Chlorpyrifos aqueous-phase synthesizing method with trichloro-acetic chloride as primary raw 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

Pending Publication Date: 2016-02-24
山东谦诚工贸科技有限公司
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Problems solved by technology

The method is complex in operation, high in cont...

Method used

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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 for 9-10 hours, heat up to 130-140°C, then feed dry Hcl gas, and 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 to 15°C and filter to obtain sodium triclopyridinate Crude.

[0019] Put the crude product of triclopyridinate sodium into a reaction kettle equipped with 100kg of water, 0.05N.N-lutidine, and 10kg32%NaOH, heat up to 105-108°C, reflux for 3 h...

Embodiment 2

[0022] Step (3) Add 2200kg of water to a 3000L glass-lined reactor, add 15.5kg of Tween-80, 3.5kg of sodium lauryl sulfate, 218kg of finished product sodium clopyridinate, 205kg of ethyl chloride, 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. Yield 98.4%, content 98.2% (gas chromatography); The Cu-cucl composite catalyst that adopts in the step (1) is copper and cuprous chloride mixture, and weight ratio is: copper: cuprous chloride=1: 2.

[0023] All the other are with embodiment 1.

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Abstract

The invention discloses a chlorpyrifos aqueous-phase synthesizing method with trichloro-acetic chloride as a primary raw material. The chlorpyrifos aqueous-phase synthesizing method includes the steps that the trichloro-acetic chloride, acrylonitrile, ortho-dichlorobenzene and a composite catalyst are reacted to obtain crude sodium trichloro pyridinol; the crude sodium trichloro pyridinol is put into a reaction still filled with water, a catalyst and alkali, heating and refluxing are carried out for 3 hours, a solvent is separated through standing, and sodium trichloro pyridinol is obtained in an aqueous-phase mode through cooling crystallizing and filtering; water is put into the reaction still, a dispersing agent, the sodium trichloro pyridinol, ethyl chloride and a catalyst are added while stirring and reacted, cooling crystallizing is carried out, and a chlorpyrifos raw-medicine finished product is obtained in a washing and suction-filtration mode. According to the chlorpyrifos aqueous-phase synthesizing method, the high-purity sodium trichloro pyridinol is prepared with the trichloro-acetic chloride as the primary raw material, and directly used as a raw material for synthesizing chlorpyrifos, and the sodium trichloro pyridinol produced with the method does not need to be refined, purified and dried. The water serves as a medium, the reaction materials are once added to synthesize the chlorpyrifos, the method is simple, operation is easy, environmental protection and energy saving are achieved, the product yield is increased, and product purity is improved.

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 fumigation 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 be used as ...

Claims

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Application Information

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IPC IPC(8): C07F9/58
CPCC07F9/58
Inventor 陈友来郝磊王兴栋
Owner 山东谦诚工贸科技有限公司
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