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Production method of 6-chloro-2-(trichloromethyl)pyridine

A technology of trichloromethylpyridine and dichloromethylpyridine is applied in the field of nitrogen fertilizer synergist 6-chloro-2-trichloromethylpyridine, which can solve the problems of low product yield, material blockage and the like, and reduce production Cost and production process control are simple and easy to implement

Active Publication Date: 2010-11-24
SHANDONG SHENGBANG LUNAN PESTICIDE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a new production method of 6-chloro-2-trichloromethylpyridine, to solve the problems of low product yield, easy generation of tar polymer, material blockage of pipelines and other problems in the existing production method , so as to achieve the purpose of improving reaction selectivity and product yield, reducing waste discharge, and making it easier for industrial production

Method used

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  • Production method of 6-chloro-2-(trichloromethyl)pyridine

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Embodiment 1

[0034] Add 96 kg of 4-chlorobenzotrifluoride into a 300L glass-lined reactor, add 160 kg of 2-methylpyridine and 20 kg of 4-chlorobenzotrifluoride into a high-level metering tank to form a 2-methylpyridine solution. Start stirring, after the reactor is heated to 165°C, feed chlorine at 9kg per hour, keep the reaction temperature at 165°C, add 2-picoline solution at 2.25kg per hour, and react for 8 hours; the reaction temperature is increased to 170°C, Keep warm, increase the amount of chlorine gas per hour to 12kg, increase the amount of 2-picoline solution to 3.375kg / h, and react for 8 hours; increase the reaction temperature to 180°C, keep warm, increase the amount of chlorine gas per hour to 15kg , the amount of 2-picoline solution added is increased to 4.5kg / h, and the reaction is carried out for 8 hours; the reaction temperature is increased to 190°C, kept warm, and the amount of chlorine gas per hour is increased to 27kg, and the amount of 2-picoline solution added is inc...

Embodiment 2

[0036] Add 1820kg of dichlorobenzene into the 3000L glass-lined reactor, add 260kg of 2-picoline and 780kg of dichlorobenzene into the high-level metering tank to make a 2-picoline solution. Start stirring, after the reactor is heated to 135°C, feed chlorine gas at a rate of 50-60 kg per hour, keep the reaction temperature at 135°C, add 2-methylpyridine solution at a rate of 35 kg per hour, and react for 10 hours; chlorine gas and 2-methylpyridine The adding speed of pyridine solution is constant, the reaction temperature is raised to 150°C, and the heat preservation is carried out. After 10 hours of reaction, the reaction temperature is raised to 160°C, heat preservation, and further reaction for 10 hours. When the cumulative addition of 2-picoline solution reaches 1040kg, stop adding For 2-picoline solution, feed chlorine gas at 10-12kg per hour, increase the temperature to 190°C, and react for another 3 hours, then take samples for GC analysis every 1 hour, the content of 6-...

Embodiment 3

[0038] Add 20kg of chlorobenzene into the 300L glass-lined reactor, add 240kg of 2-methylpyridine and 4kg of chlorobenzene into the high-level metering tank to make a 2-methylpyridine solution. Start stirring, after the reactor is heated to 160°C, feed chlorine at 15-20kg per hour and add 2-picoline solution at 2-3kg per hour, keep the reaction temperature at 160°C, react for 6 hours; increase the reaction temperature to 175°C, Keep warm, feed chlorine gas at a speed of 30~40kg / h and add 2-picoline solution at a speed of 4~6kg / h, and react for 12 hours; increase the reaction temperature to 190°C, keep warm, and feed chlorine gas at a speed of 30~50kg / h h and 2-picoline solution were added at a rate of 11-12kg / h and reacted for 15 hours; when the cumulative addition of 2-picoline solution reached 244kg, stop adding 2-picoline solution at a rate of 20-22kg per hour Feed chlorine gas at a temperature of 190°C. After another 2 hours of reaction, take samples for GC analysis ev...

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Abstract

The invention relates to a production method of a nitrogen fertilizer synergist-6-chloro-2-(trichloromethyl)pyridine, belonging to the crop production field. The production method comprises the following steps: taking 2-methylpyridine as a staring material; in the presence of solvents such as chlorobenzene, dichlorobenzene, chloro-trifluorotoluene, nitrobenzene and the like, introducing excessive chlorine at the temperature of 130-205 DEG C for chlorination to obtain a crude product of the 6-chloro-2-(trichloromethyl)pyridine; and purifying the crude product through rectification to obtain the high-purity product of the 6-chloro-2-(trichloromethyl)pyridine. The production method can overcome the defects of low yield, easy generation of a tar polymer, pipe blockage caused by materials and the like of the existing production method, thus achieving the purpose of improving reaction selectivity and product yield, reducing waste discharge and being easy to be industrialized.

Description

technical field [0001] The invention belongs to the field of crop production, and in particular relates to a large-scale production method of a nitrogen fertilizer synergist 6-chloro-2-trichloromethylpyridine. Background technique [0002] 6-Chloro-2-trichloromethylpyridine is a nitrogen fertilizer synergist that can selectively inhibit nitrification or denitrification in soil and improve nitrogen use efficiency. It is code-named CP, contains 6% nitrogen, and is white Crystalline solid, widely used in foreign countries now, with the best effect. my country has also done experiments on various crops, and it has been proved that it has a certain effect of increasing production. The application rate is about 1% of the amount of pure nitrogen applied. When its concentration in the soil is 1-10 mg / kg, it will affect the soil Nitrification has obvious inhibitory effect, and the validity period is about 30 days. For rice, corn, wheat, sorghum, cotton, rapeseed and other crops, it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 李惠跃金克强韦尉玉
Owner SHANDONG SHENGBANG LUNAN PESTICIDE
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