CN108795576A - A kind of peppermint oil dementholized method of purification - Google Patents
A kind of peppermint oil dementholized method of purification Download PDFInfo
- Publication number
- CN108795576A CN108795576A CN201810565473.4A CN201810565473A CN108795576A CN 108795576 A CN108795576 A CN 108795576A CN 201810565473 A CN201810565473 A CN 201810565473A CN 108795576 A CN108795576 A CN 108795576A
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- CN
- China
- Prior art keywords
- peppermint
- oil
- vapor
- peppermint oil
- amount
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Abstract
The invention discloses a kind of peppermint oil dementholized methods of purification, include the following steps：Prepare peppermint, distilled water, petroleum ether, zeolite, distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail are taken over, T shape pipes；Distillation：In vapor generating bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, the screw clamp for unscrewing T shape pipes, is heated to boiling, when having a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screw clamp is screwed immediately, and vapor just enters distillation fraction, starts to distill.The average oil yield of present invention operation reaches 1.649ml/100g, reach 91.61% or more of peppermint branches and leaves theory oil content, avoid in solvent extraction process that there are the remaining drawbacks of organic solvent using steam distillation simultaneously, solve method extraction Peppermint essential oil of the prior art using extraction, organic solvent residual can not be avoided in extraction process, to ensure the purity of peppermint oil dementholized, the problem of being impacted to oil.
Description
Technical field
The present invention relates to peppermint oil purification technique field, specially a kind of peppermint oil dementholized method of purification.
Background technology
Peppermint, popular name are labiate " lunar caustic grass ", that is, belong to other drying herbs.It is born in hill wetland river more
Side, rhizome grow wild underground, are born in 2100 meters of height above sea levels, but can also be grown on 3500 meters of height above sea level, being one kind having extraordinary warp more
The fragrant crop for value of helping.Complete stool green gas fragrance.Leaf spends small lavender, lip to tie the granule fruit of dark violet brown after spending life.
Peppermint is one of Chinese conventional Chinese medicine.It is pungent cool property sweating antipyretic medicine, control influenza, headache, hot eyes, body heat, throat,
The diseases such as gum swelling and pain.External application can control neuralgia, pruitus, fash and eczema etc..Usually with peppermint for tea, clear away heart-fire improving eyesight.Light
The peppermint of canopy Greenhouse Fruit Picking is the fresh vegetable on Spring Festival dining table again.It is salubrious palatable.In China, peppermint is mainly with Jiangsu, two province of Anhui
Yield is maximum.Peppermint Planting pattern has three kinds of rhizome plant, plant division plant and cutting propagation.
Peppermint oil dementholized is colourless or flaxen supernatant liquid.There is special refrigerant fragrance, it is pungent, rear cool at the beginning of taste.Be aromatic drug,
Remedium corrigens and carminative.It can be used for skin or mucous membrane generate refrigerant sense to mitigate uncomfortable and pain.Separately there is liver-smoothing, qi-regulating, profit
Courage.It is mainly used for chronic lithogenous cholecystitis, chronic cholecystitis and gall stone liver and gall pent-up, the damp and hot stagnant card of stomach.
A kind of extracting method of Peppermint essential oil is proposed in the invention of Patent No. CN107686774A, including is walked as follows
Suddenly：Dried peppermint leaf is dried to water content 5% hereinafter, being crushed to 80 mesh, 75% alcohol is added and shakes 180 points of extraction at 15 DEG C
Clock filters to obtain filter residue and extracting solution, and extracting solution is centrifuged in 240r/min, takes upper layer fluid A；The invention is using extraction
Method extracts Peppermint essential oil, and organic solvent residual can not be avoided in extraction process, right to ensure the purity of peppermint oil dementholized
Oil impacts, for this purpose, it is proposed that a kind of peppermint oil dementholized method of purification.
Invention content
The purpose of the present invention is to provide a kind of peppermint oil dementholized methods of purification, to solve mentioned above in the background art ask
Topic.
To achieve the above object, the present invention provides the following technical solutions：A kind of peppermint oil dementholized method of purification, including walk as follows
Suddenly：
(1) preparation：Prepare peppermint, distilled water, petroleum ether, zeolite, distilling flask, condenser pipe, electric jacket, temperature
Meter, conical flask, tail take over, T shape pipes；
(2) it distills：In vapor generating bottle, the water for accounting for about container 3/4ths is added, whole device to be checked is not leaked
After gas, the screw clamp of T shape pipes is unscrewed, is heated to boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, stood
Screw screw clamp, vapor just enters distillation fraction, starts to distill, and when efflux is without apparent oil droplet, when clear, stops
Distillation；
(3) it detaches：It is extracted several times with petroleum ether, crude product is obtained, through CaCL2After drying, control temperature distills to obtain
Peppermint oil.
Preferably, the peppermint amount is 100-300 grams, water consumption 710-2100ml.
Preferably, when the peppermint amount is 100g, water consumption 710ml, when peppermint amount is 150g, water consumption is
1050ml。
Preferably, when the peppermint amount is 200g, water consumption 1400ml, when peppermint amount is 250g, water consumption is
1700ml, when peppermint amount is 300g, water consumption 2100ml.
Preferably, it is identified by refractometer after isolated peppermint oil dementholized in the step (3), index of refraction closes
Lattice ranging from 1.458-1.471.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is immiscible using Herba Menthae Haplocalycis volatile oil and water, when
After heated, when the summation of the two vapour pressure is equal with atmospheric pressure, mixed liquor comes to life, and continuing heating, then volatile oil is steamed with water
Steam distillation goes out, cooling and standings, isolated peppermint oil dementholized, safety easy to operate, and free from environmental pollution, passes through steam distillation
Experiment shows that average oil yield reaches 1.649ml/100g, reaches 91.61% or more of peppermint branches and leaves theory oil content, adopts simultaneously
It is avoided in solvent extraction process there are the remaining drawback of organic solvent with steam distillation, solves the prior art using extraction
Method extract Peppermint essential oil, organic solvent residual can not be avoided in extraction process, to ensure the purity of peppermint oil dementholized,
The problem of oil is impacted.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of technical solution：A kind of peppermint oil dementholized method of purification, includes the following steps：
(1) preparation：Prepare peppermint, distilled water, petroleum ether, zeolite, distilling flask, condenser pipe, electric jacket, temperature
Meter, conical flask, tail take over, T shape pipes；
(2) it distills：In vapor generating bottle, the water for accounting for about container 3/4ths is added, whole device to be checked is not leaked
After gas, the screw clamp of T shape pipes is unscrewed, is heated to boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, stood
Screw screw clamp, vapor just enters distillation fraction, starts to distill, and when efflux is without apparent oil droplet, when clear, stops
Distillation；
(3) it detaches：It is extracted several times with petroleum ether, crude product is obtained, through CaCL2After drying, control temperature distills to obtain
Peppermint oil.
Embodiment one：
It is first to prepare for work：Prepare 100g peppermints, 710ml distilled water, petroleum ether (30 DEG C of -60 DEG C of boiling ranges), zeolite,
Distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail take over, T shape pipes；Then it is distilled：In vapor generating bottle
In, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, unscrews the screw clamp of T shape pipes, is heated to boiling
It rises, when thering are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screws screw clamp immediately, vapor just enters distiller
Point, start to distill, when efflux is without apparent oil droplet, when clear, stops distillation；It is finally separating：Extracted several times with petroleum ether
It takes, obtains crude product, through CaCL2After drying, control temperature distills to obtain 1.62ml peppermint oils, oil yield 1.620ml/
100g identifies it by refractometer that index of refraction acceptability limit is 1.458-1.471 after isolated peppermint oil dementholized.
Embodiment two：
It is first to prepare for work：Prepare 150g peppermints, 1050ml distilled water, petroleum ether (30 DEG C of -60 DEG C of boiling ranges), boiling
Stone, distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail take over, T shape pipes；Then it is distilled：It is sent out in vapor
In raw bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, unscrews the screw clamp of T shape pipes, heating
To boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screw clamp is screwed immediately, vapor, which just enters, to be steamed
Part is evaporated, starts to distill, when efflux is without apparent oil droplet, when clear, stops distillation；It is finally separating：It is more with petroleum ether point
Secondary extraction, obtains crude product, through CaCL2After drying, control temperature distills to obtain 2.43ml peppermint oils, oil yield 1.620ml/
100g identifies it by refractometer that index of refraction acceptability limit is 1.458-1.471 after isolated peppermint oil dementholized.
Embodiment three：
It is first to prepare for work：Prepare 200g peppermints, 1400ml distilled water, petroleum ether (30 DEG C of -60 DEG C of boiling ranges), boiling
Stone, distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail take over, T shape pipes；Then it is distilled：It is sent out in vapor
In raw bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, unscrews the screw clamp of T shape pipes, heating
To boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screw clamp is screwed immediately, vapor, which just enters, to be steamed
Part is evaporated, starts to distill, when efflux is without apparent oil droplet, when clear, stops distillation；It is finally separating：It is more with petroleum ether point
Secondary extraction, obtains crude product, through CaCL2After drying, control temperature distills to obtain 3.21ml peppermint oils, oil yield 1.605ml/
100g identifies it by refractometer that index of refraction acceptability limit is 1.458-1.471 after isolated peppermint oil dementholized.
Example IV：
It is first to prepare for work：Prepare 250g peppermints, 1700ml distilled water, petroleum ether (30 DEG C of -60 DEG C of boiling ranges), boiling
Stone, distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail take over, T shape pipes；Then it is distilled：It is sent out in vapor
In raw bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, unscrews the screw clamp of T shape pipes, heating
To boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screw clamp is screwed immediately, vapor, which just enters, to be steamed
Part is evaporated, starts to distill, when efflux is without apparent oil droplet, when clear, stops distillation；It is finally separating：It is more with petroleum ether point
Secondary extraction, obtains crude product, through CaCL2After drying, control temperature distills to obtain 4.21ml peppermint oils, oil yield 1.684ml/
100g identifies it by refractometer that index of refraction acceptability limit is 1.458-1.471 after isolated peppermint oil dementholized.
Embodiment five：
It is first to prepare for work：Prepare 300g peppermints, 2100ml distilled water, petroleum ether (30 DEG C of -60 DEG C of boiling ranges), boiling
Stone, distilling flask, condenser pipe, electric jacket, thermometer, conical flask, tail take over, T shape pipes；Then it is distilled：It is sent out in vapor
In raw bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight, unscrews the screw clamp of T shape pipes, heating
To boiling, when there are a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screw clamp is screwed immediately, vapor, which just enters, to be steamed
Part is evaporated, starts to distill, when efflux is without apparent oil droplet, when clear, stops distillation；It is finally separating：It is more with petroleum ether point
Secondary extraction, obtains crude product, through CaCL2After drying, control temperature distills to obtain 5.15ml peppermint oils, oil yield 1.717ml/
100g identifies it by refractometer that index of refraction acceptability limit is 1.458-1.471 after isolated peppermint oil dementholized.
The present invention is immiscible using Herba Menthae Haplocalycis volatile oil and water, after heated, summation and the atmospheric pressure phase of the two vapour pressure
Whens equal, mixed liquor comes to life, and continuing heating, then volatile oil goes out with steam distillation, cooling and standings, isolated peppermint
Oil, safety easy to operate, and also it is free from environmental pollution, show that average oil yield reaches 1.649ml/ by steam distillation experiment
100g reaches 91.61% or more of peppermint branches and leaves theory oil content, while avoiding solvent extraction process using steam distillation
In there are the remaining drawback of organic solvent, solve method extraction Peppermint essential oil of the prior art using extraction, in extraction process
Organic solvent residual can not be avoided, to ensure the purity of peppermint oil dementholized, the problem of being impacted to oil.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of peppermint oil dementholized method of purification, it is characterised in that：Include the following steps：
(1) preparation：Prepare peppermint, distilled water, petroleum ether, zeolite, distilling flask, condenser pipe, electric jacket, thermometer, cone
Shape bottle, tail take over, T shape pipes；
(2) it distills：In vapor generating bottle, the water for accounting for about container 3/4ths is added, after whole device to be checked is air tight,
The screw clamp for unscrewing T shape pipes, is heated to boiling, and when having a large amount of vapor to generate and being gone out from the branch pipe of T shape pipes, screws immediately
Screw clamp, vapor just enter distillation fraction, start to distill, and when efflux is without apparent oil droplet, when clear, stop distillation；
(3) it detaches：It is extracted several times with petroleum ether, crude product is obtained, through CaCL2After drying, control temperature distills to obtain peppermint
Oil.
2. a kind of peppermint oil dementholized method of purification according to claim 1, it is characterised in that：The peppermint amount is 100-300
Gram, water consumption 710-2100ml.
3. a kind of peppermint oil dementholized method of purification according to claim 2, it is characterised in that：When the peppermint amount is 100g,
Water consumption is 710ml, when peppermint amount is 150g, water consumption 1050ml.
4. a kind of peppermint oil dementholized method of purification according to claim 2, it is characterised in that：When the peppermint amount is 200g,
Water consumption is 1400ml, when peppermint amount is 250g, water consumption 1700ml, and when peppermint amount is 300g, water consumption 2100ml.
5. a kind of peppermint oil dementholized method of purification according to claim 1, it is characterised in that：It is detached in the step (3)
It is identified by refractometer after to peppermint oil dementholized, index of refraction acceptability limit is 1.458-1.471.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810565473.4A CN108795576A (en) | 2018-06-04 | 2018-06-04 | A kind of peppermint oil dementholized method of purification |
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| CN201810565473.4A CN108795576A (en) | 2018-06-04 | 2018-06-04 | A kind of peppermint oil dementholized method of purification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574821A (en) * | 2020-12-02 | 2021-03-30 | 太极集团重庆涪陵制药厂有限公司 | Traditional Chinese medicine volatile oil extraction equipment and extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560400A (en) * | 2014-12-26 | 2015-04-29 | 江苏省中国科学院植物研究所 | Method for extracting peppermint oil |
| CN104629904A (en) * | 2013-11-07 | 2015-05-20 | 张湉 | Peppermint oil simple extraction method |
| CN104974853A (en) * | 2015-07-17 | 2015-10-14 | 王再青 | Method for extracting peppermint essential oil |
| CN105647646A (en) * | 2015-12-30 | 2016-06-08 | 安徽银丰药业股份有限公司 | Mint leaf extraction technology |
-
2018
- 2018-06-04 CN CN201810565473.4A patent/CN108795576A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629904A (en) * | 2013-11-07 | 2015-05-20 | 张湉 | Peppermint oil simple extraction method |
| CN104560400A (en) * | 2014-12-26 | 2015-04-29 | 江苏省中国科学院植物研究所 | Method for extracting peppermint oil |
| CN104974853A (en) * | 2015-07-17 | 2015-10-14 | 王再青 | Method for extracting peppermint essential oil |
| CN105647646A (en) * | 2015-12-30 | 2016-06-08 | 安徽银丰药业股份有限公司 | Mint leaf extraction technology |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574821A (en) * | 2020-12-02 | 2021-03-30 | 太极集团重庆涪陵制药厂有限公司 | Traditional Chinese medicine volatile oil extraction equipment and extraction method |
| CN112574821B (en) * | 2020-12-02 | 2023-05-09 | 太极集团重庆涪陵制药厂有限公司 | Traditional Chinese medicine volatile oil extraction equipment and extraction method |
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Application publication date: 20181113 |