CN106699721A - Production technology of piperonyl butoxide composited by sassafras oil - Google Patents
Production technology of piperonyl butoxide composited by sassafras oil Download PDFInfo
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- CN106699721A CN106699721A CN201510774069.4A CN201510774069A CN106699721A CN 106699721 A CN106699721 A CN 106699721A CN 201510774069 A CN201510774069 A CN 201510774069A CN 106699721 A CN106699721 A CN 106699721A
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- sassafras oil
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- piperonyl butoxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/44—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D317/46—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems condensed with one six-membered ring
- C07D317/48—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring
- C07D317/50—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to atoms of the carbocyclic ring
- C07D317/54—Radicals substituted by oxygen atoms
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Abstract
A production technology of piperonyl butoxide composited by sassafras oil comprises the following procedures of catalytic hydrogenation, chloromethylation and etherification. In the catalytic hydrogenation procedure, the sassafras oil and hydrogen are mixed and react to generate dihydro sassafras oil by the action of a catalyst, and the catalyst is lithium and nickel alloy powder. In the chloromethylation procedure, the dihydro sassafras oil, hydrochloric acid and paraformaldehyde are mixed and react in the presence of an assistant to generate chloromethyl material reaction liquid, and the assistant is tetraethyl ammonium bromide. In the etherification procedure, the chloromethyl material reaction liquid, sodium hydroxide, monobutyl ether and ethidene diamine are mixed and react, and a resultant contains piperonyl butoxide. Hydrochloric acid is employed as an additive; the reaction conversion rate is increased; piperonyl butoxide is light-colored or white liquid; the yield reaches 90% or higher; the content is 95-98%.
Description
Technical field
The present invention relates to a kind of production technology of the piperonyl butoxide synthesized by sassafras oil.
Background technology
In the prior art, Chinese patent application 200410019314.2 discloses the method for purification of the piperonyl butoxide synthesized by sassafras oil, and the production technology of the piperonyl butoxide synthesized by sassafras oil generally comprises following procedures catalytic hydrogenation, chloromethylation, etherificate.But without specifically, the production technology detailed process report of the piperonyl butoxide synthesized by sassafras oil in the synthetic method of prior art.
The content of the invention
It is an object of the present invention to provide a kind of production technology of the piperonyl butoxide synthesized by sassafras oil, the yield of its final piperonyl butoxide is higher.
The technical scheme is that：A kind of production technology of the piperonyl butoxide synthesized by sassafras oil, including following procedures：
(1) catalytic hydrogenation；
(2) chloromethylation；
(3) it is etherified；
In described catalytic hydrogenation operation, by sassafras oil and hydrogen, hybrid reaction generates dihydro sassafras oil in the presence of catalyst, and described catalyst is lithium nickel alloy powder；
In described chloromethylation operation, by dihydro sassafras oil and hydrochloric acid, the paraformaldehyde hybrid reaction under conditions of having auxiliary agent, described auxiliary agent is tetraethylammonium bromide, obtains chloromethane base-material reaction solution；
In described etherificate operation, by chloromethane base-material reaction solution and NaOH, monobutyl ether, ethylenediamine hybrid reaction, piperonyl butoxide is contained in product.
In described lithium nickel alloy powder, lithium ground weight ratio is 50~60%, and remaining is nickel.
In described catalytic hydrogenation operation, the weight ratio of the described sassafras oil for feeding intake is 700 parts, the weight ratio of described catalyst is 20~60 parts, the weight ratio of the hydrogen of described addition is 7.2~16.2 parts, the reaction temperature that reaction condition is is 30~100 DEG C, reaction pressure is 4~10 kg/cms, 180~300 minutes reaction time.
In described chloromethylation operation, the charged material weight ratio of dihydro sassafras oil is 700 parts, the weight that feeds intake of hydrochloric acid
Than being 2500~3500 parts, hydrochloric acid is concentrated hydrochloric acid of the concentration more than 31% to amount, and the charged material weight ratio of paraformaldehyde is 200~300 parts, and the charged material weight ratio of auxiliary agent is 2 parts, and reaction condition is that reaction temperature is 30~80 DEG C, 4~6 hours reaction time.
In described etherificate operation, the charged material weight ratio of chloromethane base-material reaction solution is 800~900 parts, NaOH is high alkali liquid of the concentration more than 48%, the charged material weight ratio of NaOH is 400~500 parts, the charged material weight ratio of monobutyl ether is 1500~2000 parts, the charged material weight ratio of ethylenediamine is 20 parts, and reaction temperature is 30~150 DEG C, more than 14 hours reaction time.
The present invention has following advantages compared with prior art：
Reaction conversion ratio is improve as additive using hydrochloric acid, the outward appearance of piperonyl butoxide is light color or white liquid, yield is up to more than 90%, content 95%-98%.
Specific embodiment
(1) in catalytic hydrogenation operation, from the reactor of 1000 liters, add 700 kilograms of sassafras oil, 20-60 kilograms of catalyst lithium nickel alloy powder is added, 80-180 cubes of hydrogen (volume at one atm) is added, reaction condition is pressure 4-10 kg/cms, 30-100 DEG C of temperature, speed of agitator is 30-85 revs/min, and the reaction time was controlled at 180-300 minutes, obtained dihydro sassafras oil content 90%-98%.
(2) in chloromethylation operation, from the reactor of 5000 liters, 25-90 revs/min of speed of agitator, add 700 kilograms of dihydro sassafras oil, 2500-3500 kilograms of the hydrochloric acid of concentration 33% is added, 200-300 kilograms of paraformaldehyde is added, 2 kilograms of auxiliary agent tetraethylammonium bromide is added, reaction temperature is 30-80 degree, and the reaction time is 4-6 hours.
(3) in etherificate operation, from the reactor of 3000 liters, speed of agitator is 40-80 revs/min, add liquid caustic soda (NaOH) 400-500 kilogram of the concentration more than 48%, 1500-2000 kilograms of monobutyl ether is added, 20 kilograms of ethylenediamine is added, 800-900 kilograms of the chloromethane base-material reaction solution obtained in chloromethylation operation is added, 30-150 DEG C of reaction temperature, the reaction time is 14 hours to reaction end.
Contain piperonyl butoxide in final reaction solution, can be extracted by the method distilled, the method is already described in Chinese patent application 200410019314.2.
Claims (5)
1. a kind of production technology of the piperonyl butoxide synthesized by sassafras oil, including following procedures：
(1), catalytic hydrogenation；
(2), chloromethylation；
(3), it is etherified；
It is characterized in that：In described catalytic hydrogenation operation, by sassafras oil and hydrogen, hybrid reaction generates dihydro sassafras oil in the presence of catalyst, and described catalyst is lithium nickel alloy powder；
In described chloromethylation operation, by dihydro sassafras oil and hydrochloric acid, the paraformaldehyde hybrid reaction under conditions of having auxiliary agent, described auxiliary agent is tetraethylammonium bromide, obtains chloromethane base-material reaction solution；
In described etherificate operation, by chloromethane base-material reaction solution and NaOH, monobutyl ether, ethylenediamine hybrid reaction, piperonyl butoxide is contained in product.
2. the production technology of the piperonyl butoxide synthesized by sassafras oil according to claim 1, it is characterised in that：In described lithium nickel alloy powder, the weight ratio of lithium is 50~60%, and remaining is nickel.
3. the production technology of the piperonyl butoxide synthesized by sassafras oil according to claim 1, it is characterised in that：In described catalytic hydrogenation operation, the weight ratio of the described sassafras oil for feeding intake is 700 parts, the weight ratio of described catalyst is 20~60 parts, the weight ratio of the hydrogen of described addition is 7.2~16.2 parts, the reaction temperature that reaction condition is is 30~100 DEG C, reaction pressure is 4~10 kg/cms, 180~300 minutes reaction time.
4. the production technology of the piperonyl butoxide synthesized by sassafras oil according to claim 1, it is characterised in that：In described chloromethylation operation, the charged material weight ratio of dihydro sassafras oil is 700 parts, the charged material weight ratio of hydrochloric acid is 2500~3500 parts, hydrochloric acid is concentrated hydrochloric acid of the concentration more than 31%, the charged material weight ratio of paraformaldehyde is 200~300 parts, the charged material weight ratio of auxiliary agent is 2 parts, and reaction condition is that reaction temperature is 30~80 DEG C, 4~6 hours reaction time.
5. the production technology of the piperonyl butoxide synthesized by sassafras oil according to claim 1, it is characterised in that：In described etherificate operation, the charged material weight ratio of chloromethane base-material reaction solution is 800~900 parts, NaOH is high alkali liquid of the concentration more than 48%, the charged material weight ratio of NaOH is 400~500 parts, the charged material weight ratio of monobutyl ether is 1500~2000 parts, the charged material weight ratio of ethylenediamine is 20 parts, and reaction temperature is 30~150 DEG C, more than 14 hours reaction time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510774069.4A CN106699721A (en) | 2015-11-13 | 2015-11-13 | Production technology of piperonyl butoxide composited by sassafras oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510774069.4A CN106699721A (en) | 2015-11-13 | 2015-11-13 | Production technology of piperonyl butoxide composited by sassafras oil |
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| CN106699721A true CN106699721A (en) | 2017-05-24 |
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| CN201510774069.4A Withdrawn CN106699721A (en) | 2015-11-13 | 2015-11-13 | Production technology of piperonyl butoxide composited by sassafras oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114586799A (en) * | 2022-03-25 | 2022-06-07 | 南京生兴有害生物防治技术股份有限公司 | Pine wood nematode disease treating agent and preparation method thereof |
-
2015
- 2015-11-13 CN CN201510774069.4A patent/CN106699721A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114586799A (en) * | 2022-03-25 | 2022-06-07 | 南京生兴有害生物防治技术股份有限公司 | Pine wood nematode disease treating agent and preparation method thereof |
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| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170524 |