CN1580053A - Method for purifying piperonyl butoxide synthesized from sassafras oil - Google Patents
Method for purifying piperonyl butoxide synthesized from sassafras oil Download PDFInfo
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- CN1580053A CN1580053A CN 200410019314 CN200410019314A CN1580053A CN 1580053 A CN1580053 A CN 1580053A CN 200410019314 CN200410019314 CN 200410019314 CN 200410019314 A CN200410019314 A CN 200410019314A CN 1580053 A CN1580053 A CN 1580053A
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- piperonyl butoxide
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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
The present invention relates to a kind of method of purification, belong to the deep processing and utilization technology of sassafras wood oil by sassafras wood oil synthetic piperonyl butoxide.
Background technology
Piperonyl butoxide is the synergistic agent of the extraordinary pyrethrins insecticide of a kind of effect.It prevents that by suppressing the mixed-functional oxidase of insect insect from developing immunity to drugs, thereby increases insecticidal effect.WO02087337, CN1381181, GB2388778, RU2146090, GB829556, US3920440 (A1), US5883112, patent report such as GB1415515 and US2904464 the piperonyl butoxide main application fields: piperonyl butoxide is added in the cinerins, is mainly used in the control of crop pests such as grain, cotton, fruits and vegetables in agricultural; Kill the moth in mosquito, fly and the clothing in the household; By suppressing moth protection building and textile materials; In foodstuffs industry, be widely used for killing and prevent the insect in production plant, warehouse and the packaging vessel.
The synthetic of piperonyl butoxide is starting raw material with natural sassafras wood oil generally, through catalytic hydrogenation, Blanc chloromethylation and three steps of Willamson etherificate.US2878266, HU22948, HU34452, CA946850, AU9116082, GB1344850, patent reports such as US3767806 (A1) and GB839494 the synthetic technology of piperonyl butoxide.The synthetic piperonyl butoxide mixture that obtains had both comprised light constituent impurity such as diethylene glycol monobutyl ether, chloromethyl dihydrosafrole and toluene solvant, also comprised two piperonyl methane and two contour material that boils of piperonyl ether.GB857541, the GB1344850 patent report method of purification of piperonyl butoxide: remove some light constituent impurity such as solvent with simple distillation, then the mixture that takes off after light excised components such as diethylene glycol monobutyl ether, two piperonyl methane and two piperonyl ethers with rectification under vacuum (absolute pressure is lower than 0.15mmHg).Piperonyl butoxide has thermo-sensitivity, and when temperature is higher than 230 ℃, piperonyl butoxide can be transformed into other higher-boiling compound.The separating and purifying method that two patents of GB857541 and GB1344850 are reported all adopts the high vacuum rectification partition method, because the pressure drop and the certain liquid holdup of tower still inherent of rectifying tower body, make total system reach very high vacuum tightness, assurance makes tower still temperature be lower than 230 ℃, is difficult to accomplish in actual production.Using above-mentioned separation method, to exist the operational cycle long, and yield is lower and be difficult to shortcomings such as controlled polymerization conversion.
Summary of the invention
The object of the present invention is to provide a kind of method of purification by sassafras wood oil synthetic piperonyl butoxide.This method technology is simple, and product produce purity and yield height, and process is pollution-free.
The present invention is realized by following technical proposals: spacing is the molecular distillation apparatus of the short-path evaporator of 2～15cm between employing generating surface and the condensing surface, purification is by the method for sassafras wood oil synthetic piperonyl butoxide, it is characterized in that operating with following processing condition: pressure is 0.01～100Pa, vaporization temperature is 90～200 ℃, cooling temperature is-15～80 ℃, the vaporizer and the condenser temperature difference are 30～120 ℃, and stir speed (S.S.) is 10～1000rpm.And carry out two-stage and separate, flash trapping stage removal normal pressure boiling range is 150～210 ℃ a light constituent impurity, secondary separates the double distilled obtain with flash trapping stage and is divided into raw material, removes normal pressure boiling range wherein and be 220～320 ℃ heavy constituent, obtains purity and reaches piperonyl butoxide more than 98.0%.
Advantage of the present invention is: technology is simple, the operating time is short, yield is high, do not produce any other high boiling material matter, not polymerization, environmentally safe in the process.Compare with existing method, present method is separated the only process secondary distillation separation of process that the purification piperonyl butoxide reaches desired concn, and easy and simple to handle, distillation temperature is low, does not have easy conversion of traditional separation method or shortcomings such as polymerization and low yield.
Embodiment:
(feeder volume 250ml, 0.048 square metre of evaporation area add 100g piperonyl butoxide liquid mixture in the feeder of blade applicator rotating speed 50～1000rpm), this mixture effective constituent piperonyl butoxide content is 46.37% at molecular distillation apparatus.Open raw material preheating device, be warmed up to 85 ℃, and keep constant temperature.The open cold radiator cooler, keeping cooling temperature is 20 ℃, adds liquid nitrogen in cold-trap, open rotary-vane vaccum pump and oil diffusion pump, make the working pressure of system reach 0.1Pa, the exact constant temperature groove that unlatching evaporation material is used heats thermal oil, makes temperature-stable 92 ℃ of required vaporization temperatures, begin charging then, feeding rate is 100g/h, and the rotating speed of blade applicator is 140rpm, after still-process finishes, get overhead product 41.2g, last running 58.8g; To distill gained last running for the first time is to distill under 100 ℃ as raw material in vaporization temperature, and light constituent overhead product 34.4g is product, vinasse 6.8g.Product is colourless or the pale yellow oily liquid body, and piperonyl butoxide content is 98.36%, yield 73.0%.
The finished product of above embodiment are composed as follows:
Diethylene glycol monobutyl ether 0.09%
Chloromethyl dihydrosafrole 0.40%
Piperonyl butoxide 98.36%
Two piperonyl methane 0.35%
Two piperonyl ethers 0.80%
Claims (1)
1, a kind of method of purification by sassafras wood oil synthetic piperonyl butoxide, spacing is the molecular distillation apparatus of the short-path evaporator of 2～15cm between employing generating surface and the condensing surface, it is characterized in that operating with following processing condition: pressure is 0.01～100Pa, vaporization temperature is 90～200 ℃, cooling temperature is-15～80 ℃, the vaporizer and the condenser temperature difference are 30～120 ℃, and stir speed (S.S.) is 10～1000rpm; And carry out two-stage and separate, flash trapping stage removal normal pressure boiling range is 150～210 ℃ a light constituent impurity, secondary separates the double distilled obtain with flash trapping stage and is divided into raw material, removes normal pressure boiling range wherein and be 220～320 ℃ heavy constituent, obtains purity and reaches piperonyl butoxide more than 98.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019314 CN1255399C (en) | 2004-05-20 | 2004-05-20 | Method for purifying piperonyl butoxide synthesized from sassafras oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019314 CN1255399C (en) | 2004-05-20 | 2004-05-20 | Method for purifying piperonyl butoxide synthesized from sassafras oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1580053A true CN1580053A (en) | 2005-02-16 |
| CN1255399C CN1255399C (en) | 2006-05-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410019314 Expired - Fee Related CN1255399C (en) | 2004-05-20 | 2004-05-20 | Method for purifying piperonyl butoxide synthesized from sassafras oil |
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| CN (1) | CN1255399C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106422383A (en) * | 2016-10-10 | 2017-02-22 | 肇庆市和邦机械制造有限公司 | Short-range evaporator |
| WO2024121591A1 (en) * | 2022-12-05 | 2024-06-13 | Endura S.P.A. | Distillation of piperonyl butoxide |
-
2004
- 2004-05-20 CN CN 200410019314 patent/CN1255399C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106422383A (en) * | 2016-10-10 | 2017-02-22 | 肇庆市和邦机械制造有限公司 | Short-range evaporator |
| WO2024121591A1 (en) * | 2022-12-05 | 2024-06-13 | Endura S.P.A. | Distillation of piperonyl butoxide |
| WO2024120993A1 (en) * | 2022-12-05 | 2024-06-13 | Endura S.P.A. | Piperonyl butoxide distillation process with rectification for obtaining high purity pbo |
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| Publication number | Publication date |
|---|---|
| CN1255399C (en) | 2006-05-10 |
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