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Method for preparing 2-chloro-6-trichloromethylpyridine

A technology of trichloromethylpyridine and picoline, which is applied in the field of industrial preparation of 2-chloro-6-trichloromethylpyridine, can solve problems such as low productivity, increased production cost, and expensive raw materials

Inactive Publication Date: 2012-03-28
LANGFANG BEIXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The disadvantage of the above method is that it can only be produced intermittently, the productivity is low, the price of raw materials is expensive, and the production cost increases.

Method used

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  • Method for preparing 2-chloro-6-trichloromethylpyridine
  • Method for preparing 2-chloro-6-trichloromethylpyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] When the temperature of the primary chlorination tank 1 reaches 190-200°C, dry chlorine gas B is introduced at 180kg / h, and 2-picoline A is continuously added at 30kg / h; the chlorinated semi-finished product continuously flows into the secondary chlorination tank 2 , where 108kg / h of chlorine gas is introduced separately, and the temperature is controlled at 190-200°C; the temperature of the three-stage chlorination kettle 3 is 190-200°C, and chlorine gas is separately passed at 90kg / h; the temperature of the fourth-stage chlorination kettle 4 is 190-200°C ℃, gas chromatographic tracking, chlorine gas is fed separately at 72kg / h. The crude product D of 2-chloro-6-trichloromethylpyridine flowing out continuously has a content of 94% and a yield of 88%. The 2-chloro-6-trichloromethylpyridine product with a content of 99% was obtained through vacuum distillation.

[0043] The HCl tail gas produced by the reaction also contains excess chlorine gas. First, absorb HCl gas wi...

Embodiment 2

[0046] When the temperature of the primary chlorination tank 1 reaches 80°C, chlorine gas B is introduced at 180 kg / h, and 2-picoline A is continuously added at 18 kg / h at the same time; the chlorinated semi-finished product continuously flows into the secondary chlorination tank 2, where Chlorine gas is fed separately at 180kg / h, and the temperature is controlled at 230°C; the temperature of the third-stage chlorination kettle 3 is 80°C, and chlorine gas is passed through separately at 18g / h; h Chlorine gas is introduced separately. The crude product D of 2-chloro-6-trichloromethylpyridine flowing out continuously has a content of 88% and a yield of 85%. The 2-chloro-6-trichloromethylpyridine product with a content of 99% was obtained through vacuum distillation.

[0047] The HCl tail gas produced by the reaction also contains excess chlorine gas. First, absorb HCl gas with water to produce hydrochloric acid E. After the remaining wet chlorine gas is dried in a concentrated ...

Embodiment 3

[0050] When the temperature of the primary chlorination kettle 1 reaches 210°C, feed dry chlorine gas B at 180kg / h, and simultaneously add 2-picoline A continuously at 45kg / h; the chlorination semi-finished product continuously flows into the secondary chlorination kettle 2, and Chlorine gas is fed separately at 18kg / h, and the temperature is controlled at 80°C; the temperature of the third-stage chlorination kettle 3 is 230°C, and chlorine gas is passed through separately at 180g / h; / h Chlorine gas is introduced separately. The crude product D of 2-chloro-6-trichloromethylpyridine flowing out continuously has a content of 90% and a yield of 86%. The 2-chloro-6-trichloromethylpyridine product with a content of 99% was obtained through vacuum distillation.

[0051] The HCl tail gas produced by the reaction also contains excess chlorine gas. First, absorb HCl gas with water to produce hydrochloric acid E. After the remaining wet chlorine gas is dried through the concentrated su...

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Abstract

The invention discloses a method for preparing 2-chloro-6-trichloromethylpyridine. In the method, 2-methyl pyridine is used as a raw material and a multi-stage liquid-phase continuous chlorination process is adopted; therefore, the method has the advantages of simplicity, high efficiency, environment friendliness and low cost.

Description

technical field [0001] The invention relates to a preparation method of 2-chloro-6-trichloromethylpyridine, in particular to an industrial preparation method of 2-chloro-6-trichloromethylpyridine by adopting liquid phase continuous chlorination. Background technique [0002] 2-Chloro-6-trichloromethylpyridine is an important pharmaceutical and pesticide intermediate, and a well-known nitrogen fertilizer synergist, and its application fields are constantly expanding. [0003] Previously reported preparation methods include: [0004] The patent number is US3424754, and the patent name is "Preparation of 2-Chloro-6-trichloromethylpyridine". The method first makes 2-methylpyridine into hydrochloride and then chlorates it; [0005] The patent number is US3420833, and the patent name is "production of polychlorinated pyridine compounds by gas phase method". The method is chlorination in gas phase at 400 °C; [0006] The patent number is US3418323, and the patent name is "2-chlor...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 肖才根
Owner LANGFANG BEIXIN CHEM
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