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Method for treating 4 chloro pyridine in solvent

A treatment method, the technology of tetrachloropyridine, applied in the direction of organic chemistry, etc., can solve the problems of high cost, long time, and time-consuming alkali hydrolysis in the separation and purification process, and achieve the effect of simple and reliable process

Active Publication Date: 2007-06-13
SHANDONG TIANCHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation and purification process is costly and takes a long time
The alkali hydrolysis of solid tetrachloropyridine with potassium hydroxide is also time-consuming, the yield is not ideal, and potassium hydroxide is relatively expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Containing 2% (accounting for the percentage of the total mass of the oil phase, the same below) o-dichlorobenzene of tetrachloropyridine and 40% sodium hydroxide solution and polyethylene glycol with a molecular weight of 600 are added in the same reaction kettle, and the oil phase and The volume ratio of the water phase is controlled at 1:1, the catalyst consumption is 1% of the total weight of the oil phase and the water phase, react at 80°C, and stir with 100 rev / min, follow the reaction process with gas chromatography to determine the end point.

Embodiment 2

[0019] O-dichlorobenzene containing 5% tetrachloropyridine, 20% sodium hydroxide solution and polyethylene glycol with a molecular weight of 200 are added to the same reaction kettle, the volume ratio of the oil phase and the water phase is controlled at 1:5, and the amount of catalyst 2% of the total weight of the oil phase and the water phase, reacted at 120° C., and stirred at 200 rpm, followed the reaction process with gas chromatography to determine the end point.

Embodiment 3

[0021] Containing nitrobenzene of 1% tetrachloropyridine and 10% sodium hydroxide solution and polyethylene glycol with a molecular weight of 800 are added in the same reaction kettle, the oil phase and water phase volume ratio are controlled at 1: 0.5, and the catalyst consumption is 0.3% of the total weight of the oil phase and the water phase were reacted at 40° C. and stirred at 40 rpm, and the reaction process was followed by gas chromatography to determine the end point.

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Abstract

This invention relates to a treatment method of tetrachloro pyridine in solvent. The stated solvent is chlorpyrifos intermediate for producing trichloro pyridine sodium alcoholate salt or kalium salt. Its characteristic is including that under effect of the phase-transfer catalyst, solvent containing by-product tetrachloro pyridine is transformed into trichloro pyridine sodium alcoholate salt or kalium salt by using water solution of natrium hydroxydatum or caustic potash. The mentioned phase-transfer catalyst utilizes carbowax of low molecular. In this invention, there is no need to separate and purify the by-product tetrachloro pyridine existing in solvent in the technology of using trichloroacetyl chloride route to synthesize trichloro pyridine sodium alcoholate salt or kalium salt as intermediate, but directly using lye to process to transform it into trichloro pyridine sodium alcoholate salt or kalium salt. The method reduces the procedure of separation and purification in present technique. Technology is simple and reliable, yield is near theoretical value.

Description

technical field [0001] The invention relates to a treatment method for by-products contained in solvents in the production of pesticide chlorpyrifos intermediates. Background technique [0002] Chlorpyrifos (chlorpyrifos), the chemical name is O, O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate is a highly efficient, broad-spectrum, medium and low toxicity organic Phosphorus pesticides are the replacement products of my country's current pesticide structure adjustment. Due to the limitations of raw materials, technology and equipment, my country mostly adopts the route of trichloroacetyl chloride to synthesize the intermediate triclopyridin sodium salt or potassium salt, and then condenses the triclopyridinol sodium salt or potassium salt with ethyl chloride to obtain chlorpyrifos . The synthetic method of triclopyridinol sodium salt or potassium salt is, using cuprous chloride as a catalyst, adding trichloroacetyl chloride and acrylonitrile in a solvent (o-dichlorob...

Claims

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Application Information

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IPC IPC(8): C07D213/63C07D213/61
Inventor 徐国庆
Owner SHANDONG TIANCHENG BIOTECH
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