CN105505583A - A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid - Google Patents
A method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid Download PDFInfo
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- CN105505583A CN105505583A CN201510821381.4A CN201510821381A CN105505583A CN 105505583 A CN105505583 A CN 105505583A CN 201510821381 A CN201510821381 A CN 201510821381A CN 105505583 A CN105505583 A CN 105505583A
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- spiceleaf
- pelargonii graveolentis
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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
- C11B9/022—Refining
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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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- 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
Abstract
The invention relates to a method of extracting bay leaf oil from bay leaves with subcritical n-butane fluid. The method includes smashing, adding into a tank, dipping with an n-butane solvent, extracting, distilling, and the like. Extraction temperature and pressure can be accurately controlled by utilization of a subcritical extraction device. The method is high in extraction efficiency, low in device manufacturing cost, high in raw material treating amount, simple in process, low in production cost and free of solvent residue. A whole process of the method is performed at low temperature under an oxygen-free state. Extraction and separation are performed at the same time. The extraction speed is high. Recovery and reutilization of the solvent can be achieved.
Description
Technical field
The invention belongs to spice and extract field, specifically, is a kind of method that subcritical normal butane fluid extracts Oleum Pelargonii Graveolentis from spiceleaf.
Background technology
Spiceleaf (bayleaf also makes laurelleaf), have another name called fragrant Chinese mugwort, fragrant osmanthus leaf, Folium Lauri nobilis, cinnamomum japonicum, for the Lauraceae moon belongs to evergreen dungarunga, originate in Mediterranean Zone, also have cultivation on China Zhejiang, Jiangsu, Fujian, Guangdong, Guangxi, Sichuan, Hunan, Anhui and other places.Its cured leaf ovalize, top point (or blunt), short petiole, edgewave wave-like, page green (sometimes yellow), north look shallow, the long 25mm ~ 100mm of leaf, wide 20mm ~ 45mm.Blade edible, is commonly used in the cooking, is used for western-style food, soup, meat, vegetables, boiled dinner etc., has Titian to increase taste effect.Chinese materia medica thinks that it also has the effect of coordinating intestines and stomach, dispelling cold analgesia, raising immunizing power.Containing essential oil, catechin, flavonoid compound and pycnogenols etc. in leaf.Spiceleaf essential oil has fresh strong and comfortable fragrance and sharp flavor, and fragrance is similar with cajuput oil to cloves, the sweet pungent grace of lingering fragrance, and fragrance is sweet and not bitter, is commonly used in daily essence.
The method of current extraction Oleum Pelargonii Graveolentis commonly uses steam distillation, also useful supercritical CO
2fluids extraction, but actually rare.Steam distillation Extracting temperature is higher, and the composition easily making boiling point lower volatilization, extract volatile oil yield lower, be generally 0.5% ~ 1.5%.Supercritical CO in recent years
2abstraction technique development is comparatively rapid, and the plants essential oil obtained is safe, clean, and extraction efficiency is high, but equipment running cost is high, supercritical CO
2extraction Oleum Pelargonii Graveolentis, yield is generally 2% ~ 3%.
Subcritical abstraction technology is a kind of novel extraction isolation technique grown up based on closely knit fluid extraction theory, some low boiling point solvents are utilized to have lower viscosity and higher spread coefficient at subcritical state, mass transfer is fast, the feature that dissolving power is strong, according to similar dissolve mutually theory, by controlling the pressure and temperature of extraction solvent, effective constituent is dissolved from target compound, to be extractedly to reach after balance decompression separation subcritical fluids again, thus obtain target component, be considered to a kind of green, Sustainable development technology.These advantages make subcritical abstraction technology be developed rapidly, are especially widely applied in the extraction of natural product, are widely used in fields such as medicine, food, biology, essence and flavoring agents.Conventional subcritical fluids has propane, butane, Tetrafluoroethane, dme and No. six solvents etc.
Subcritical abstraction is the new technology be born after supercritical liquid extraction technique, Chinese patent literature 201310741244.0 discloses a kind of method of subcritical fluid extraction tea leaf extract, comprise the following steps, by tealeaves temperature 15 ~ 60 DEG C, under pressure 0.4 ~ 3MPa, adopt the continuous dynamic extraction 30-270min of dme subcritical fluids, be extracted mixture; Tea grounds in the described extraction mixture obtained is removed, and keeps temperature 40 ~ 60 DEG C, under pressure-0.08 ~ 1.2MPa, described dme subcritical fluids is gasified, can tea leaf extract be obtained.The method of the subcritical fluid extraction tea leaf extract of this invention, temperature required and pressure is low in leaching process, can ensure that in tealeaves, biologically active substance is not destroyed, and equipment cost is lower; The tea grounds water content obtained after extraction is low, and has good recycle value, can be widely used in the preparation field of tea extract.Chinese patent literature 95112535.4 discloses a kind of Oleum Pelargonii Graveolentis and manufacture method thereof.The method adopts high temperature (120 DEG C) water extraction, and technique is coarse, not only product can be caused to run off but also be unfavorable for the character of maintenance product.
Summary of the invention
The present invention is to overcome the deficiencies in the prior art, improves extraction efficiency, provides a kind of method of the method extracting Oleum Pelargonii Graveolentis from spiceleaf-subcritical normal butane fluid extraction Oleum Pelargonii Graveolentis newly.
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) first the spiceleaf cleaned up is dried to Han Shui Liang≤7wt%, is crushed to 40 ~ 60 orders, then load in 200 ~ 300 order pockets of 2 ~ 3L;
2) start heat recirculated water system, preheating extractor 55 ~ 60 DEG C, by step 1) described in spiceleaf is housed pocket put in extractor, airtight, to be evacuated to vacuum tightness be 0.05 ~ 0.1MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent;
4) start heat recirculated water system, extract;
5) be then separated with vacuum pump interlock reduction vaporization with membrane compressor in separating tank;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, through molecular distillation, obtain final Oleum Pelargonii Graveolentis product.Preferably, step 1 described in 2) middle spiceleaf drying mode is 50 ~ 60 DEG C of oven dry 2 ~ 3 hours, or natural air drying.
Preferably, described step 2) in add soybean oil, soybean oil is put in extractor together with the pocket that spiceleaf is housed.
Preferably, described step 2) in the weight ratio of soybean oil and spiceleaf be 1 ~ 28:100.
Preferably, described step 2) in the weight ratio of soybean oil and spiceleaf be 6 ~ 8:100.
Preferably, in add the liquid material of normal butane and described spiceleaf volume ratio be 1 ~ 2:1, flood spiceleaf pocket.
Preferably, described step 4) middle extracting pressure 0.5 ~ 0.7MPa, extraction temperature 55 ~ 60 DEG C, extracts 3 ~ 4 times, and the time of each extraction is 50 ~ 60 minutes.
Preferably, described step 5) in separation temperature be 60 ~ 65 DEG C, first vacuumize with membrane compressor and make pressure reach-0.01 ~-0.02Mpa, then open vacuum pump evacuation to 0.05 ~ 0.1MPa, each disengaging time is 35 ~ 40 minutes.
Preferably, described step 6) temperature of Middle molecule distillation is 80 ~ 85 DEG C, vacuum tightness is 0.05 ~ 0.08MPa.
The described pocket that spiceleaf is housed is nylon in lightweight material, and weight can be ignored.
The volume of extractor described in device is 160L, step 3) in import 50 ~ 66V% that the amount of normal butane is extractor volume.
The product purity of the Oleum Pelargonii Graveolentis that the present invention obtains is higher, and its characterization data is as following table:
Table 1 Oleum Pelargonii Graveolentis makings is analyzed
By GC-MS technology, we are divided into from identifying 46 peaks, determine its chemical structural formula and relative content, and these compositions are terpene and containing oxygen derivative thereof, comprising monoterpenes, and monoterpene containing oxygen derivative, sesquiterpene, sesquialter anvil containing oxygen derivative.As can be seen from relative content, this volatilization main body of oil is Terpane, terpinyl acetate, Terpineol 350, alpha-Terpineol 350.
Beneficial effect of the present invention:
The present invention selects normal butane fluid to adopt the subcritical processing method extracting Oleum Pelargonii Graveolentis from spiceleaf as extraction solvent first, the boiling point of normal butane is-0.5 DEG C, be gaseous state at normal temperatures and pressures, be liquid after pressurization, water insoluble, there is good solvent properties, and the feature such as lower emergent pressure and higher critical temperature.Easily realize control of industrialization, extracting and developing is effective.
Use the inventive method extraction Oleum Pelargonii Graveolentis, yield reaches 7.1%, and being 7 ~ 14 times of vapour method, is supercritical CO
22.3 ~ 3.5 times of flow process, and extraction component is comparatively complete, and rate of extraction is fast, and extraction agent recycle efficiency is high, environmentally safe.Through experimental verification, under above processing condition, the yield of Oleum Pelargonii Graveolentis is 7.1%, and outward appearance is blackish green, in paste.
In order to improve the state of the Oleum Pelargonii Graveolentis of subcritical normal butane extraction further, dilute Oleum Pelargonii Graveolentis in extraction process, the state both having optimized Oleum Pelargonii Graveolentis turn improves productive rate.
The method utilizes at different temperatures and pressures exactly, and normal butane fluid is comparatively large to the dissolubility difference of Oleum Pelargonii Graveolentis, realizes the Extraction and separation to Oleum Pelargonii Graveolentis.
The method extraction efficiency is high, equipment manufacturing cost is low, feed throughput is large, technical process is simple, production cost is low, no solvent residue, whole process is carried out under low temperature, anaerobic state, extraction, separation are carried out simultaneously, and extraction rate is fast, can realize the recycle and reuse of solvent.
Accompanying drawing explanation
Fig. 1 is subcritical abstraction device of the present invention;
Fig. 2 is that the GC-MS of Oleum Pelargonii Graveolentis analyzes collection of illustrative plates.
Embodiment
Subcritical abstraction device mainly comprises 2 extractors, 1 separating tank, 2 solvent storage tanks, also has compressor, condenser and water circulation system.With specific embodiment, content of the present invention is described below.
Embodiment 1:
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) first by little of water content≤7wt% for spiceleaf 55 ± 5 DEG C oven dry 2 ~ 3 cleaned up, be crushed to 40 ~ 60 orders, then loading volume is in the 300 order pockets of 3L, is weighed as 50.30 kilograms;
2) by step 1) described in spiceleaf is housed pocket put in extractor, airtight, and heated extractor extraction by water circulation system, when temperature to be heated reaches 55 DEG C, being evacuated to vacuum tightness is 0.1MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent, the liquid material volume ratio adding normal butane and spiceleaf is 1:1, and solvent floods pocket;
4) start heat recirculated water system, be warming up to 55 DEG C and extract, extracting pressure 0.1MPa, the time of each extraction is 50 minutes, extracts 3 times;
5) then in separating tank, reduction vaporization is separated, repeated isolation 3 times, and separation temperature is 60 DEG C, first vacuumizes and makes pressure reach-0.01MPa, then open vacuum pump evacuation to 0.1MPa with membrane compressor, each disengaging time 35 minutes;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, keep temperature 80 DEG C, vacuum tightness is 0.05MPa molecular distillation, finally obtain outward appearance blackish green, in thickness paste Oleum Pelargonii Graveolentis 3.57 kilograms, yield is 7.10%.
The normal butane gas be evaporated from separating tank, after compressor compression, becomes liquid through condenser and enters solvent storage tank and continue to recycle.After having extracted, open extractor, take out pocket, pour out material slag.
Embodiment 2:
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) first by little of water content≤7wt% for spiceleaf 55 ± 5 DEG C oven dry 2 ~ 3 cleaned up, be crushed to 40 ~ 60 orders, then loading volume is in the 300 order pockets of 3L, is weighed as 50.50 kilograms;
2) by step 1) described in the pocket of spiceleaf is housed and 3.58 kilograms of soybean oil are put in extractor, airtight, and by water circulation system, extraction is heated extractor, when temperature to be heated reaches 60 DEG C, being evacuated to vacuum tightness is 0.5MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent, the liquid material volume ratio adding normal butane and spiceleaf is 2:1, and solvent floods pocket;
4) start heat recirculated water system, be warming up to 60 DEG C and extract, extracting pressure 0.7MPa, the time of each extraction is 60 minutes, extracts 4 times;
5) then in separating tank, reduction vaporization is separated, repeated isolation 4 times, and separation temperature is 65 DEG C, takes out negative pressure to-0.05MPa, then open vacuum pump evacuation to 0.2MPa, each disengaging time 40 minutes with membrane compressor and vacuum pump interlock;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, keep temperature 85 DEG C, vacuum tightness is 0.08MPa molecular distillation, finally obtain outward appearance blackish green, in thickness paste Oleum Pelargonii Graveolentis 3.65 kilograms, yield is 7.29%.
The normal butane gas be evaporated from separating tank, after compressor compression, becomes liquid through condenser and enters solvent storage tank and continue to recycle.After having extracted, open extractor, take out pocket, pour out material slag.
Embodiment 3:
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) be first crushed to 40 ~ 60 orders by little for the spiceleaf 55 ± 5 DEG C cleaned up oven dry 2 ~ 3 up to water content≤7wt%, then loading volume is in the 300 order pockets of 3L, is weighed as 50.10 kilograms;
2) by step 1) described in the pocket of spiceleaf is housed and the soybean oil of 14.43 kilograms is put in extractor, airtight, and by water circulation system, extraction is heated extractor, when temperature to be heated reaches 56 DEG C, being evacuated to vacuum tightness is 0.25MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent, the liquid material volume ratio adding normal butane and spiceleaf is 1.5:1, and solvent floods pocket;
4) start heat recirculated water system, be warming up to 56 DEG C and extract, extracting pressure 0.6MPa, the time of each extraction is 50 minutes, extracts 3 times;
5) then in separating tank, reduction vaporization is separated, repeated isolation 3 times, and separation temperature is 62 DEG C, first vacuumizes and makes pressure reach-0.02Mpa, then open vacuum pump evacuation to 0.1MPa with membrane compressor, each disengaging time 35 minutes;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, keep temperature 81 DEG C, vacuum tightness is 0.06MPa molecular distillation, finally obtain outward appearance blackish green, in thickness paste Oleum Pelargonii Graveolentis 3.61 kilograms, yield is 7.20%.
The normal butane gas be evaporated from separating tank, after compressor compression, becomes liquid through condenser and enters solvent storage tank and continue to recycle.After having extracted, open extractor, take out pocket, pour out material slag.
Embodiment 4:
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) be first crushed to 40 ~ 60 orders by little for the spiceleaf 55 ± 5 DEG C cleaned up oven dry 2 ~ 3 up to water content≤7wt%, then loading volume is in the 300 order pockets of 3L, is weighed as 50.20 kilograms;
2) by step 1) described in the pocket of spiceleaf is housed and 3.55 kilograms of soybean oil are put in extractor, airtight, and by water circulation system, extraction is heated extractor, when temperature to be heated reaches 58 DEG C, being evacuated to vacuum tightness is 0.2MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent, the volume ratio adding the liquid material of normal butane and spiceleaf is 1.2:1, and solvent floods pocket;
4) start heat recirculated water system, be warming up to 57 DEG C and extract, extracting pressure 0.55MPa, the time of each extraction is 53 minutes, extracts 4 times;
5) then in separating tank, reduction vaporization is separated, repeated isolation 4 times, and separation temperature is 62 DEG C, first vacuumizes and makes pressure reach-0.02Mpa, then open vacuum pump evacuation to 0.2MPa with membrane compressor, each disengaging time 36 minutes;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, keep temperature 81 DEG C, vacuum tightness is 0.06MPa molecular distillation, finally obtain outward appearance blackish green, in thickness paste Oleum Pelargonii Graveolentis 3.57 kilograms, yield is 7.10%.
The normal butane gas be evaporated from separating tank, after compressor compression, becomes liquid through condenser and enters solvent storage tank and continue to recycle.After having extracted, open extractor, take out pocket, pour out material slag.
Embodiment 5:
Subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, comprises the steps:
1) be first crushed to 40 ~ 60 orders by little for the spiceleaf 55 ± 5 DEG C cleaned up oven dry 2 ~ 3 up to water content≤7wt%, then loading volume is in the 300 order pockets of 3L, is weighed as 50.10 kilograms;
2) by step 1) described in the pocket of spiceleaf is housed and 3.68 kilograms of soybean oil are put in extractor, airtight, and by water circulation system, extraction is heated extractor, when temperature to be heated reaches 59 DEG C, being evacuated to vacuum tightness is 0.3MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent, the volume ratio adding the liquid material of normal butane and spiceleaf is 1.3:1, and solvent floods pocket;
4) start heat recirculated water system, be warming up to 57 DEG C and extract, extracting pressure 0.65MPa, the time of each extraction is 53 minutes, extracts 3 times;
5) then in separating tank, reduction vaporization is separated, repeated isolation 3 times, and separation temperature is 64 DEG C, first vacuumizes and makes pressure reach-0.03Mpa, then open vacuum pump evacuation to 0.3MPa with membrane compressor, each disengaging time 37 minutes;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, keep temperature 80 ~ 85 DEG C, vacuum tightness is 0.07MPa molecular distillation, finally obtain outward appearance blackish green, in thickness paste Oleum Pelargonii Graveolentis 3.57 kilograms, yield is 7.10%.
The normal butane gas be evaporated from separating tank, after compressor compression, becomes liquid through condenser and enters solvent storage tank and continue to recycle.After having extracted, open extractor, take out pocket, pour out material slag.What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, other amendments that those of ordinary skill in the art make technical scheme of the present invention or equivalently to replace, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of right of the present invention.
Claims (9)
1. subcritical normal butane fluid extracts a method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, comprises the steps:
1) first the spiceleaf cleaned up is dried to Han Shui Liang≤7wt%, is crushed to 40 ~ 60 orders, then loading volume is in 200 ~ 300 order pockets of 2 ~ 3L;
2) start heat recirculated water system, preheating extractor 55 ~ 60 DEG C, by step 1) described in spiceleaf is housed pocket put in extractor, airtight, to be evacuated to vacuum tightness be 0.05 ~ 0.1MPa, discharges air in extractor;
3) ram pump is used toward step 2) described extractor interior importing n-butane solvent;
4) start heat recirculated water system, extract;
5) be then separated with vacuum pump interlock reduction vaporization with membrane compressor in separating tank;
6) combining step 5) Oleum Pelargonii Graveolentis that obtains, through molecular distillation, obtain final Oleum Pelargonii Graveolentis product.
2. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 1) middle spiceleaf drying mode is 50 ~ 60 DEG C of oven dry 2 ~ 3 hours, or natural air drying.
3. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 2) in add soybean oil, soybean oil is put in extractor together with the pocket that spiceleaf is housed.
4. a kind of subcritical normal butane fluid as claimed in claim 3 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 2) in the weight ratio of soybean oil and spiceleaf be 1 ~ 28:100.
5. a kind of subcritical normal butane fluid as claimed in claim 4 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 2) in the weight ratio of soybean oil and spiceleaf be 6 ~ 8:100.
6. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 3) in add the liquid material of normal butane and described spiceleaf volume ratio be 1 ~ 2:1, flood spiceleaf pocket.
7. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 4) middle extracting pressure 0.5 ~ 0.7MPa, extraction temperature 55 ~ 60 DEG C, extract 3 ~ 4 times, the time of each extraction is 50 ~ 60 minutes.
8. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 5) in separation temperature be 60 ~ 65 DEG C, first vacuumizing with membrane compressor makes pressure reach-0.01 ~-0.02Mpa, open vacuum pump evacuation to 0.05 ~ 0.1MPa again, each disengaging time is 35 ~ 40 minutes.
9. a kind of subcritical normal butane fluid as claimed in claim 1 extracts the method for Oleum Pelargonii Graveolentis from spiceleaf, it is characterized in that, described step 6) Middle molecule distillation temperature be 80 ~ 85 DEG C, vacuum tightness is 0.05 ~ 0.08MPa.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903227A (en) * | 2016-06-22 | 2016-08-31 | 伊犁天药生物科技有限公司 | Lavender absolute oil and preparation method thereof |
| CN106176849A (en) * | 2016-07-08 | 2016-12-07 | 禹州市合同泰药业有限公司 | A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae |
| CN106433989A (en) * | 2016-11-12 | 2017-02-22 | 郑州雪麦龙食品香料有限公司 | Method for extracting pimento berry oil through subcritical normal butane fluid |
| CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
| CN108424816A (en) * | 2018-05-30 | 2018-08-21 | 郑州雪麦龙食品香料有限公司 | A kind of extraction process of thyme essential oil |
| CN108559635A (en) * | 2018-05-30 | 2018-09-21 | 郑州雪麦龙食品香料有限公司 | A kind of extraction process of perilla herb oil |
| CN108707511A (en) * | 2018-05-30 | 2018-10-26 | 郑州雪麦龙食品香料有限公司 | A kind of extraction process of citronella oil |
| CN108753464A (en) * | 2018-06-20 | 2018-11-06 | 江西思派思香料化工有限公司 | It is a kind of transfer and extracting natural perfume method and device |
| CN112457920A (en) * | 2020-12-01 | 2021-03-09 | 江西一森正气生物科技有限公司 | Extraction processing system of essential oil |
| CN114561246A (en) * | 2022-02-18 | 2022-05-31 | 东莞市农业科学研究中心 | Preparation method and bacteriostatic application of camphor tree essential oil |
| CN116240070A (en) * | 2022-05-04 | 2023-06-09 | 新纪元食品科技(佛山)有限公司 | Process for leaching grease |
-
2015
- 2015-11-24 CN CN201510821381.4A patent/CN105505583B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 宋国辉等: "加压液化气亚临界萃取技术在农产品加工中的应用", 《农产品加工（学刊）》 * |
| 常进文等: "用亚临界四号溶剂和分子蒸馏技术提取苦水玫瑰挥发油", 《香料香精化妆品》 * |
| 杨靖等: "月桂叶精油的3种制备方法比较及应用", 《烟草科技》 * |
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| CN105903227B (en) * | 2016-06-22 | 2018-04-10 | 伊犁天药生物科技有限公司 | lavender absolute oil and preparation method thereof |
| CN105903227A (en) * | 2016-06-22 | 2016-08-31 | 伊犁天药生物科技有限公司 | Lavender absolute oil and preparation method thereof |
| CN106176849A (en) * | 2016-07-08 | 2016-12-07 | 禹州市合同泰药业有限公司 | A kind of subcritical fluid techniques extracts the method for Yu's Essential Oil of Radix Angelicae Dahuricae |
| CN106433989B (en) * | 2016-11-12 | 2019-11-12 | 郑州雪麦龙食品香料有限公司 | A kind of method of many fragrant fruit oil of subcritical normal butane fluid extraction |
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