SU60206A1 - Method for the release of menthol - Google Patents
Method for the release of mentholInfo
- Publication number
- SU60206A1 SU60206A1 SU3278A SU3278A SU60206A1 SU 60206 A1 SU60206 A1 SU 60206A1 SU 3278 A SU3278 A SU 3278A SU 3278 A SU3278 A SU 3278A SU 60206 A1 SU60206 A1 SU 60206A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- menthol
- water
- oil
- distilled
- release
- Prior art date
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Одним из способов выделени ментола из м тного масла вл етс получение его высококип щих эфиров , отгонки низкокип щих примесей и омылени остатка.One way to isolate menthol from crud oil is to obtain its high boiling point ethers, distill off low boiling point impurities, and saponify the residue.
Автор насто щего изобретени : предлагает освобождать м тное масло от политерпенов, затем, в присутствии или отсутствии растворител , оксалировать под уменьшенным давлением, с целью образовани щавелевокислых эфиров 1ментола1 . При проведении процесса отгон ютс вода и примеси, в остатке остаетс эфир. Его омыл ют и ментол отгон ют с вод йнм паром. Применение растворител не Я1вл етс об зательным условием, проведени процесса, поскольку 1НИ5кокип щие фракции ментолового масла могут заменить их.The author of the present invention: proposes to free the cumin oil from polyterpenes, then, in the presence or absence of a solvent, to oxalate under reduced pressure in order to form 1 menthol ethers 1. During the process, water and impurities are distilled off, and ether remains in the residue. It is washed and menthol is distilled from the water with steam. The use of a solvent is not a necessary condition for carrying out the process, since 1N55 boiling fractions of menthol oil can replace them.
Пример. В колбу, снабженную водоуловителем, загружают м тное масло и щавелевую кислоту. М тное масло предвариггельно освобож )даетс от политерпенов, а щавелевой кислоты беретс 1-2%-й избыток против теоретически необходимого ДЛЯ получени диментилоксалата . Далее колбу соедин ют с вакуум-насосом , довод т разрежениеExample. Mint oil and oxalic acid are loaded into a flask equipped with a water trap. Mint oil is preliminarily freed from polyterpenes, and oxalic acid is taken up by a 1-2% excess against the theoretically necessary for the preparation of dimethyl oxalate. Next, the flask is connected to a vacuum pump, the vacuum is adjusted
до 60 мм и нагревают при 60° медленно повыща температуру. При нагревании происходит отгонка воды и низкокип щей фракции м тного масла, которые и собираютс в водоотделителе. Как только закончитс отгонка воды, разрежение в колбе довод т до 10 мм и нагревают реакционную массу до 130-140°. Образовавщийс щавелевокислый эфир ментола кипит, при указанном разрежении , при 225° и- отгонки его не приходитс опасатьс .to 60 mm and heated at 60 ° slowly raising the temperature. When heated, distillation of water and low boiling fraction of ground oil occurs, which are collected in a water separator. As soon as the distillation of water is finished, the vacuum in the flask is adjusted to 10 mm and the reaction mass is heated to 130-140 °. The resulting menthol ether menthol boils, at the indicated vacuum, at 225 ° and its distillation is not to be feared.
В результате процесса Б колбе остаетс диментилоксалат, который омыл ют 10%-м pacTiBopoM щелоч-и и ментол отгон ют с парами воды. Из отгона продукт экстрагируют дихлорэтаном, а экстракт разгон ют. Щелочные растворы, после омылеии эфира,содержат щавелевую кислоту; ее можно регенерировать одним из общеприн тых способов.As a result of process B, a flask of dimethyl oxalate remains, which is washed with 10% pacTiBopoM alkali and menthol is distilled off with water vapor. From the distillate, the product is extracted with dichloroethane, and the extract is distilled. Alkaline solutions, after the hydrolysis of ether, contain oxalic acid; it can be regenerated by one of the conventional methods.
Предмет изобретени .The subject matter of the invention.
Способ выделени ментола: из м тного масла путем получени его эфира, отгонки примесей и омылени- эфира, отличающийс тем, что м тное масло, освобожденное от политерпенов, в присутствии или отСутствии углеводородов, как растворителей , нагревают под уменьшенным да1влением со щавелевой кислотой до прекращени отго«ки води и примесей, после чего эфир омыл ют и ментол отгон ют с вод ным паром.Method of separating menthol: from mint oil by obtaining its ester, distilling off impurities and omylenyether, characterized in that ground oil, freed from polyterpenes, in the presence or absence of hydrocarbons, as solvents, is heated under reduced pressure with oxalic acid until its termination Stripping off water and impurities, after which the ether is saponified and menthol is distilled off with steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU3278A SU60206A1 (en) | 1940-06-03 | 1940-06-03 | Method for the release of menthol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU3278A SU60206A1 (en) | 1940-06-03 | 1940-06-03 | Method for the release of menthol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU60206A1 true SU60206A1 (en) | 1940-11-30 |
Family
ID=48242135
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU3278A SU60206A1 (en) | 1940-06-03 | 1940-06-03 | Method for the release of menthol |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU60206A1 (en) |
-
1940
- 1940-06-03 SU SU3278A patent/SU60206A1/en active
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