Preparation method of efficient chlorenthrin

A high-efficiency technology of permethrin, which is applied in the field of preparation of high-efficiency permethrin, can solve the problems of increasing the difficulty of wastewater treatment, wasting energy, and high ammonia nitrogen

Pending Publication Date: 2022-03-15
JIANGSU YOUJIA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since epimerization is usually carried out at a lower temperature and requires a long time of heat preservation, a large amount of energy is wasted, and epimerization usually uses organic amines as catalysts, resulting in high ammonia nitrogen in the wastewater produced by the treatment, increasing the The difficulty of wastewater treatment

Method used

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  • Preparation method of efficient chlorenthrin
  • Preparation method of efficient chlorenthrin
  • Preparation method of efficient chlorenthrin

Examples

Experimental program
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Effect test

Embodiment 1

[0043]A preparation method for beta-permethrin, comprising the following steps:

[0044] (1) Add 50 g of pentynyl alcohol, 100 g of toluene, 25 g of glacial acetic acid and 0.1 g of pig liver esterase into a four-neck flask, stir in a water bath and raise the temperature to 40° C., and keep the temperature for 24 hours to complete the reaction. Add 100g of water to wash the synthetic solution, separate the organic phase, dry it with sodium sulfate, remove the toluene at normal pressure to 130°C, then reduce the pressure to 100pa, and rectify to obtain 33g of S-pentynyl alcohol acetate with a content of 98%, R / S=5 / 95, yield 48.3%, remaining material R-pentynyl alcohol 21.8g, content 98%, R / S=95 / 5, yield 53.1%.

[0045] (2) Dissolve 30.9 g of the above-mentioned S-pentynyl acetate in 80 g of toluene, add 80 g of water and 25 g of liquid caustic soda, stir and heat up to 50° C., and keep the temperature for 2 hours to complete the reaction. Separate the organic phase, wash the ...

Embodiment 2

[0050] A preparation method for beta-permethrin, comprising the following steps:

[0051] (1) Add 500kg pentynyl alcohol, 1000kg toluene, 250g glacial acetic acid and 1kg pig liver esterase in the reactor, stir the water bath and heat up to 45 ° C, after 20 hours of insulation, the reaction is complete. Add 1000kg of water to wash the synthetic solution, separate the organic phase, remove the toluene from the organic phase at normal pressure to 125°C, then reduce the pressure to 100pa, and rectify to obtain 330kg of S-pentynyl alcohol acetate, with a content of 98%, R / S=5 / 95, the yield is 48.3%, the remaining material R-pentynyl alcohol is 218kg, the content is 98%, R / S=95 / 5, the yield is 53.1%.

[0052] (2) Dissolve the above-mentioned 309kg of S-pentynyl alcohol acetate in 1000kg of toluene, add 1000kg of water and 500kg of liquid caustic soda, stir and heat up to 52°C, and after 1 hour of insulation, the reaction is complete. Separate the organic phase, wash the organic p...

Embodiment 3

[0057] A preparation method for beta-permethrin, comprising the following steps:

[0058] (1) Add 125 g of pentynyl alcohol, 200 g of toluene, 50 g of glacial acetic acid and 0.5 g of pig liver esterase into a four-neck flask, stir in a water bath and raise the temperature to 35° C. After 26 hours of incubation, the reaction is complete. Add 500g of water to wash the synthetic solution, separate the organic phase, dry it with sodium sulfate, remove the toluene at normal pressure to 120°C, then reduce the pressure to 200pa, and rectify to obtain 82.5g of S-pentynyl alcohol acetate with a content of 98%, R / S=5 / 95, yield 48.3%, remaining material R-pentynol 54.5g, content 98%, R / S=95 / 5, yield 53.1%.

[0059] (2) Dissolve 82.5 g of the above-mentioned S-pentynyl acetate in 80 g of toluene, add 100 g of water and 80 g of liquid caustic soda, stir and heat up to 50° C., and keep the temperature for 2.5 hours to complete the reaction. Separate the organic phase, wash the organic ph...

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Abstract

The invention discloses a preparation method of beta-chlorenthrin, which comprises the following steps: by taking alkynyl pentanol as a raw material, selectively synthesizing acetate, hydrolyzing acetate, separating R-alkynyl pentanol and S-alkynyl pentanol, respectively synthesizing chlorenthrin with trans-S-DV-chrysanthemoyl chloride and trans-R-DV-chrysanthemoyl chloride, and curing and crushing to obtain beta-chlorenthrin raw powder. The method changes the situation that traditional chlorenthrin needs to be subjected to crystallization epimerization to improve effective bodies, and the method is mild and feasible in process condition, low in production cost, high in purity and wide in industrial production prospect.

Description

technical field [0001] The invention relates to a preparation method of beta-methrinthrin, which belongs to the technical field of chemical synthesis. Background technique [0002] Beta-permethrin is an important pyrethroid widely used in end products containing pyrethrins such as mosquito coils, and its molecular formula is C 16 h 20 Cl 2 o 2 , chemical name chemical name 1-ethynyl-2-methylpent-2-enyl-trans-2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropanesulfate, Its structural formula is as follows: [0003] [0004] For a long time, the production of permethrin raw powder is to first synthesize trans-permethrin and trans-pentyl alcohol, then synthesize permethrin, and then obtain high-efficiency through epimerization or crystallization. Permethrin. Since epimerization is usually carried out at a lower temperature and requires a long time of heat preservation, a large amount of energy is wasted, and epimerization usually uses organic amines as catalysts, resulting i...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C67/00C07C69/747C12P7/62C12P41/00
CPCC07C67/14C07C67/00C07C29/095C12P41/001C12P41/004C12P7/62C07C2601/02C07B2200/07C07C69/747C07C33/048
Inventor吴孝举孔勇谢邦伟陈鼎斌冯素流李志峰葛桂冬孙浩
OwnerJIANGSU YOUJIA CHEM