Method for continuous production of 2-chloro-5-methylpyridine

A picoline and production method technology, applied in the field of continuous production of 2-chloro-5-picoline, can solve the problems of small production capacity, high cost, low production efficiency, etc.

Active Publication Date: 2015-03-18
JIANGSU YANGNONG CHEM GROUP +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for continuous production of 2-chloro-5-picoline, and overcome the problems of low production efficiency, small production capacity, high cost and difficult continuous production of some technologies in the existing synthetic technology

Method used

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  • Method for continuous production of 2-chloro-5-methylpyridine

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Embodiment 1

[0011] Add toluene of 1 / 10 of the volume of the container into the first, second, and third-stage mixing reactors, raise the temperature in the first, second, and third-stage reactors to 30°C, and control the pressure in the first-stage reactors to -1000kPa; 2-Chloro-4-formyl valeronitrile, phosphorus trichloride, and toluene are transported to the first-stage tank-type mixed reactor for reaction through metering pumps 1, 2, and 3 at a volume ratio of 1:0.1:0.01, and then passed through the overflow In the form of flow, it goes to the two-stage tank reactor, the three-stage tank reactor, and the receiving tank for continuous reaction, and finally adds alkali to the neutralization tank to adjust the pH of the system to be greater than 7 to obtain crude 2-chloro-5-picoline , and its yield to 2-chloro-4-formylvaleronitrile was 75%.

Embodiment 2

[0013] Add 1 / 10 of the container volume of chlorinated benzene to the first, second, and third-stage mixing reactors, raise the temperature in the first, second, and third-stage reactors to 120°C, and control the pressure in the first-stage reactors to +1000kPa ; 2-chloro-4-formyl valeronitrile, phosphorus pentachloride, and chlorinated benzene are delivered to the first-stage tank-type mixed reactor by metering pumps 1, 2, and 3 in a volume ratio of 1:10:10 for reaction , and then proceed to the secondary tank reactor, the three-level tank reactor, and the receiving tank in the form of overflow for continuous reaction, and finally add alkali to the neutralization tank to adjust the pH of the system to be greater than 7 to obtain crude 2-chloro- 5-Methylpyridine with a yield of 79% to 2-chloro-4-formylvaleronitrile.

Embodiment 3

[0015] Add 1 / 10 of the volume of benzene in the first, second, and third-stage tank-type mixed reactors, raise the temperature in the first, second, and third-stage stills to 70°C, and control the pressure in the first-stage still to 0kPa; -Chloro-4-formylvaleronitrile, phosphorus oxychloride, and benzene are transported to the first-stage tank-type mixed reactor for reaction through metering pumps 1, 2, and 3 at a volume ratio of 1:0.3:1, and then through the overflow in the form of two-stage tank reactor, three-stage tank reactor, and receiving tank for continuous reaction, and finally add alkali to the neutralization tank to adjust the pH of the system to be greater than 7 to obtain crude 2-chloro-5-picoline , and its yield to 2-chloro-4-formylvaleronitrile was 90.2%.

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Abstract

The invention relates to a method for continuous production of an intermediate of a pyridine heterocycle insecticide, namely 2-chloro-5-methylpyridine. The method comprises the following steps: conveying 2-chloro-4-formylvaleronitrile, a chlorinating agent and an organic solvent into a kettle type mixing reactor through a metering pump for reaction, then putting into a three-stage kettle type reactor receiving kettle in an overflow form sequentially to perform continuous reaction, finally putting into a neutralizing kettle, and adding alkali to regulate the pH value of a system to be more than 7, thereby obtaining crude 2-chloro-5-methylpyridine. According to the method provided by the invention, the defects of high power consumption in intermittent reaction, non-uniform material mixing, difficulty in temperature control and effect of being prone to outshoot accidents are overcome, and the advantages of short reaction time, high selectivity in chemical synthesis reaction and high yield are realized. The method further has the advantages of mild conditions, stable quality, easiness in large-scale production, relatively low cost and relatively few three wastes, and is conductive to industrialized energy conservation, consumption reduction and production.

Description

technical field [0001] The invention relates to a production method of a pesticide intermediate, in particular to a continuous production method of an intermediate 2-chloro-5-picoline of a pyridine heterocyclic pesticide. Background technique [0002] At present, the overall direction of the development of the pesticide industry is high efficiency (low application per unit area), safety (safety for humans, animals, and the environment), economy (low application cost) and convenient use (high-efficiency dosage forms). However, new pesticides such as imidacloprid, acetamiprid, fluazifop-p-p, and valero-p-p-p-methylpyridine heterocyclic insecticides and herbicides have systemic, broad-spectrum, high-efficiency, and low-toxicity properties. , less dosage, long duration, good safety, strong drug resistance and other advantages, has been widely used in large areas abroad, and 2-chloro-5-methylpyridine is the synthesis of the above-mentioned high-efficiency new pesticides and futur...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 郑亚清丁克鸿周颖华张寅胡俊冀超孙伟
Owner JIANGSU YANGNONG CHEM GROUP
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