CN105132184B - A kind of method of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil - Google Patents
A kind of method of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil Download PDFInfo
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- CN105132184B CN105132184B CN201510585007.9A CN201510585007A CN105132184B CN 105132184 B CN105132184 B CN 105132184B CN 201510585007 A CN201510585007 A CN 201510585007A CN 105132184 B CN105132184 B CN 105132184B
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Abstract
The present invention relates to a kind of methods of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil.Using gardenia as raw material, by following steps: (1) dry in the shade crushing for mast fresh flower or brine fermentation pre-processes；(2) gardenia is obtained to pretreatment and carries out subcritical abstraction, obtain gardenia flower oil；(3) ethyl alcohol is added in gardenia flower oil or acetone carries out dewaxing treatment；(4) gardenia flower oil after dewaxing treatment is subjected to short-range molecular distillation, obtains cape jasmine flower essential oil.Present invention process route is simple, and yield is high, superior product quality, is suitble to expanding production.
Description
Technical field
The invention belongs to plant extract essential oil field, it is related to a kind of subcritical abstraction and molecular distillation coupling preparation gardenia
The preparation process of essential oil belongs to natural extract field.
Technical background
Cape jasmine (Gardenia jasminoides Ellis) is Rubiaceae Gardenia Ellis, is a kind of small-sized evergreen shrubs.Cape jasmine
Son is born in hill, adaptable, is distributed mainly on subtropical and tropical zones.Gardenia is Rubiaceae Gardenia Ellis Xianghualing area,
Cultivation adaptability is strong, and grey color gives off a strong fragrance, and is famous one of the eight big fragrant flowers in China.Gardenia is a kind of rare natural
Fragrance, contained by effective component gardenia essential oil as high-grade fragrance applications in various products, have clearing heat-fire, treatment
Pyreticosis, ease off the pressure, moisturizing skin the benefits of.It was found that the main component of cape jasmine flowers volatile oil is linalool, in jasmine
Ester, farnesene, β-myrcene, methyl benzoate, ocimenum etc..
The existing method for extracting gardenia essential oil is to extract fresh gardenia with petroleum ether gardenia concrete is made, and is added
3~6 times of ethyl alcohol, cold filtration remove insoluble wax, are then cooled to -15~25 DEG C, refilter paraffin removal, ethanol solution
Remove ethyl alcohol through vacuum distillation to get essential oil liquid is arrived, the shortcomings that yield is usually 0.05~0.06%, this method be fragrance compared with
Difference, color is deeper, and yield is lower, and remaining organic solution can generate adverse effect to human body.Plants essential oil is fragrance work
The important source material and export material of industry, with the fast development of spices and essence industry, research cape jasmine flower essential oil has increasingly heavier
The realistic meaning wanted.This patent, which is coupled using subcritical abstraction with molecular distillation, prepares cape jasmine flower essential oil, this method simple process,
Easy to operate, essential oil yield is high, easy industrialized production.
Summary of the invention
It is an object of the invention to overcome the shortcomings of that cape jasmine flower essential oil in industrialized production, provides a kind of subcritical abstraction
The preparation method of preparation cape jasmine flower essential oil is coupled with molecular distillation.
To achieve the above object, the present invention adopts the following technical scheme:
1. a kind of method of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil, it is characterised in that by following step
Rapid composition:
First step pretreatment
Cape jasmine fresh flower after removal of impurities, is crushed, obtains extraction feed by a；
B crushes cape jasmine fresh flower, 15%~20% saline immersion of mass volume ratio 1: 5~10 is added, at normal temperature
2~7d of spontaneous fermentation, extruding are filtered to remove salt water, obtain extraction feed；
Second step subcritical abstraction
By the resulting extraction feed of the first step a or b, it is put into extraction kettle, by liquid solvent injection extraction kettle and mast fresh flower
The mass volume ratio of raw material mixing, liquid solvent and raw material is 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, extraction pressure
It is extracted under conditions of 0.6~0.8Mpa of power 2~3 times, 0.5~1.0h, after extraction, will carry the liquid of gardenia flower oil every time
It in state solvent delivery to separating still, is then evaporated under reduced pressure, liquid solvent is made sufficiently to gasify, temperature 30 is controlled in evaporation process
~50 DEG C, after equal solvent recycling completely, extracted thick gardenia flower oil is released from separating still bottom, yield is 1.05~
1.72%；
Third step dewaxing
By the resulting thick gardenia flower oil of second step, mass volume ratio is added and is sunk for 1: 5~1: 20 ethyl alcohol or acetone
Drop processing, is centrifuged 10~20min at 5000~10000rpm/min, removes precipitating, and filtrate is dried under reduced pressure at 30 DEG C, obtains
The gardenia flower oil of purification, yield are 68~82%；
4th step molecular distillation
The gardenia flower oil of purification is subjected to short-range molecular distillation, 50~120 DEG C of vapo(u)rizing temperature, 40~80mbar of vacuum degree,
0.5~1.5ml/ml of flow, 60~300r/min of knifing rotating speed, cooling temperature -10~0 DEG C, light component are cape jasmine flower essential oil,
Yield is 58.2~64.7%.
2. the liquid solvent in second step is selected from one or more of propane, butane, iso-butane, dimethyl ether and ether.
Beneficial effects of the present invention:
A kind of subcritical abstraction provided by the present invention and molecular distillation coupling preparation cape jasmine flower essential oil method, also have with
Lower feature:
(1) present invention process route is short, and to raw material using sufficiently, products application is extensive；
(2) recovery rate is high, no solvent residue, is suitble to large-scale production.
Specific embodiment
Following embodiment is some citings of the invention, should not be seen as limitation of the invention.
Embodiment 1
By cape jasmine fresh flower by removal of impurities after, crush, obtain extraction feed, be put into extraction kettle, by propane injection extraction kettle with
The mass volume ratio of the mixing of mast fresh flower raw material, propane and raw material is 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, extraction
It is extracted under conditions of 0.6~0.8Mpa of pressure power 2~3 times, 0.5~1.0h, after extraction, will carry gardenia flower oil every time
Delivery of propane to separating still in, be then evaporated under reduced pressure, propane made sufficiently to gasify, in evaporation process control temperature 30~50
DEG C, etc. propane recoveries it is complete after, release extracted thick gardenia flower oil from separating still bottom, yield is 1.05~1.72%；Institute
The thick gardenia flower oil obtained is added the ethyl alcohol that mass volume ratio is 1: 5~1: 20 and carries out settlement treatment, in 5000~10000rpm/
It is centrifuged 10~20min under min, removes precipitating, filtrate is dried under reduced pressure at 30 DEG C, the gardenia flower oil refined, yield 68
~82%；The gardenia flower oil of purification is subjected to short-range molecular distillation, 50~120 DEG C of vapo(u)rizing temperature, 40~80mbar of vacuum degree, stream
0.5~1.5ml/ml, 60~300r/min of knifing rotating speed are measured, cooling temperature -10~0 DEG C, light component is cape jasmine flower essential oil, is received
Rate is 58.2~64.7%.
Embodiment 2
It by cape jasmine fresh flower, crushes, 15%~20% saline immersion of mass volume ratio 1: 5~10 is added, at normal temperature certainly
So 2~7d of fermentation, extruding are filtered to remove salt water, are put into extraction kettle, butane injection extraction kettle are mixed with mast fresh flower raw material, fourth
The mass volume ratio of alkane and raw material is 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, 0.6~0.8Mpa's of extracting pressure
Under the conditions of extract 2~3 times, 0.5~1.0h, after extraction, is transported to separating still for the butane for carrying gardenia flower oil every time
It is interior, be then evaporated under reduced pressure, butane made sufficiently to gasify, in evaporation process control 30~50 DEG C of temperature, etc. butane recoveries it is complete
Afterwards, extracted thick gardenia flower oil is released from separating still bottom, yield is 1.05~1.72%；Resulting thick gardenia flower oil, adds
Enter mass volume ratio be 1: 5~1: 20 acetone carry out settlement treatment, at 5000~10000rpm/min be centrifuged 10~
20min removes precipitating, and filtrate is dried under reduced pressure at 30 DEG C, the gardenia flower oil refined, and yield is 68~82%；It will purification
Gardenia flower oil carry out short-range molecular distillation, 50~120 DEG C of vapo(u)rizing temperature, 40~80mbar of vacuum degree, 0.5~1.5ml/ of flow
Ml, 60~300r/min of knifing rotating speed, cooling temperature -10~0 DEG C, light component are cape jasmine flower essential oil, and yield is 58.2~
64.7%.
Embodiment 3
It by cape jasmine fresh flower after removal of impurities, crushes, is put into extraction kettle, by iso-butane injection extraction kettle and mast fresh flower raw material
Mixing, the mass volume ratio of iso-butane and raw material are 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, extracting pressure 0.6
It is extracted under conditions of~0.8Mpa 2~3 times, 0.5~1.0h, after extraction, will carry the iso-butane of gardenia flower oil every time
It is transported in separating still, is then evaporated under reduced pressure, iso-butane is made sufficiently to gasify, 30~50 DEG C of temperature are controlled in evaporation process,
After equal iso-butanes recycling completely, extracted thick gardenia flower oil is released from separating still bottom, yield is 1.05~1.72%；Gained
Thick gardenia flower oil, be added mass volume ratio be 1: 5~1: 20 ethyl alcohol carry out settlement treatment, in 5000~10000rpm/min
10~20min of lower centrifugation removes precipitating, and filtrate is dried under reduced pressure at 30 DEG C, the gardenia flower oil refined, and yield is 68~
82%；The gardenia flower oil of purification carries out short-range molecular distillation, 50~120 DEG C of vapo(u)rizing temperature, 40~80mbar of vacuum degree, flow
0.5~1.5ml/ml, 60~300r/min of knifing rotating speed, cooling temperature -10~0 DEG C, light component are cape jasmine flower essential oil, yield
It is 58.2~64.7%.
Embodiment 4
It by cape jasmine fresh flower, crushes, 15%~20% saline immersion of mass volume ratio 1: 5~10 is added, at normal temperature certainly
So 2~7d of fermentation, extruding are filtered to remove salt water, obtain extraction feed, be put into extraction kettle, by dimethyl ether injection extraction kettle and mast
The mass volume ratio of the mixing of fresh flower raw material, dimethyl ether and raw material is 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, extraction
It is extracted under conditions of 0.6~0.8Mpa of pressure 2~3 times, 0.5~1.0h, after extraction, will carry gardenia flower oil every time
Dimethyl ether is transported in separating still, is then evaporated under reduced pressure, and dimethyl ether is made sufficiently to gasify, in evaporation process control temperature 30~
50 DEG C, after waiting dimethyl ether recycling completely, extracted thick gardenia flower oil is released from separating still bottom, yield is 1.05~
1.72%；Resulting thick gardenia flower oil is added the acetone that mass volume ratio is 1: 5~1: 20 and carries out settlement treatment, 5000~
It is centrifuged 10~20min under 10000rpm/min, removes precipitating, filtrate is dried under reduced pressure at 30 DEG C, the gardenia flower oil refined,
Yield is 68~82%；The gardenia flower oil progress short-range molecular distillation of purification, 50~120 DEG C of vapo(u)rizing temperature, vacuum degree 40~
80mbar, 0.5~1.5ml/ml of flow, 60~300r/min of knifing rotating speed, cooling temperature -10~0 DEG C, light component are cape jasmine
Flower essential oil, yield are 58.2~64.7%.
Embodiment 5
It by cape jasmine fresh flower after removal of impurities, crushes, is put into extraction kettle, ether injection extraction kettle is mixed with mast fresh flower raw material
It closing, the mass volume ratio of ether and raw material is 1: 5~1: 8 (g: mL), at 30~50 DEG C of extraction temperature, extracting pressure 0.6~
It is extracted under conditions of 0.8Mpa 2~3 times, 0.5~1.0h, after extraction, the ether for carrying gardenia flower oil is conveyed every time
It into separating still, is then evaporated under reduced pressure, ether is made sufficiently to gasify, 30~50 DEG C of temperature are controlled in evaporation process, waits ether
After recycling completely, extracted thick gardenia flower oil is released from separating still bottom, yield is 1.05~1.72%；Resulting thick cape jasmine
Caul-fat is added the ethyl alcohol that mass volume ratio is 1: 5~1: 20 and carries out settlement treatment, is centrifuged 10 at 5000~10000rpm/min
~20min removes precipitating, and filtrate is dried under reduced pressure at 30 DEG C, the gardenia flower oil refined, and yield is 68~82%；Purification
Gardenia flower oil carry out short-range molecular distillation, 50~120 DEG C of vapo(u)rizing temperature, 40~80mbar of vacuum degree, 0.5~1.5ml/ of flow
Ml, 60~300r/min of knifing rotating speed, cooling temperature -10~0 DEG C, light component are cape jasmine flower essential oil, and yield is 58.2~
64.7%.
Claims (1)
1. a kind of method of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil, it is characterised in that by following steps group
At:
First step pretreatment
Cape jasmine fresh flower after removal of impurities, is crushed, obtains extraction feed by a；
B crushes cape jasmine fresh flower, 15%~20% saline immersion of mass volume ratio 1:5 ~ 10 is added, at normal temperature spontaneous fermentation 2
~ 7d, extruding are filtered to remove salt water, obtain extraction feed；
Second step subcritical abstraction
By the resulting extraction feed of the first step a or b, it is put into extraction kettle, it will be in propane, butane, iso-butane, dimethyl ether and ether
A kind of solvent injection extraction kettle mixed with mast fresh flower raw material, the mass volume ratio g:mL of raw material and liquid solvent is 1:5 ~ 1:
8, it is extracted under conditions of 30 ~ 50 DEG C of extraction temperature, 0.6 ~ 0.8Mpa of extracting pressure 2~3 times, 0.5 ~ 1.0h, extraction are tied every time
Then Shu Hou is evaporated under reduced pressure in the solvent delivery to separating still for carrying gardenia flower oil, solvent is made sufficiently to gasify, steam
30~50 DEG C of temperature of control during hair after equal solvent recycling completely, releases extracted thick gardenia flower oil from separating still bottom,
Yield is 1.05~1.72%；
Third step dewaxing
By the resulting thick gardenia flower oil of second step, mass volume ratio is added and is carried out at sedimentation for the ethyl alcohol or acetone of 1:5 ~ 1:20
Reason is centrifuged 10~20min at 5000~10000 rpm, removes precipitating, and filtrate is dried under reduced pressure at 30 DEG C, is refined
Gardenia flower oil, yield are 68 ~ 82%；
4th step molecular distillation
The gardenia flower oil of purification is subjected to short-range molecular distillation, 50 ~ 120 DEG C of vapo(u)rizing temperature, 40 ~ 80 mbar of vacuum degree, flow
0.5~1.5ml/ml, 60 ~ 300 r/min of knifing rotating speed, cooling temperature -10 ~ 0 DEG C, light component are cape jasmine flower essential oil, yield
It is 58.2~64.7%.
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