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Method for preparing coumaphos by aqueous phase method

A phosphatophos, water-phase technology, applied in chemical instruments and methods, chemicals for biological control, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of poor production safety, high reaction temperature, time It can reduce the production cost, reduce the reaction temperature and shorten the reaction time.

Active Publication Date: 2012-06-06
辽宁凤凰蚕药厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large amount of methyl ethyl ketone is used as a solvent, and methanol is used as a precipitation carrier. The reaction temperature is high and the time is long. After the reaction is completed, after multiple precipitation, recrystallization, solvent recovery and other post-processing steps, the production safety is poor, the pollution is high, and the cost is high.

Method used

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  • Method for preparing coumaphos by aqueous phase method
  • Method for preparing coumaphos by aqueous phase method

Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Feeding intake: 300 kilograms of water are dropped into 500 liters of reactors earlier, start agitator, then throw 36 kilograms of potassium carbonate, 45 kilograms of 3-chloro-4-methyl-7 hydroxycoumarin, phase transfer catalyst 1, 2 kg of 4-dimethylaminopyridine, add 40-45 kg of ethyl chloride.

[0023] (2) Temperature control: After feeding, time the reaction at room temperature for 1 hour. When the temperature was raised to 60° C., the reaction was carried out for 30 minutes, and the material was discharged.

[0024] (3) Discharging, washing and drying: put the material into the vacuum filter, filter out the waste water, wash the muscarinic acid with water until it is neutral, and then send it to the drying room to control the temperature at 75-80°C for drying.

Embodiment 2

[0026] (1) Feeding: Pour 300 kg of water into the reactor, start the agitator and add 36 kg of potassium carbonate, and then add 3-chloro-4-methyl-7 hydroxyarcohol after the potassium carbonate is dissolved (about 5 to 10 minutes). 45 kg of bean element, open the heating valve of the reaction kettle, add 3 kg of triethylamine when the temperature of the liquid in the kettle rises to 40~45°C, and then put 40~45 kg of ethyl chloride that has been weighed in advance and put into the metering tank. into the reactor.

[0027] (2) Temperature control: After the addition of chloride, when the temperature of the liquid in the tank rises to 70°C, start timing and control the temperature at 70-73°C for 2 hours, then open the cooling water valve to cool down, and wait for the liquid temperature in the tank to drop When the temperature reaches about 55°C, the reaction ends and the material is discharged.

[0028] (3) Discharging, washing and drying: put the material into the vacuum filte...

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Abstract

The invention relates to a method for preparing coumaphos by an aqueous phase method, belonging to the field of chemical vermifuge synthesis technologies. The method comprises the following steps: (A) feeding materials: feeding water into a reaction kettle, starting a stirrer, then feeding an acid-binding agent, 3-chlorin-4-methyl-7 hydroxy coumarin and a phase transfer catalyst, and adding ethylchloride; (B) controlling temperature: reacting at room temperature after feeding the materials, increasing the temperature to 50-80 DEG C and then reacting for 20-150 minutes, and discharging the materials; (C) discharging, washing and drying the materials: placing the materials into a vacuum filter to filter out waste water, then washing the coumaphos as a target product to be neutral by clear water, and then delivering the coumaphos as the target product into a drying chamber for controlling the temperature and drying. The invention has low reaction temperature, short reaction time and high yield, prevents a large quantity of organic solvents from being used, eliminates flammable and explosive hidden troubles and is outstanding in environmental protection effect.

Description

technical field [0001] The invention belongs to the field of synthetic technology of chemical insecticides, and in particular relates to a method for preparing muscarinum by an aqueous phase method. Background technique [0002] Mysphos is O, O-diethyl-O-(3-chloro-4-methylcoumarin-7) phosphorothioate, which is mainly used for the prevention and treatment of tussah parasitoid flies, bee mites, and livestock in vitro Parasitic diseases and pet medicine, etc. Due to its unique chemical structure, pharmacology and toxicity characteristics, compared with other chemical insecticides and miticides, the drug has high efficiency, low residue and no pollution, and is relatively safe to be used in animal products and bee products. [0003] 3-Chloro-4-methyl-7-hydroxycoumarin and ethyl chloride are subjected to condensation reaction to obtain muscarinum. As far as the search information about its synthesis is concerned, the synthesis of its condensation process still stays at the level...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/655A01P7/00A61P33/14
Inventor 张惠淳王立石牛雄雷杨金琛
Owner 辽宁凤凰蚕药厂
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