CN102807921A - Method for preparing cypress essential oil by combining water vapor distillation with supercritical CO2 extraction - Google Patents
Method for preparing cypress essential oil by combining water vapor distillation with supercritical CO2 extraction Download PDFInfo
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- CN102807921A CN102807921A CN 201210339865 CN201210339865A CN102807921A CN 102807921 A CN102807921 A CN 102807921A CN 201210339865 CN201210339865 CN 201210339865 CN 201210339865 A CN201210339865 A CN 201210339865A CN 102807921 A CN102807921 A CN 102807921A
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Abstract
The invention relates to a method for preparing cypress essential oil by combining water vapor distillation with supercritical CO2 extraction. The obtained cypress essential oil has clear luster, natural fragrant flavor and double efficacies of heath care and medical treatment. The production process is environment-friendly. The method comprises the following steps: firstly, cleaning washing perennial woody cypress rootstock and drying; finely crushing dry cypress wood ship, feeding the crushed dry cypress wood ships into the bottom of a water vapor distillation tank and enabling the wood chips to be uniformly distributed; then distilling the wood chips with water steam, enabling the obtained liquid to enter a constant-temperature oil-water separator to obtain the cypress essential oil and cypress hydrolat, namely a solution in a water phase; collecting the cypress wood chips subjected to the distillation and extraction and filling the cypress wood chips into an extraction kettle; setting the temperature to be 45-60D EG C, the pressure to be 20-30MPa, the dynamic extraction time to be 2-3 hours and the static extraction time to be 3 hours; secondarily extracting the cypress in the extraction kettle with supercritical CO2; and finally, mixing the essential oil obtained by distillation of the water steam with the essential oil obtained by extraction of the supercritical CO2, adding active carbon for decoloring and filtering out impurities by using a filter screen to obtain the cypress essential oil.
Description
Technical field
The present invention relates to a kind of extracts essential oil method, relate to more specifically a kind ofly unite supercritical CO with wet distillation
2The method that Chinese juniper another name for oil is got in the extraction process preparation.
Technical background
Essential oil is the general name that has certain volatile oily composition in the plant materials, has more biomedical activity, like anti-inflammatory, and analgesia; Calm the nerves, expelling parasite is eliminated the phlegm, cough-relieving; Wind dispelling, sweating, degerming; Skin care or the like, to improving the body normal physiological activity, promotion and protection immunity system have great importance.The research proof, different essential oils all have all well and good curative effect for the disease of internal secretion, metabolism, urinary system, venereal disease, immunity system, gynaecopathia, muscle, skeletal diseases, dermatosis, neural system and Psychiatric disorders, eye, ear, nose, oral cavity, odontopathy, respiratory system aspect, the disease of blood circulation aspect, the disease of Digestive tract aspect.But, often be limited to use owing to reasons such as the synthetic essential oil inherent insecurity of chemical industry.And Chinese juniper another name for oil is universally acknowledged senior natural perfume, is derived from rare tree species such as Japan cypress, Chamaecyparis formosensis and yellow Chinese juniper.The pure natural essential oil that forms refines in institutes such as Japan cypress, and its oil is limpid, and quality is excellent, and it is multiple to human body beneficial's composition to contain chamene, widdrene, eedrene, cypress camphor and Hydagen B etc., has health care and medical dual-use function.Have the very strong calm effect of allaying excitement like cypress camphor, and cancer cells such as lung cancer are had suppress effect more by force.Hydagen B is a kind of good wide spectrum natural antibiotics, can effectively kill multiple germ.The GB tissue of American-European Japanese various countries, FAO (food and agriculture organization) and WHO (World Health Organization) all are spendable natural additive with its authorization.Chinese juniper another name for oil also has multiple good physiological and pharmacological activity simultaneously.External report, it contains the sensory nervous system of neuropeptide, cardiovascular, pulmonary function, thermoregulation, stomach and intestine function to some has remarkably influenced, also has effects such as anti-inflammatory, analgesia, antibiotic, antiviral and deinsectization.
Essential oil generally refines preparation through steam distillation, extrusion process, cold-maceration or solvent-extraction process on producing.In traditional technology, generally extract Chinese juniper another name for oil through wet distillation.But the steam distillation productive rate is lower, extracts the essential oil quantity not sufficient.The productive rate of extrusion process and cold-maceration is on the low side equally.And solvent-extraction process very easily causes extraction solvent residual, and some poisonous and hazardous solvents greatly influence the essential oil quality; Tend to have irritating smell in the essential oil, it is impure to show as fragrance, and color is dark excessively; Transparency is bad or the like, and processing tends to cause environmental pollution to organic solvent.Supercritical CO
2Extraction process is a kind of environmental protection essential oil extracting process efficiently, but this method can not obtain volatile and water-soluble effective constituent.
Summary of the invention
The objective of the invention is to overcome the deficiency of original technology, a kind of wet distillation and supercritical CO are provided
2The method of extraction process associating is extracted Chinese juniper another name for oil.Chinese juniper wood rhizome etc. is at first carried out wet distillation extract the part essential oil; The wooden slag particle of Chinese juniper wood after will extracting then is dry, sends in the supercritical extraction unit again, extracts wherein remaining Chinese juniper another name for oil; Can greatly improve productive rate, and obtain quality essential oil product preferably.
The supercritical extraction unit that the present invention adopted is a HA420-40-96 type supercritical CO
2Extraction plant, Huaan, Nantong break bounds extraction ltd produces.
A kind of wet distillation associating supercritical CO
2Extraction prepares the method for Chinese juniper another name for oil:
(1) forest farms, province such as osmanthus, Yunnan, western part of China Sichuan and Shanxi are provided, the perennial wooden Chinese juniper wood rhizome material of become a useful person Japan cypress and yellow Chinese juniper is removed impurity such as epidermis sandy soil with the water blast gun washes clean, then with infrared drier cure to water cut below 10%.Be cut into mechanical chopper again and be about 7 centimetres, wide about 3 centimetres, the fuzz stick of thickness about 0.3 centimetre.
(2) pulverizing Chinese juniper wood fuzz stick makes it become the particle powder between the 5-30 order, and the bottom of the wet distillation of packing into jar also keeps the wood chip uniform distribution.
(3) constantly feed 100 ℃ water vapour to the retort bottom, and open the vapour line of retort top, connect spiral condenser, the time length is 2 to 3 hours.After the steam condensation, the liquid that obtains gets into the thermostatical oil separator, separates the profit two-phase, further filters removal impurity with filter screen, and can get Chinese juniper another name for oil is the solution of aqueous phase with Chinese juniper wood hydrosol.
(4) the Chinese juniper wood wood chip that wet distillation was extracted is collected, and dry through drying machine once more, is filled in the extraction kettle of HA420-40-96 supercritical extraction unit.
(5) setting extraction temperature is 45 to 60 ℃, and extracting pressure is 20 to 30MPa, and the dynamic extraction time is 2 to 3 hours, and the static extracting time is 3 hours, with supercritical CO
2Chinese juniper wood in the extraction kettle extracts once more.
(6) after extraction process finishes, close well heater, pressure is set is 0 and close CO
2Air valve is opened the multiplication of voltage valve, takes out the residual wooden slag of Chinese juniper in the extraction kettle, collects the Chinese juniper another name for oil of extraction back gained simultaneously with receiving bottle, treats CO
2Weigh after the volatilization fully and obtain product.
(7) essential oil and the supercritical CO that wet distillation are obtained
2Extraction gained essential oil mixes, and adds about 50 to 100 gram activated carbon and decolours, and removes impurity with strainer filtering, can obtain the transparent oily Chinese juniper of orange yellow another name for oil.
The present invention has following characteristics:
Chinese juniper another name for oil colours of the present invention pool clarification, the natural fragrance of fragrance, outward appearance and quality are all excellent, and it is multiple to human body beneficial's composition to contain chamene, widdrene, eedrene and cypress camphor etc. simultaneously, has health care and medical double effects.
Of the present invention is raising and improvement to traditional wet distillation and supercritical extraction method, and the essential oil that especially to be fit to perennial Chinese juniper wood rhizome be raw material extracts.Do not add any poisonous and harmful solvent in the production, meet the needs of environmental protection.
The steam distillation yield that the present invention is more traditional improves.The yield that the script wet distillation obtains essential oil is about about 1%, and a large amount of essential oils are present in the wooden slag, cause a lot of wastes.And yield of the present invention is about 3%, is more than the original twice.
The present invention is except obtaining essential oil, and the aqueous phase solution product that can keep simultaneously in the wet distillation is a hydrosol.
Gained essential oil effective constituent cypress camphor content of the present invention is higher, can significantly improve the grade of product.
The Chinese juniper another name for oil of gained of the present invention, through China Guangzhou Analysis &. Test Center, authoritative institution's repeated detection such as the little spectrum analysis in Shanghai test center identify that its staple such as table 1 are listed.
The main effective constituent of table 1 Chinese juniper another name for oil
Embodiment
Come the present invention is further described below in conjunction with specific embodiment.
Embodiment one:
Concrete steps are following:
(1) forest farms, province such as osmanthus, Yunnan, western part of China Sichuan and Shanxi are provided, 200 kilograms on the perennial wooden Chinese juniper wood rhizome of become a useful person Japan cypress and yellow Chinese juniper is removed impurity with the water blast gun Washing, again with infrared drier cure to water cut below 10%; Be cut into mechanical chopper at last and be about 7 centimetres, wide about 3 centimetres, thickness is at 0.3 centimetre fuzz stick.With the particle below meticulous powder to 5 order of fuzz stick, be packed into the bottom of wet distillation jar and keep the wood chip uniform distribution.
(2) constantly feed 100 ℃ water vapour to the retort bottom, and open the vapour line of retort top, connect spiral condenser, the time length is 2 hours.After the steam condensation, the liquid that obtains gets into the thermostatical oil separator, separates the profit two-phase, further filters removal impurity with filter screen, can get part Chinese juniper another name for oil and Chinese juniper wood hydrosol (being the solution of aqueous phase).
(4) the Chinese juniper wood wood chip that wet distillation was extracted is collected; And dry through drying machine once more, be filled in the extraction kettle of HA420-40-96 supercritical extraction unit after, setting extraction temperature is 45 ℃; Extracting pressure is 20MPa; The dynamic extraction time is 2 hours, and the static extracting time is 3 hours, with supercritical CO
2Chinese juniper wood in the extraction kettle extracts once more.
(5) close well heater after about 3 hours, pressure is set is 0 and close CO
2Air valve is opened the multiplication of voltage valve, takes out the residual wooden slag of Chinese juniper in the extraction kettle, collects the Chinese juniper another name for oil of extraction back gained simultaneously with receiving bottle, treats CO
2After the volatilization fully, essential oil and supercritical CO that wet distillation is obtained
2Extraction gained essential oil mixes, and adds about 50 gram activated carbon and decolours, and removes impurity with strainer filtering, can obtain the transparent oily Chinese juniper of orange yellow another name for oil.
Embodiment two:
Concrete steps are following:
(1) forest farms, province such as osmanthus, Yunnan, western part of China Sichuan and Shanxi are provided, 220 kilograms on the perennial wooden Chinese juniper wood rhizome of become a useful person Japan cypress and yellow Chinese juniper is removed impurity with the water blast gun Washing, again with infrared drier cure to water cut below 10%; Be cut into mechanical chopper at last and be about 7 centimetres, wide about 3 centimetres, thickness is at 0.3 centimetre fuzz stick.With the particle below meticulous powder to 15 order of fuzz stick, be packed into the bottom of wet distillation jar and keep the wood chip uniform distribution.
(2) constantly feed 100 ℃ water vapour to the retort bottom, and open the vapour line of retort top, connect spiral condenser, the time length is 2.5 hours.After the steam condensation, the liquid that obtains gets into the thermostatical oil separator, separates the profit two-phase, further filters removal impurity with filter screen, can get part Chinese juniper another name for oil and Chinese juniper wood hydrosol (being the solution of aqueous phase).
(4) the Chinese juniper wood wood chip that wet distillation was extracted is collected; And dry through drying machine once more, be filled in the extraction kettle of HA420-40-96 supercritical extraction unit after, setting extraction temperature is 55 ℃; Extracting pressure is 23MPa; The dynamic extraction time is 2.5 hours, and the static extracting time is 3 hours, with supercritical CO
2Chinese juniper wood in the extraction kettle extracts once more.
(5) close well heater after about 3 hours, pressure is set is 0 and close CO
2Air valve is opened the multiplication of voltage valve, takes out the residual wooden slag of Chinese juniper in the extraction kettle, collects the Chinese juniper another name for oil of extraction back gained simultaneously with receiving bottle, treats CO
2After the volatilization fully, essential oil and supercritical CO that wet distillation is obtained
2Extraction gained essential oil mixes, and adds about 80 gram activated carbon and decolours, and removes impurity with strainer filtering, can obtain the transparent oily Chinese juniper of orange yellow another name for oil.
Embodiment three:
Concrete steps are following:
(1) forest farms, province such as osmanthus, Yunnan, western part of China Sichuan and Shanxi are provided, 240 kilograms on the perennial wooden Chinese juniper wood rhizome of become a useful person Japan cypress and yellow Chinese juniper is removed impurity with the water blast gun Washing, again with infrared drier cure to water cut below 10%; Be cut into mechanical chopper at last and be about 7 centimetres, wide about 3 centimetres, thickness is at 0.3 centimetre fuzz stick.With the particle below meticulous powder to 30 order of fuzz stick, be packed into the bottom of wet distillation jar and keep the wood chip uniform distribution.
(2) constantly feed 100 ℃ water vapour to the retort bottom, and open the vapour line of retort top, connect spiral condenser, the time length is 3 hours.After the steam condensation, the liquid that obtains gets into the thermostatical oil separator, separates the profit two-phase, further filters removal impurity with filter screen, can get part Chinese juniper another name for oil and Chinese juniper wood hydrosol (being the solution of aqueous phase).
(4) the Chinese juniper wood wood chip that wet distillation was extracted is collected; And dry through drying machine once more, be filled in the extraction kettle of HA420-40-96 supercritical extraction unit after, setting extraction temperature is 60 ℃; Extracting pressure is 30MPa; The dynamic extraction time is 2 hours, and the static extracting time is 3 hours, with supercritical CO
2Chinese juniper wood in the extraction kettle extracts once more.
(5) close well heater after about 3 hours, pressure is set is 0 and close CO
2Air valve is opened the multiplication of voltage valve, takes out the residual wooden slag of Chinese juniper in the extraction kettle, collects the Chinese juniper another name for oil of extraction back gained simultaneously with receiving bottle, treats CO
2After the volatilization fully, essential oil and supercritical CO that wet distillation is obtained
2Extraction gained essential oil mixes, and adds about 100 gram activated carbon and decolours, and removes impurity with strainer filtering, can obtain the transparent oily Chinese juniper of orange yellow another name for oil.
Claims (1)
1. a wet distillation is united supercritical CO
2Extraction prepares the method for Chinese juniper another name for oil, it is characterized in that this method is by following
Step realizes:
(1) forest farms, province such as osmanthus, Yunnan, western part of China Sichuan and Shanxi is provided the perennial wooden Chinese juniper wood rhizome material washes clean of become a useful person Japan cypress and yellow Chinese juniper, drying; Be cut into mechanical chopper and be about 7 centimetres; Wide about 3 centimetres, thickness behind the fuzz stick about 0.3 centimetre, pulverizing Chinese juniper wood fuzz stick; Make it become the particle between the 5-30 order, the bottom of the wet distillation of packing into jar also keeps the wood chip uniform distribution;
(2) the continuous steam that feeds 100 ℃ to the alembic bottom; And open the steam pipework of alembic top; Connect coil condenser; After the steam condensation; The liquid that obtains gets into the thermostatical oil separator; Separate the profit two-phase, filter and remove impurity, obtaining Chinese juniper another name for oil is the solution of aqueous phase with Chinese juniper wood hydrosol;
(3) the Chinese juniper wood wood chip that wet distillation was extracted is collected; Behind the after drying, be filled in the extraction kettle of HA420-40-96 supercritical extraction unit, setting extraction temperature is 45 to 60 ℃; Extracting pressure is 20 to 30MPa; The dynamic extraction time is 2 to 3 hours, and the static extracting time is 3 hours, with supercritical CO
2After Chinese juniper wood in the extraction kettle extracted once more, essential oil and supercritical CO that wet distillation is obtained
2Extraction gained essential oil mixes, and adds activated carbon and decolours, and further filters removal impurity with filter screen, can obtain the transparent oily Chinese juniper of orange yellow another name for oil.
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| CN105273843A (en) * | 2015-11-27 | 2016-01-27 | 四川昱天成科技有限公司 | Extraction method of wood essential oil |
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| CN105159074B (en) * | 2015-08-19 | 2017-08-29 | 四川九渊医药科技有限公司 | The optimization method of volatile oil in a kind of extensive extraction medicinal material |
| CN105273843A (en) * | 2015-11-27 | 2016-01-27 | 四川昱天成科技有限公司 | Extraction method of wood essential oil |
| CN105726363A (en) * | 2016-02-26 | 2016-07-06 | 广州环亚化妆品科技有限公司 | Plant care composition and preparation method thereof |
| CN105754721A (en) * | 2016-02-29 | 2016-07-13 | 广东阿妈生物科技有限公司 | Platycladus orientalis essential oil with efficient sterilization and inflammation diminishing functions as well as preparation method and application of platycladus orientalis essential oil |
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| CN108837003A (en) * | 2018-06-25 | 2018-11-20 | 陈靈悦 | A kind of degradable respiratory tract harmful microbe material and preparation method thereof |
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| CN109593112A (en) * | 2018-12-29 | 2019-04-09 | 中商国能孵化器集团有限公司 | A kind of insect bioprotein extract and the preparation method and application thereof |
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Application publication date: 20121205 |