CN108048220A - A kind of method of low temperature extraction rosemary oil - Google Patents
A kind of method of low temperature extraction rosemary oil Download PDFInfo
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- CN108048220A CN108048220A CN201711376952.3A CN201711376952A CN108048220A CN 108048220 A CN108048220 A CN 108048220A CN 201711376952 A CN201711376952 A CN 201711376952A CN 108048220 A CN108048220 A CN 108048220A
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- extraction
- rosemary
- rosemary oil
- temperature
- carbon dioxide
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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
- C11B9/025—Recovery by solvent extraction
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of low-temperature extraction method of rosemary oil, this method is that rosemary oil is extracted from rosemary leave with supercritical liquid extraction technique.Rosemary leave is dried before extraction, is crushed, extraction temperature is 35~40 DEG C, and pressure is 30~40MPa；Carbon dioxide is 200~400kg/h by the flow of extraction kettle, and extraction time is 2~4h.The present invention is by the use of the CO 2 fluid under above-critical state as extractant, which recycles in same system, and solvent consumption is small, and price is cheap, therefore extracts at low cost.CO 2 fluid is green non-pollution solvent, and the rosemary oil of extraction has the features such as quality is good, and purity is high, and color and luster is good, free from extraneous odour, no solvent residue, non-environmental-pollution, and extraction temperature is low, the heat-sensitive substance in survivable product, and extraction cycle is short.Present invention process is simple, and low energy consumption.
Description
Technical field
The invention belongs to technical field of natural product extraction, and in particular to a kind of supercritical extraction method of rosemary oil.
Background technology
Rosemary is Labiatae Rosmarinus plant, and evergreen shrubs, ingredient is mainly diterpene phenols, flavonoids, triterpene
Class and essential oil etc. can be widely used in drug, foods and cosmetics etc..Traditional rosemary oil extractive technique is organic molten
The problems such as agent extraction method although recovery rate is higher, exists and destroys active ingredient, dissolvent residual, while solvent-oil ratio is big, easily
Environmental pollution is caused, limits application of the rosemary oil in pharmaceuticals and food, so the fan of developmental research green high-efficient changes
Sesame oil extractive technique is the key that one of comprehensive utilization rosemary.Supercritical liquid extraction technique is developed in recent years one
Kind of high efficient separation technology, be the fluid by the use of under supercriticality as extractant, extracted from liquid or solid material
A kind of new separation technology of certain component.
The content of the invention
It is an object of the present invention to provide a kind of methods of low temperature extraction rosemary oil, improve the quality of rosemary oil, subtract
Small environment pollution reduces extraction cost.
Technical scheme：
The present invention proposes a kind of low-temperature extraction method of rosemary oil, and this method is using supercritical carbon dioxide fluid
Rosemary oil is extracted from rosemary leave；Comprise the following steps：Drying → crushing → extraction → separation.
Wherein, drying is that rosemary leave is put into baking oven, and rosemary is dried to water content for 10 at a temperature of 50~60 DEG C
~12% dry rosemary leave.Crushing is that dried rosemary leave is put into the fan that 20~40 mesh of grain size is ground into pulverizer
Repeatedly spiceleaf powder.By drying process, the requirement to the temperature and pressure of supercritical carbon dioxide can be reduced so that in relatively low temperature
Under degree and pressure can either high efficiency complete extraction, and the service life of device can be extended, and the material after crushing disclosure satisfy that
Our requirements to material particular diameter increase the contact area of material and solvent, can greatly improve extraction yield.
Extraction step is that suitable rosemary leave powder is put into the material barrel of extraction kettle, and carbon dioxide is injected and is extracted
Kettle is taken, carbon dioxide in extraction kettle is kept to be contacted in supercriticality with natural material, makes the oiliness in rosemary leave powder
Ingredient is dissolved among supercritical fluid.
Wherein, supercritical temperature is 35~40 DEG C, and pressure is 30~40MPa；The stream that carbon dioxide passes through extraction kettle
It measures as 200~400kg/h, extraction time is 2~4h.
Separating step is under optimum process condition, separating still pressure is adjusted in 4~6.5MPa or so, from separating still
Collect the fluid containing rosemary oil in outlet.Under optimum process condition, the recovery rate of rosemary oil is 1.45%, recovery rate=extraction
Go out amount of substance/material quality * 100%.
Compared with prior art, the invention has the characteristics that：By the use of the CO 2 fluid under supercriticality as extraction
Solvent is taken, which recycles in same system, and solvent consumption is small and price is cheap, therefore extracts at low cost；Extraction temperature
It spends low, reduces energy consumption；CO 2 fluid is green non-pollution solvent, and the rosemary oil of extraction has quality good, and purity is high,
The features such as color and luster is good, free from extraneous odour, no solvent residue, non-environmental-pollution, and extraction cycle is short.Present invention process is simple, and low energy consumption.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment.
Embodiment 1：
Embodiment is as follows：Rosemary leave is put into baking oven, it is dried to water content 10% at a temperature of 50 DEG C, it will be dry
Rosemary leave after dry, which is put into pulverizer, is ground into 20 mesh powders；It weighs rosemary leave powder 3.0kg and is put into extraction kettle
In material barrel, carbon dioxide is injected into extraction kettle, the temperature and pressure for keeping carbon dioxide in extraction kettle is super at it
Critical condition is contacted with natural material；Extraction temperature is 35 DEG C, pressure 30MPa；The stream that carbon dioxide passes through extraction kettle
Measure makes the oil components in rosemary leave powder be completely dissolved among supercritical fluid for 200kg/h, extraction time 3h, from
Collect the fluid containing rosemary oil in the outlet of separating still.Obtain discharging 42.5g, recovery rate 1.45%.
Embodiment 2：
Embodiment is as follows：Rosemary leave is put into baking oven, it is dried to water content 12% at a temperature of 55 DEG C, it will be dry
Rosemary leave after dry, which is put into pulverizer, is ground into 30 mesh powders；It weighs rosemary leave powder 3.4kg and is put into extraction kettle
In material barrel, carbon dioxide is injected into extraction kettle, the temperature and pressure for keeping carbon dioxide in extraction kettle is super at it
Critical condition is contacted with natural material；Extraction temperature is 35 DEG C, pressure 40MPa；The stream that carbon dioxide passes through extraction kettle
Measure makes the oil components in rosemary leave powder be completely dissolved among supercritical fluid for 300kg/h, extraction time 3h, from
Collect the fluid containing rosemary oil in the outlet of separating still.Obtain discharging 49.0g, recovery rate 1.44%.
Embodiment 3：
Embodiment is as follows：Rosemary leave is put into baking oven, it is dried to water content 10% at a temperature of 60 DEG C, it will be dry
Rosemary leave after dry, which is put into pulverizer, is ground into 40 mesh powders；It weighs rosemary leave powder 3.75kg and is put into extraction kettle
In material barrel, carbon dioxide is injected into extraction kettle, the temperature and pressure for keeping carbon dioxide in extraction kettle is super at it
Critical condition is contacted with natural material；Extraction temperature is 40 DEG C, pressure 40MPa；The stream that carbon dioxide passes through extraction kettle
Measure makes the oil components in rosemary leave powder be completely dissolved among supercritical fluid for 400kg/h, extraction time 4h,
The fluid containing rosemary oil is collected from the outlet of separating still.Obtain discharging 45.8g, recovery rate 1.22%.
Each embodiment result of the test is as follows：
Certainly, simply the concrete application example of the present invention, the also other embodiments of the present invention are all using equivalent more than
The technical solution that replacement or equivalent transformation are formed, all falls within protection domain of the presently claimed invention.
Claims (3)
1. a kind of method of low temperature extraction rosemary oil, this method is to be carried using supercritical carbon dioxide fluid from rosemary leave
Take rosemary oil, it is characterised in that：Rosemary leave is dried before extraction, is crushed, it will be after moderately crushing during extraction
Rosemary leave powder is put into the material barrel of extraction kettle, and carbon dioxide injected extraction kettle, keep temperature in extraction kettle and
Pressure carbon dioxide supercriticality and contacted with natural material, make the rosemary oil ingredient in rosemary leave powder
It is dissolved among supercritical fluid, the fluid containing rosemary oil is collected from the outlet of separating still.
2. the method for low temperature extraction rosemary oil according to claim 1, it is characterised in that：The drying is by rosemary
Leaf is put into baking oven, and water content is dried in the range of 10~12% to it at a temperature of 50~60 DEG C；The crushing is will to dry
Rosemary leave afterwards is put into the rosemary leave powder that pulverizer is ground into 20~40 mesh of grain size.
3. the method for low temperature extraction rosemary oil according to claim 1 or 2, it is characterised in that：The supercriticality
Temperature is 35~40 DEG C, and pressure is 30~40MPa；Carbon dioxide is 200~400kg/h by the flow of extraction kettle, is extracted
It is 2~4h, 4~6.5MPa of separating still pressure to take the time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711376952.3A CN108048220A (en) | 2017-12-19 | 2017-12-19 | A kind of method of low temperature extraction rosemary oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711376952.3A CN108048220A (en) | 2017-12-19 | 2017-12-19 | A kind of method of low temperature extraction rosemary oil |
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| CN108048220A true CN108048220A (en) | 2018-05-18 |
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| CN201711376952.3A Pending CN108048220A (en) | 2017-12-19 | 2017-12-19 | A kind of method of low temperature extraction rosemary oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609275A (en) * | 2019-01-04 | 2019-04-12 | 湖北瑞晟生物有限责任公司 | A kind of extraction process of Rosemary Oil |
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| CN102199092A (en) * | 2010-03-26 | 2011-09-28 | 禹州市森源本草天然产物有限公司 | Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L. |
| CN104498179A (en) * | 2014-12-18 | 2015-04-08 | 贵州航天乌江机电设备有限责任公司 | Method for extracting okra seed oil |
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| CN104711113A (en) * | 2014-12-18 | 2015-06-17 | 贵州航天乌江机电设备有限责任公司 | Method for making onion oil at low temperature |
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2017
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1333326A (en) * | 2001-08-27 | 2002-01-30 | 海南万恒生物工程有限公司 | Rosemary essential oil, antioxidant and preparation process thereof |
| CN102199092A (en) * | 2010-03-26 | 2011-09-28 | 禹州市森源本草天然产物有限公司 | Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L. |
| CN104498179A (en) * | 2014-12-18 | 2015-04-08 | 贵州航天乌江机电设备有限责任公司 | Method for extracting okra seed oil |
| CN104560380A (en) * | 2014-12-18 | 2015-04-29 | 贵州航天乌江机电设备有限责任公司 | Process for extracting wheat germ oil by using supercritical method |
| CN104711113A (en) * | 2014-12-18 | 2015-06-17 | 贵州航天乌江机电设备有限责任公司 | Method for making onion oil at low temperature |
| CN106281711A (en) * | 2016-08-28 | 2017-01-04 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of rosemary ethereal oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609275A (en) * | 2019-01-04 | 2019-04-12 | 湖北瑞晟生物有限责任公司 | A kind of extraction process of Rosemary Oil |
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