Preparation of high efficiency cholrempenthrin raw powder
A technology of permethrin and raw powder, which is applied in the field of preparation of high-efficiency permethrin raw powder, can solve problems such as safety and environmental accidents, material rush, waste of raw materials, etc., and achieves mild and feasible process conditions and reasonable process route , the effect of high total product yield
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Embodiment 1
[0033] (1) Add 200g of dichloroethane and 200g of sodium acetylene to the reaction kettle with condenser reflux, stirring, dropping, heating and cooling, stir and cool down to -10°C, slowly add 30g of sodium hydroxide, about Add 1 hour, then raise the temperature to 50°C, add 100g of pentenal dropwise for 2 hours, keep warm for 10 hours after the dropwise addition, the reaction is complete, add 100g of water for hydrolysis, separate the organic phase, and wash the organic phase with acid and water , dried over sodium sulfate, and desolvated to obtain 120 g of pentynyl alcohol. Boiling point: 140-160°C, content 98%, yield 94.8%.
[0034] (2) Dissolve 62g of pentynyl alcohol in the previous step in 460g of toluene, add 0.1g of triethylamine as a catalyst, stir and cool down to 5°C, add 116g of all-trans DV-chrysanthemum acid chloride dropwise, dropwise for 2 hours, dropwise After the addition was complete, the reaction was completed at 20° C. for 6 hours. Washing twice with wa...
Embodiment 2
[0037] (1) In the reactor with condenser reflux, stirring and dropping, heating and cooling, add 200g of petroleum ether, feed acetylene until the reactor is emptied and a large amount of acetylene gas is released, after the acetylene gas of the reaction system is saturated Stop the ventilation, stir and cool down to -10°C, slowly add 30g of sodium hydroxide, and finish the addition in about 1 hour, then raise the temperature to 40°C, add 100g of pentenal dropwise, for 2 hours, keep the temperature for 20 hours after the dropwise addition, and the reaction is complete , add 100 g of water for hydrolysis, separate the organic phase, wash the organic phase with acid and water, dry over sodium sulfate, and remove the solvent to obtain 110 g of pentynyl alcohol. Boiling point: 140-160°C, content 95%, yield 85%.
[0038] (2) Dissolve 62g of pentynyl alcohol in the previous step in 530g of xylene, add 0.01g of pyridine as a catalyst, stir and cool down to 5°C, add 116g of all-trans ...
Embodiment 3
[0041](1) In the reaction kettle with condenser reflux, stirring and dropwise addition and heating, cooling, add 200g cyclohexane, feed acetylene gas to the reactor evacuation and a large amount of acetylene gas is released, the acetylene gas in the reaction system After saturation, stop the ventilation, stir and cool down to 0°C, slowly add 50g of potassium hydroxide, and finish the addition in about 1 hour, then raise the temperature to 20°C, add 100g of pentenal dropwise, for 2 hours, keep the temperature for 30 hours after the dropwise addition, and react Complete, add water for hydrolysis, separate the organic phase, wash the organic phase with acid and water, dry over sodium sulfate, and remove the solvent to obtain 121 g of pentynyl alcohol. Boiling point: 140-160°C, content 95%, yield 92.7%.
[0042] (2) Dissolve 62 g of pentynyl alcohol in the previous step in 420 g of cyclohexane, add 0.1 g of liquid caustic soda catalyst NaOH, stir and cool down to 5°C, add 116 g of...
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