Aqueous-phase synthesis method of chlorpyrifos by using trichloro-acetic chloride as initial material

A technology of trichloroacetyl chloride and chlorpyrifos, which is applied in the field of fine chemical synthesis, can solve the problems of complex operation, low yield, and high control requirements, and achieve the effects of simple method, improved purity, and easy operation

Inactive Publication Date: 2013-03-27
JIANGSU QIHENG AGRI & CHEM TECHCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complex in operation, high in control requirements, and low in yield, which is not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for synthesizing chlorpyrifos in water phase with trichloroacetyl chloride as an initial raw material, comprising the following steps:

[0018] 32kg trichloroacetyl chloride, 12kg acrylonitrile, 100kg o-dichlorobenzene and 0.4kgCu-cucl composite catalyst are dropped into the reactor, the Cu-cucl composite catalyst that adopts is copper and cuprous chloride mixture, weight ratio is : Copper: Cuprous Chloride = 1:1; heat up to 105-110°C, reflux reaction for 9-10 hours, heat up to 130-140°C, then feed dry Hcl gas, keep warm for 8 hours. Vacuum (vacuum degree -0.08Mpa~-0.09Mpa) to collect low boilers, add 55kg of NaOH solution with a concentration of 20% after cooling the feed liquid, keep warm at 50-60°C, react for 2 hours, cool down to 15°C and filter to obtain sodium clopyridinate Crude.

[0019] Put the crude product of triclopyridinate sodium into a reaction kettle equipped with 100kg of water, 0.05N.N-lutidine, 10kg of 32%NaOH, heat up to 105-108°C, reflux...

Embodiment 2

[0022] Step (3) Add 2200kg of water to a 3000L glass-lined reactor, and add 15.5kg of Tween-80, 3.5kg of sodium lauryl sulfate, 218kg of finished sodium clopyridinate, 205kg of ethyl chloride, and 5kg of 30% Trimethylamine solution 0.8kg 4-dimethylaminopyridine, 5kg polyethanol 400, adjust pH=9.7, heat up to 50°C, react for 2.5 hours, cool down to 20°C to crystallize, discharge, wash with water and suction filter, dry to obtain chlorpyrifos finished product. The yield is 98.4%, and the content is 98.2% (gas chromatography); the Cu-cucl composite catalyst used in step (1) is a mixture of copper and cuprous chloride, and the weight ratio is: copper: cuprous chloride = 1:2. All the other are with embodiment 1.

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Abstract

The invention discloses an aqueous-phase synthesis method of chlorpyrifos by using trichloro-acetic chloride as an initial material. The method comprises steps of: reacting trichloro-acetic chloride, acrylonitrile, orthodichlorobenzene and a compound catalyst to obtain a 3,5,6-Trichloropyridin-2-ol sodium crude product; adding the 3,5,6-Trichloropyridin-2-ol sodium crude product into a reaction kettle with water, a catalyst and alkali, heating for reflux for 3 h, standing to separate out a solvent, and cooling, crystallizing and filtering an aqueous-phase to obtain the 3,5,6-Trichloropyridin-2-ol sodium; and adding water into the reaction kettle, adding a dispersing agent, 3,5,6-Trichloropyridin-2-ol sodium, ethyl chloride and a catalyst with stirring, reacting, cooling, crystallizing, washing and conducting suction filtration to obtain a chlorpyrifos active compound product. The invention employs trichloro-acetic chloride as the initial material to produce high-purity 3,5,6-Trichloropyridin-2-ol sodium, which is used directly as a raw material for the synthesis of chlorpyrifos. The sodium alkoxide produced by the method does not require refining, purifying or drying; water is used as the medium; and reaction materials are added at once for synthesis of chlorpyrifos. The method has advantages of simpleness, easy operation, environmental protection, energy saving, increased product yield, and improved product purity.

Description

technical field [0001] The invention relates to the field of fine chemical synthesis, in particular to a method for synthesizing chlorpyrifos. Background technique [0002] Chlorpyrifos, chemical name 0,0-diethyl-0-(3,5,6-trichloro-2-pyridyl) phosphorothioate, is a broad-spectrum organophosphorus insecticide with contact, stomach toxicity and fumigating properties It is a substitute for highly toxic organophosphorus pesticides. At present, the intermediate sodium chlorpyrifos is mostly used in the synthesis of chlorpyrifos in China. The purity of sodium alkoxide determines the quality of chlorpyrifos. According to relevant domestic literature reports, most of the key addition and cyclization reactions when sodium clopyridinate manufacturers produce sodium alkoxide use a single cuprous chloride as catalyst, which makes the addition and cyclization time long, with many by-products and low yield , the sodium alkoxide produced must be refined, purified, and dried before it can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58
Inventor 王健
Owner JIANGSU QIHENG AGRI & CHEM TECHCO
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