 140°C, and distilled under a vacuum of 0.095MPa to collect fractions at a temperature of 132-138°C to obtain 412g of fractions. The content of 2,3,6-trichloropyridine, 2,6-dichloropyridine and 2,3,5,6-tetrachloropyridine contained in is 92.7% by weight, 4.04% by weight and 3.26% by weight, respectively, 2, The distillation yield of 3,6-trichloropyridine is 97.8%.

[0038] Take 0.11g of the above fraction for digestion, and make a 25ml solution of the digestion pr...

Embodiment 2

[0042] This example is used to illustrate the preparation method of 2,3,6-trichloropyridine of the present invention.

[0043] 100 g of 2,6-dichloropyridine prepared by the method of Example 1 and the product material after the contact reaction with chlorine gas were bubbled with nitrogen for 1 hour at 200°C, and then cooled to 140°C. Distilled under the condition of 0.085MPa, collected fractions with a temperature of 160-165°C, and obtained fractions of 90.1g, which contained 2,3,6-trichloropyridine, 2,6-dichloropyridine and 2,3, The contents of 5,6-tetrachloropyridine were 93.2% by weight, 3.75% by weight, and 2.96% by weight, respectively, and the distillation yield of 2,3,6-trichloropyridine was 94.3%.

[0044] Take 0.12g of the above fraction for digestion, and make a 25ml solution of the digestion product for ICP analysis. The measured iron ion concentration is 0.0210mg / L, which is close to the iron ion concentration of the blank sample (deionized water) 0.0182mg / L.

[...

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Abstract

The invention discloses a preparation method of trichloropyridine. The method comprises the following steps: enabling a low chlorinated pyridine compound to react with chlorine in a contact manner in the existence of a catalyst, so as to obtain a contact reaction product, wherein the catalyst is one or more of ferric chloride, zinc chloride, magnesium chloride and aluminum chloride; and leading in an inactive gas to the contact reaction product to distill. By adopting the method disclosed by the invention, the distillation yield of the trichloropyridine can be up to over 90%, and the obtained product trichloropyridine does not contain a catalyst ingredient. In addition, the distilled residue can be applied to catalyzed synthesis of the trichloropyridine.

Description

technical field [0001] The invention relates to a preparation method of trichloropyridine, in particular to a preparation method of 2,3,6-trichloropyridine. Background technique [0002] 2,3,6-Trichloropyridine (hereinafter referred to as three CP) is an important pharmaceutical and pesticide intermediate. For example, in pesticide chemistry, 2,3,6-trichloropyridine is mainly used to synthesize new insecticides chlorantraniliprole and cyantraniliprole. In the synthetic method of 2,3,6-trichloropyridine, it is currently widely used to use 2,6-dichloropyridine as a raw material, and 2,6-dichloropyridine is chlorinated by chlorine gas through the catalysis of Lewis acid Three CPs are obtained, wherein, the commonly used Lewis acids of metal chlorides are used as catalysts, such as ferric chloride, zinc chloride, aluminum chloride, etc., and ferric chloride is preferably used. This method has the advantages of simple process, low cost and high yield. [0003] For example, in ...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 张小航李勇李季
Owner 盐城恒盛化工有限公司
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