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Method for purifying piperonyl butoxide synthesized from sassafras oil

A technology of piperonyl butoxide and a purification method, applied in directions such as organic chemistry, can solve the problems of long operation period, difficult to control polymerization conversion, low yield and the like, and achieve the effects of short operation time, easy operation and high yield

Inactive Publication Date: 2005-02-16
TIANJIN UNIV
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

The separation and purification methods reported in the two patents of GB857541 and GB1344850 all use high vacuum rectification separation method. Due to the pressure drop of the rectification tower body and the inherent certain liquid holding capacity of the tower kettle, the whole system must reach a high degree of vacuum. It is difficult to ensure that the temperature of the tower kettle is lower than 230°C in actual production
The application of the above separation method has the disadvantages of long operation period, low yield and difficulty in controlling the polymerization conversion.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0007] Add 100g piperonyl butoxide liquid mixture into the feeder of the molecular distillation device (feeder volume 250ml, evaporation area 0.048 square meters, film wiper speed 50~1000rpm), the active ingredient piperonyl butoxide content of the mixture is 46.37 %. Turn on the raw material preheating device, raise the temperature to 85°C, and maintain a constant temperature. Turn on the cooling device, keep the cooling temperature at 20°C, add liquid nitrogen into the cold trap, turn on the rotary vane vacuum pump and the oil diffusion pump, make the operating pressure of the system reach 0.1Pa, turn on the precision constant temperature tank for evaporating materials to conduct heat transfer oil Heating, so that the temperature is stable at the required evaporation temperature of 92 ° C, then start feeding, the feed rate is 100g / h, the rotating speed of the wiper is 140rpm, after the distillation process ends, distillate 41.2g, heavy fraction 58.8 g: Distill the heavy fra...

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Abstract

The invention discloses a purification method of piperonyl butoxide synthetized from the sassafras oil and belongs to deep-processing technology of the sassafras oil. The method adopts the molecular distillation equipment and controls the pressure between 0.01Pa and 100Pa, the evaporating temperature between 90deg.C and 200deg.C, coolant temperature between -15deg.C and 80deg.C, the difference in temperature of the evaporator and the condenser between 30deg.C and 120deg.C and the milling speed between 10rpm and 1000rpm. The operational condition has two class separations. The purity of the piperonyl butoxide synthetized can reach above 98%. The invention is featured by the simple technique, short operation time, high yield, no other material with high boiling point during the reaction, no polymerization and no environmental pollution.

Description

technical field [0001] The invention relates to a method for purifying piperonyl butoxide synthesized from sassafras oil, which belongs to the deep processing and utilization technology of sassafras oil. Background technique [0002] Piperonyl butoxide is a very effective synergist for pyrethrin insecticides. It prevents insects from developing resistance by inhibiting the multifunctional oxidase of insects, thereby increasing the insecticidal effect. Patents such as WO02087337, CN1381181, GB2388778, RU2146090, GB829556, US3920440 (A1), US5883112, GB1415515 and US2904464 report the main application fields of piperonyl butoxide: piperonyl butoxide is added to pyrethrins and is mainly used in food in agriculture Prevention and control of crop pests such as cotton, fruits and vegetables; killing mosquitoes, flies and moths in clothing at home; protecting construction and textile materials by inhibiting moths; widely used in the food industry to kill and prevent production work...

Claims

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Application Information

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IPC IPC(8): C07D317/54
Inventor 许松林应安国王淑华向爱双徐世民
Owner TIANJIN UNIV
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