CN108048220A - A kind of method of low temperature extraction rosemary oil - Google Patents

A kind of method of low temperature extraction rosemary oil Download PDF

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Publication number
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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CN
China
Prior art keywords
extraction
rosemary
rosemary oil
temperature
carbon dioxide
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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.)
Pending
Application number
CN201711376952.3A
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Chinese (zh)
Inventor
滕春娟
朱成业
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Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
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Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd filed Critical Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
Priority to CN201711376952.3A priority Critical patent/CN108048220A/en
Publication of CN108048220A publication Critical patent/CN108048220A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction

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

A kind of method of low temperature extraction rosemary oil
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.
CN201711376952.3A 2017-12-19 2017-12-19 A kind of method of low temperature extraction rosemary oil Pending CN108048220A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711376952.3A CN108048220A (en) 2017-12-19 2017-12-19 A kind of method of low temperature extraction rosemary oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711376952.3A CN108048220A (en) 2017-12-19 2017-12-19 A kind of method of low temperature extraction rosemary oil

Publications (1)

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CN108048220A true CN108048220A (en) 2018-05-18

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Cited By (1)

* Cited by examiner, † Cited by third party
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

Citations (6)

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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 examiner, † Cited by third party
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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Application publication date: 20180518

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