CN110373270A - A kind of method that additive and extraction essential oil are used in plants essential oil extraction - Google Patents
A kind of method that additive and extraction essential oil are used in plants essential oil extraction Download PDFInfo
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- CN110373270A CN110373270A CN201910640009.1A CN201910640009A CN110373270A CN 110373270 A CN110373270 A CN 110373270A CN 201910640009 A CN201910640009 A CN 201910640009A CN 110373270 A CN110373270 A CN 110373270A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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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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Abstract
The present invention provides a kind of plants essential oil extraction additives, are fatty alcohol polyoxypropylene ether type compound R (CH2CH2CH2O)nH, wherein group R is containing C6‑12Fatty alcohol radical, the value of polymerization degree n is 5~10.The present invention also provides a kind of method of extraction essential oil, this method mainly utilizes supercritical carbon dioxide extracting and above-mentioned additive is added extracts plants essential oil from plant material.The present invention can be realized using above-mentioned additive and more efficiently be extracted to the aroma substance of natural plant raw material, effectively improve the extraction efficiency of plants essential oil, and the additional amount of above-mentioned additive is relatively low, without removing additive after supercritical carbon dioxide extracting, the higher plants essential oil of quality can be directly obtained, the loss of aroma substance caused by can be avoided because of removing additive.
Description
Technical field
The invention belongs to flavors and fragrances preparation fields, and in particular to a kind of plants essential oil extraction additive and extraction plant
The method of essential oil.
Background technique
Plants essential oil be it is a kind of exist and the leaf of fragrant plant, root, skin, flower and fruit in, can be with steam distillation, and have
The volatility oily liquids of certain smell.Currently, the method for obtaining plants essential oil mainly has extrusion, steam distillation, has
Solvent extraction method etc..Extrusion, extraction by steam distillation efficiency are lower, and organic solvent extraction not only needs largely to have
Solvent, environment easy to pollute, and the operations such as freezing dewaxing, distillation, complex process are generally required in last handling process.In recent years
Come, supercritical carbon dioxide extraction method shows good growth momentum in terms of essential oil preparation, it is using overcritical
The characteristics of high osmosis of carbon dioxide under state, mobility, low sticky and nontoxic, tasteless, no solvent residue, is to raw material
A kind of method extracted, studies have shown that supercritical carbon dioxide extracting can be protected preferably with conventional solvent extraction phase ratio
The odor characteristic for holding raw material is that one kind of production high-quality natural perfume material is effective suitable for thermal sensitivity, volatile perfume molecules
Means.For example, Du Lijun etc. be published in analysis test journal, 2019,38 (1), it is entitled " steam distillation with it is overcritical
CO2It is recorded in the paper of extraction combination gas chromatography-mass spectrometry analysis pepper another name for oil component " and uses supercritical CO2Method is to essential oil
Natural component destroy it is less, remain a large amount of active constituent, and essential oil acquisition amount is higher.
Although supercritical carbon dioxide has the advantages that all various aspects, carbon dioxide is a low polar solvent always,
Solvability is poor, and the fragrance component higher for polarity in plant (alcohols, ketone, acids etc.) extraction efficiency is lower.Have
Report is added in supercritical carbon dioxide using ethyl alcohol, methanol as entrainer, can be improved the extraction effect of supercritical carbon dioxide
(Fang Yanxiong, Lyu Qianjiang, Zhang Yongcheng, et al. supercritical carbon dioxide extraction isolation technics [J] are finely and customizations for rate
Product, 2002,10 (6): 17-19.；Song Ruoyuan, once Jun was magnificent, Wu Huachang, et al. supercritical carbon dioxide extracting onion Beijing opera
Ketone technical study [J] processing of farm products, 2018,465 (19): 39-41.).But the additional amount of above-mentioned entrainer often compared with
Greatly, while extracting aroma component, the dissolution of the macromoleculars such as protein, polysaccharide is also resulted in, although improving to a certain extent
Extraction efficiency, but need to post-process further to remove macromolecular substances therein, while during removing entrainer,
Long-time heating will cause the loss of volatile, oxidizable fragrance matter again, and product sensory style and features is caused not protrude.
Summary of the invention
In view of this, the present invention is it is necessory to provide the side of a kind of plants essential oil extraction additive and extraction essential oil
Method, to solve the above problems.
For this purpose, technical solution provided by the invention are as follows: a kind of plants essential oil extraction additive, is fatty alcohol polyoxypropylene
Ether type compound R (CH2CH2CH2O)nH, wherein group R is containing C6-12Fatty alcohol radical, the value of polymerization degree n is 5~10.This
" C in text6-12" represent and contain 6~12 carbon atoms, the value of the degree of polymerization " n " is positive integer, can be 5,6,7,8,9 or 10.
Based on above-mentioned, the group R is containing C6-12Straight chain fatty alcohol radical or contain C6-12Branched fatty alcohol radical.That is, described
Additive can be straight-chain fatty alcohol base polyoxypropylene ether type compound or Branched fatty alcohol radical polyethenoxy ether type compound.
Based on above-mentioned, the group R is containing C6-12Alkane alcohol radical, contain C6-12Alkene alcohol radical or contain C6-12Alkynes alcohol
Base.That is, the additive can for alkane alcohol radical polyoxypropylene ether type compound, alkene alcohol radical polyethenoxy ether type compound or
Alkynes alcohol radical polyoxypropylene ether type compound.
Based on above-mentioned, the fatty alcohol polyoxypropylene ether type compound is linear paraffin alcohol radical polyethenoxy ether, structure letter
Formula is CH3(CH2)4-10CH2O(CH2CH2CH2O)5-10H。
Based on above-mentioned, the fatty alcohol polyoxypropylene ether type compound is branched paraffin alcohol radical polyethenoxy ether, structure letter
Formula is [CH3(CH2)m1][CH3(CH2)m2]CHCH2O(CH2CH2CH2O)5-10H, wherein the value of the sum of m1 and m2 is 2~8, and
M1 and m2 is 0 or positive integer.
Preferably, the fatty alcohol polyoxypropylene ether type compound can for five polyethenoxy ether of 2- methyl anyl alcohol, just oneself
Seven polyethenoxy ether of alcohol, ten polyoxyethylene ether of n-heptanol, six polyethenoxy ether of n-octyl alcohol, five polyethenoxy ether of 3- propyl octanol,
Five polyethenoxy ether of n-nonyl alcohol, seven polyethenoxy ether of positive undecyl alcohol, five polyethenoxy ether of 2- alkynyl lauryl alcohol, 2- ethyl butanol ten
Polyethenoxy ether, six polyethenoxy ether of 2- propyl hexanol, five polyethenoxy ether of 3- alkenyl octanol, six polyethenoxy ether of Decanol,
Six polyethenoxy ether of 2- methyl-decanol, nine polyethenoxy ether of 2- butyl enanthol, five polyethenoxy ether of n-heptanol or 2- methyl 11
Six polyethenoxy ether of alcohol etc..
The present invention also provides a kind of methods of extraction essential oil, comprising steps of above-mentioned addition is added into plant material
Agent and supercritical carbon dioxide solvent carry out plants essential oil extraction processing, wherein the additional amount of the additive is described super faces
The 0.02%~0.8% of boundary's carbon dioxide solvent quality.Wherein, the additional amount of the additive according to the actual situation, Ke Yiwei
The supercritical carbon dioxide solvent quality 0.02%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%,
0.6%, 0.7%, 0.8% etc..
Based on above-mentioned, the solid-liquid ratio of the plant material and the supercritical carbon dioxide solvent is 1:8~1:12g/mL.
Preferably, the solid-liquid ratio is 1:9~1:11g/mL.
Based on the method for above-mentioned extraction essential oil, the plant material and the additive are placed in extraction kettle, so
Afterwards under conditions of 45 DEG C~65 DEG C and 15~35MPa, injects 1~5h of the supercritical carbon dioxide solvent extraction and extracted
Liquid carries out separating-purifying processing to the extract liquor, the plants essential oil is made.Wherein it is possible to using static extracting method or move
State cycling extraction method obtains the extract liquor.Preferably, during obtaining the extract liquor, in above-mentioned temperature and pressure item
Under part, 2~4h is extracted with the flow velocity dynamic circulation of 20~30L/h and obtains the extract liquor.
Based on above-mentioned, described the step of carrying out separating-purifying processing to the extract liquor includes: that the extract liquor is introduced into
Cooling processing is carried out in first order separator, enters back into the separator of the second level and removes removing carbon dioxide, and the plants essential oil is made.
Specifically, the extract liquor enters in the first order separator, handles removing wherein low big of dissolubility by decrease temperature and pressure
Molecular substance enters back into the second level separator, and supercritical carbon dioxide solvent is discharged from outlet in gaseous form, finally
Obtain the plants essential oil.
Based on above-mentioned, the plant material from one of the root of fresh plant, stem, leaf, flower, fruit, pericarp or
It is arbitrarily combined.Wherein, according to actual needs, the plant material can pre-process into graininess, sheet or filiform.
Compared with prior art, due to additive fatty alcohol polyoxypropylene ether type compound R provided by the invention
(CH2CH2CH2O)nR group in H is containing C6-12Fatty alcohol radical, polarity is lower, has preferably with plants essential oil extraction solvent
Compatibility, such as butane, carbon dioxide；Polyoxypropylene ether group energy in the fatty alcohol polyoxypropylene ether type compound simultaneously
Enough increase the solvability of the extraction solvent, promotes the dissolution of highly polar component in plant material, it is therefore, described
Fatty alcohol polyoxypropylene ether type compound uses the additive of solvent as plants essential oil extraction, and plants essential oil extraction can be assisted to use
Solvent extraction plants essential oil improves the extraction efficiency of plants essential oil.The additive fatty alcohol polyoxypropylene ether class compound can
For use as the additive of the abstraction techniques such as supercritical extraction technique, subcritical abstraction technology, extracted for example, being used as subcritical butane
Additive, additive of supercritical carbon dioxide extraction method of technology etc..
The present invention also provides a kind of method of extraction essential oil, which mainly utilizes supercritical extraction technique,
Using carbon dioxide as extractant, and the additive fatty alcohol polyoxypropylene ether type compound is added and is extracted from plant material
Plants essential oil；Additive due to fatty alcohol polyoxypropylene ether type compound as carbon dioxide had both had with carbon dioxide preferably
Compatibility, and the solvability of carbon dioxide can be improved, promote the dissolution of highly polar essential oil component in plant material,
So the aroma substance progress that the method for the extraction essential oil provided by the invention can be realized to natural plant raw material is higher
Effect ground extracts, and effectively improves the extraction efficiency of plants essential oil.In addition, since the fatty alcohol polyoxypropylene ether type compound is at this
Invent the additional amount in the extracting method of the plants essential oil provided compare it is lower, using being not necessarily to after supercritical carbon dioxide extracting
The additive fatty alcohol polyoxypropylene ether type compound is removed, the higher plants essential oil of quality, and this method can be obtained
The loss of aroma substance caused by being also avoided that because of removing additive.Therefore, the plant of above method preparation provided by the present invention
Object essential oil full aroma is true to nature, can be used for the fields such as tobacco, daily use chemicals, food, medicine, agricultural.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be described in further detail.
Embodiment 1
It is five polyethenoxy ether of n-nonyl alcohol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extraction Rosa Damascana using above-mentioned additive, comprising: will be new after drying
Fresh rose lobe 100g is placed in supercritical extraction reactor, then be added 4.45g (i.e. additive amount be carbon dioxide quality 0.5%,
Under the experiment condition, the density of carbon dioxide is 890.92kg/m3) five polyethenoxy ether of n-nonyl alcohol, open carbon dioxide storage
Tank supplies valve injection supercritical carbon dioxide solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL), in 45 DEG C, pressure 30MPa, stream
Dynamic extraction 4h, obtains rose extract under conditions of fast 25L/h；The rose extract be introduced into first order separator into
The processing of row cooling decompression, removes the low macromolecular substances of dissolubility therein, handles using second level separator, therein super
Critical carbon dioxide solvent is discharged from outlet in gaseous form, obtains Rosa Damascana, yield 0.82%.
Reference examples 1
This reference examples 1 provide a kind of method for extracting Rosa Damascana, and the main distinction of this method and embodiment 1 is: this
Five polyethenoxy ether of n-nonyl alcohol is not added in reference examples 1, specifically, the method that this reference examples 1 provide includes: will be new after drying
Fresh rose lobe 100g, is transferred in supercritical extraction reactor, and the ethyl alcohol 100mL that volume fraction is 10% is then added, opens two
Carbonoxide storage tank supplies valve and injects supercritical carbon dioxide solvent 1000mL, in 45 DEG C, the item of pressure 30MPa, flow velocity 25L/h
Dynamic extraction 4h under part obtains rose extraction stoste；The rose extract, which is introduced into first order separator cool down, to be subtracted
Pressure processing, removes the low macromolecular substances of dissolubility therein, handles using second level separator, and carbon dioxide therein is molten
Agent is discharged in gaseous form；It is handled again through rotary evaporation and removes ethyl alcohol entrainer, obtain rose medicinal extract, yield 1.05%；
The ethyl alcohol that obtained rose medicinal extract volume fraction is 95% dewaxes 2 times in -10 DEG C of freezings to remove wax, depressurizes rotary evaporation
It goes out alcohol solvent, obtains Rosa Damascana 0.32g, yield 0.32%.
Rosa Damascana constituent analysis test
The embodiment 1 and the resulting Rosa Damascana of reference examples 1 for accurately weighing 300mg respectively, are dissolved with methylene chloride respectively
Afterwards, internal standard (phenethyl acetate) is added, constituent analysis is carried out to the two respectively by GC-MS, the results are shown in Table 1 for analysis.Its
In, the instrument condition which uses is as follows:
Chromatographic column: DB-5MS capillary column (30m × 0.25mm × 0.25 μm)；Injector temperature: 250 DEG C；Carrier gas: high-purity
Helium；Flow velocity 1.0mL/min；Sample volume: 1 μ L；Split ratio 10:1；Temperature programming: 60 DEG C of holding 1min, then with 5 DEG C/min's
Heating rate is heated to 260 DEG C, and keeps 5min.
Ionization mode: EI；Ion source temperature: 230 DEG C；Electron energy: 70eV；Level four bars temperature: 150 DEG C；Electron multiplication
Device voltage: 1.89kV；33~500amu of mass scan range；Scanning mode: full scan；Solvent delay: 7.0min.
1 Rosa Damascana constituent analysis table of table
Note: "-" expression is not detected
As can be seen from Table 1: under the conditions of same detection, using GC-MS method, in the Rosa Damascana that embodiment 1 obtains
It is capable of detecting when 31 kinds of components, and is capable of detecting when 28 kinds of components in the Rosa Damascana that reference examples 1 obtain；And embodiment 1
To the effective component of Rosa Damascana be apparently higher than the active constituent content of the Rosa Damascana that reference examples 1 obtain, therefore, and compare
The extracting method for the Rosa Damascana that example 1 provides is compared, and in the extracting method for the Rosa Damascana that embodiment 1 provides, joined addition
Five polyethenoxy ether of agent n-nonyl alcohol can extract more effective components from rose, to absolutely prove in embodiment 1
Five polyethenoxy ether of additive n-nonyl alcohol, which is added, can be improved supercritical carbon dioxide to the extraction efficiency of rose effective component.
Embodiment 2
The present embodiment provides a kind of plants essential oil extractions to be positive seven polyethenoxy ether of undecyl alcohol with additive.
The present embodiment provides a kind of methods of extraction Rosa Damascana using above-mentioned additive, comprising: will be new after drying
Fresh rose lobe 100g is placed in supercritical extraction reactor, then be added 5.36g (i.e. additive amount be carbon dioxide quality 0.7%,
Under the experiment condition, the density of carbon dioxide is 850.83kg/m3) seven polyethenoxy ether of positive undecyl alcohol, open carbon dioxide
Storage tank supplies valve injection supercritical carbon dioxide solvent 900mL (i.e. solid-liquid ratio 1:9g/mL), in 55 DEG C, pressure 30MPa, stream
Dynamic extraction 4h, obtains rose extract under conditions of fast 25L/h；The rose extract be introduced into first order separator into
The processing of row cooling decompression, removes the low macromolecular substances of dissolubility therein, handles using second level separator, therein super
Critical carbon dioxide solvent is discharged from outlet in gaseous form, obtains Rosa Damascana, yield 0.83%.
Embodiment 3
It is ten polyethenoxy ether of 2- ethyl butanol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extraction Rosa Damascana using above-mentioned additive, comprising: will be new after drying
Fresh rose lobe 100g is placed in supercritical extraction reactor, then be added 3.90g (i.e. additive amount be carbon dioxide quality 0.4%,
Under the experiment condition, the density of carbon dioxide is 813.52kg/m3) ten polyethenoxy ether of 2- ethyl butanol, open titanium dioxide
Carbon storage tank supplies valve injection supercritical carbon dioxide solvent 1200mL (i.e. solid-liquid ratio 1:12g/mL), in 45 DEG C, pressure
Dynamic extraction 4h under conditions of 20MPa, flow velocity 25L/h, obtains rose extract；The rose extract is introduced into the first fraction
From cooling decompression processing is carried out in device, the low macromolecular substances of dissolubility therein are removed, are handled using second level separator,
Supercritical carbon dioxide solvent therein is discharged from outlet in gaseous form, obtains Rosa Damascana, yield 0.80%.
From embodiment 1,2 and 3 and reference examples 1 it can be seen that the side for the extraction Rosa Damascana that embodiment 1,2 and 3 provides
Method is separately added into fatty alcohol polyoxypropylene ether additive while using supercritical carbon dioxide extraction method, extracts to rose
It can be obtained by Rosa Damascana after taking liquid to carry out two-stage separating treatment, do not need additionally to remove corresponding additive；Reference examples 1 mention
The method of the extraction Rosa Damascana of confession, is added entrainer ethanol solution while using supercritical carbon dioxide extraction method,
The rose extraction stoste that this method obtains needs first through two-stage separating treatment, then rotates processing and remove ethyl alcohol entrainment therein
Agent can just obtain Rosa Damascana followed by dewaxing treatment.Though the yield for the Rosa Damascana that embodiment 1,2 and 3 obtains is slightly lower
The yield of rose medicinal extract is obtained in reference examples 1, but is higher than the yield for the Rosa Damascana that reference examples 1 obtain.It can be seen that embodiment
1, rose can be effectively facilitated by fatty alcohol polyoxypropylene ether additive being added in the method for the 2 and 3 extraction Rosa Damascanas provided
The extraction of aroma component in valve, and compared with ethyl alcohol is added in the method that reference examples 1 provide, it eliminates in post-processing and removes second
The step of alcohol entrainer, preparation process is simplified.
Embodiment 4
It is six polyethenoxy ether of 2- propyl hexanol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extracted tobacco essential oil using above-mentioned additive, comprising: by the fresh cigarette of 100g
Silk filling into supercritical carbon dioxide extracting kettle, then be added 0.83g (i.e. additive amount be carbon dioxide quality 0.1%,
Under the experiment condition, the density of carbon dioxide is 834.89kg/m3) six polyethenoxy ether of 2- propyl hexanol, open carbon dioxide
Storage tank supply valve injection supercritical carbon dioxide solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL), 50 DEG C, pressure 25MPa,
Dynamic extraction 2h, obtains tobacco extraction liquid under conditions of flow velocity 30L/h；The tobacco extraction liquid is introduced into first order separator
Cooling decompression processing is carried out, the low macromolecular substances of dissolubility therein are removed, is handled using second level separator, it is therein
Supercritical carbon dioxide solvent is discharged from outlet in gaseous form, obtains essential oil of tobaccos, and the yield of the essential oil of tobaccos is 1.63%.
Embodiment 5
It is five polyethenoxy ether of 3- alkenyl octanol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extracted tobacco essential oil using above-mentioned additive, comprising: by the fresh cigarette of 100g
Silk filling into supercritical carbon dioxide extracting kettle, then be added 1.00g (i.e. additive amount be carbon dioxide quality 0.15%,
Under the experiment condition, the density of carbon dioxide is 834.89kg/m3) five polyethenoxy ether of 3- alkenyl octanol, open titanium dioxide
Carbon storage tank supply valve injection supercritical carbon dioxide solvent 800mL (i.e. solid-liquid ratio 1:8g/mL), 50 DEG C, pressure 25MPa,
Dynamic extraction 2h, obtains tobacco extraction liquid under conditions of flow velocity 30L/h；The tobacco extraction liquid is introduced into first order separator
Cooling decompression processing is carried out, the low macromolecular substances of dissolubility therein are removed, is handled using second level separator, it is therein
Carbon dioxide solvent becomes gaseous state, separates with extract, releases carbon dioxide gas, obtains essential oil of tobaccos, tobacco essence
The yield of oil is 1.83%.
Embodiment 6
It is six polyethenoxy ether of 2- methyl-decanol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extracted tobacco essential oil using above-mentioned additive, comprising: by the fresh cigarette of 100g
Silk filling into supercritical carbon dioxide extracting kettle, then be added 0.92g (i.e. additive amount be carbon dioxide quality 0.1%,
Under the experiment condition, the density of carbon dioxide is 834.89kg/m3) six polyethenoxy ether of 2- methyl-decanol, open carbon dioxide
Storage tank supply valve injection supercritical carbon dioxide solvent 1100mL (i.e. solid-liquid ratio 1:11g/mL), 50 DEG C, pressure 25MPa,
Dynamic extraction 2h, obtains tobacco extraction liquid under conditions of flow velocity 30L/h；The tobacco extraction liquid is introduced into first order separator
Cooling decompression processing is carried out, the low macromolecular substances of dissolubility therein are removed, is handled using second level separator, wherein surpassing
Critical carbon dioxide solvent is discharged from outlet in gaseous form, obtains essential oil of tobaccos, and the yield of the essential oil of tobaccos is 1.62%.
Embodiment 7
It is nine polyethenoxy ether of 2- normal-butyl enanthol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extracted tobacco essential oil using above-mentioned additive, comprising: by the fresh cigarette of 100g
Silk filling into supercritical carbon dioxide extracting kettle, then be added 1.00g (i.e. additive amount be carbon dioxide quality 0.1%,
Under the experiment condition, the density of carbon dioxide is 834.89kg/m3) nine polyethenoxy ether of 2- normal-butyl enanthol, open titanium dioxide
Carbon storage tank supplies valve injection supercritical carbon dioxide solvent 1200mL (i.e. solid-liquid ratio 1:12g/mL), in 50 DEG C, pressure
Dynamic extraction 2h under conditions of 25MPa, flow velocity 30L/h, obtains tobacco extraction liquid；The tobacco extraction liquid is introduced into the first fraction
From cooling decompression processing is carried out in device, the low macromolecular substances of dissolubility therein are removed, are handled using second level separator,
Carbon dioxide solvent therein becomes gaseous state, separates with extract, releases carbon dioxide gas, obtains essential oil of tobaccos, should
The yield of essential oil of tobaccos is 1.74%.
Reference examples 2
This reference examples provides a kind of method of extracted tobacco essential oil, and this method and the difference of embodiment 4-7 essentially consist in, this
Fatty alcohol polyoxypropylene ether class additive is not added in reference examples 2；The solid-liquid ratio of this reference examples 2 and the solid-liquid ratio of embodiment 5-7
It is different.Specifically, the extracting method that this reference examples provides are as follows: fill the fresh pipe tobacco of 100g to supercritical carbon dioxide extracting kettle
In, carbon dioxide storage tank supply valve injection supercritical carbon dioxide solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL) is opened,
50 DEG C, pressure 25MPa, dynamic extraction 2h under conditions of flow velocity 30L/h, obtain extraction stoste；The extraction stoste is introduced into
Cooling decompression processing is carried out in primary separator, is removed the low macromolecular substances of dissolubility therein, is separated using the second level
Device processing, supercritical carbon dioxide solvent therein are discharged from outlet in gaseous form, obtain essential oil of tobaccos, the essential oil of tobaccos
Yield is 0.96%.
Embodiment 8
It is five polyethenoxy ether of n-heptanol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extraction tealeaves essential oil using above-mentioned additive, comprising: 100g is fresh
Tealeaves blade is transferred in supercritical extraction reactor, and 3.43g is then added, and (i.e. additive amount is the 0.4% of carbon dioxide quality, at this
Under experiment condition, the density of carbon dioxide is 857.82kg/m3) five polyethenoxy ether of n-heptanol, it opens carbon dioxide storage tank and supplies
Supercritical carbon dioxide solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL) is injected to valve, in 45 DEG C, pressure 25MPa, flow velocity
Dynamic extraction 3h under conditions of 20L/h obtains tea extraction liquid；The tea extraction liquid, which is introduced into first order separator, to carry out
Cooling decompression processing, removes the low macromolecular substances of dissolubility therein, handles using second level separator, therein super to face
Boundary's carbon dioxide solvent is discharged from outlet in gaseous form, obtains tealeaves essential oil, and the yield of tealeaves essential oil is 1.02%.
Embodiment 9
It is five polyethenoxy ether of 2- alkynyl lauryl alcohol that the present embodiment provides a kind of plants essential oil extractions with additive.
The present embodiment provides a kind of methods of extraction tealeaves essential oil using above-mentioned additive, comprising: 100g is fresh
Tealeaves blade is transferred in supercritical extraction reactor, then be added 0.43g (i.e. additive amount be carbon dioxide quality 0.05%,
Under the experiment condition, the density of carbon dioxide is 857.82kg/m3) five polyethenoxy ether of 2- alkynyl lauryl alcohol, open titanium dioxide
Carbon storage tank supplies valve injection supercritical carbon dioxide solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL), in 45 DEG C, pressure
Dynamic extraction 3h under conditions of 25MPa, flow velocity 20L/h, obtains tea extraction liquid；The tea extraction liquid is introduced into the first fraction
From device and cooling decompression processing is carried out, removes the low macromolecular substances of dissolubility therein, is handled using second level separator,
Supercritical carbon dioxide solvent therein is discharged from outlet in gaseous form, obtains tealeaves essential oil, the yield of the tealeaves essential oil is
0.74%.
Reference examples 3
This reference examples provides a kind of method for extracting tealeaves essential oil, and the difference of this method and embodiment 8 and 9 essentially consists in,
Fatty alcohol polyoxypropylene ether class additive is not added in this reference examples 3.Specifically, the extracting method that this reference examples provides are as follows: will
100g fresh tealeaves blade is transferred in supercritical extraction reactor, is opened carbon dioxide storage tank supply valve and is injected overcritical dioxy
Change carbon solvent 1000mL (i.e. solid-liquid ratio 1:10g/mL), dynamic extraction under conditions of 45 DEG C, pressure 25MPa, flow velocity 20L/h
3h obtains extraction stoste；The extraction stoste is introduced into progress cooling decompression processing in first order separator, removes therein molten
The low macromolecular substances of solution property, are handled, supercritical carbon dioxide solvent therein is in gaseous form using second level separator
It is discharged from outlet, obtains tealeaves essential oil, the yield of the tealeaves essential oil is 0.65%.
Therefore, when preparing plants essential oil, addition adds the method for extraction essential oil provided in an embodiment of the present invention on a small quantity
Add agent fatty alcohol polyoxypropylene ether type compound, supercritical carbon dioxide can be effectively improved to the extraction efficiency of plants essential oil；
And compared with general additive such as methanol, ethyl alcohol, the additive fatty alcohol polyoxypropylene ether type compound of addition
Ratio is lower, saves the process of removing additive, saves preparation step, reduces removing additive process bring fragrance object
The loss of matter.
Finally it should be noted that: the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, it should be understood by those ordinary skilled in the art that: still
It can modify to a specific embodiment of the invention or some technical features can be equivalently replaced；Without departing from this hair
The spirit of bright technical solution should all cover within the scope of the technical scheme claimed by the invention.
Claims (10)
1. a kind of plants essential oil extraction additive, is fatty alcohol polyoxypropylene ether type compound R (CH2CH2CH2O)nH, wherein
Group R is containing C6-12Fatty alcohol radical, the value of polymerization degree n is 5~10.
2. additive according to claim 1, which is characterized in that the group R is containing C6-12Straight chain fatty alcohol radical or contain
C6-12Branched fatty alcohol radical.
3. additive according to claim 2, which is characterized in that the group R is containing C6-12Alkane alcohol radical, contain C6-12
Alkene alcohol radical or contain C6-12Alkynes alcohol radical.
4. additive according to claim 3, which is characterized in that the fatty alcohol polyoxypropylene ether type compound is straight chain
Alkane alcohol radical polyethenoxy ether, skeleton symbol CH3(CH2)4-10CH2O(CH2CH2CH2O)5-10H。
5. additive according to claim 3, which is characterized in that the fatty alcohol polyoxypropylene ether type compound is branch
Alkane alcohol radical polyethenoxy ether, skeleton symbol are [CH3(CH2)m1][CH3(CH2)m2]CHCH2O(CH2CH2CH2O)5-10H, wherein
The value of the sum of m1 and m2 is 2~8, and m1 and m2 is 0 or positive integer.
6. a kind of method of extraction essential oil, comprising steps of being added described in any one of Claims 1 to 5 into plant material
Additive and supercritical carbon dioxide solvent carry out plants essential oil extraction processing, wherein the additional amount of the additive is institute
State the 0.02%~0.8% of supercritical carbon dioxide solvent quality.
7. the method for extraction essential oil according to claim 6, which is characterized in that the plant material surpasses with described
The solid-liquid ratio of critical carbon dioxide solvent is 1:8~1:12 g/mL.
8. the method for extraction essential oil according to claim 6 or 7, which is characterized in that by the plant material and institute
It states additive to be placed in extraction kettle, then under conditions of 45 DEG C~65 DEG C and 15~35 MPa, injects the overcritical dioxy
Change 1~5 h of carbon solvent extraction and obtain extract liquor, separating-purifying processing is carried out to the extract liquor, the plants essential oil is made.
9. the method for extraction essential oil according to claim 8, which is characterized in that described to divide the extract liquor
Include: that the extract liquor is introduced into first order separator and carries out cooling processing from the step of purification processes, enters back into the second level
Removing carbon dioxide is removed in separator, and the plants essential oil is finally made.
10. the method for extraction essential oil according to claim 9, which is characterized in that the plant material is from new
One of the root of fresh plant, stem, leaf, flower, fruit, pericarp or its arbitrary combine.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3959154A (en) * | 1975-04-30 | 1976-05-25 | Robert Powers Cox | Method and composition for retarding the evaporation of ammonia and amines |
| CN102485771A (en) * | 2010-12-03 | 2012-06-06 | 中国石油天然气股份有限公司 | Fatty alcohol polyoxypropylene polyoxyethylene ether carboxylate, preparation thereof and application thereof |
| CN105395458A (en) * | 2015-12-15 | 2016-03-16 | 上海相宜本草化妆品股份有限公司 | Herbal composition and application thereof |
| CN105754570A (en) * | 2016-03-24 | 2016-07-13 | 中国石油大学(华东) | Supercritical CO2 microemulsion formed by anionic-nonionic amphoteric surfactant |
-
2019
- 2019-07-16 CN CN201910640009.1A patent/CN110373270B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3959154A (en) * | 1975-04-30 | 1976-05-25 | Robert Powers Cox | Method and composition for retarding the evaporation of ammonia and amines |
| CN102485771A (en) * | 2010-12-03 | 2012-06-06 | 中国石油天然气股份有限公司 | Fatty alcohol polyoxypropylene polyoxyethylene ether carboxylate, preparation thereof and application thereof |
| CN105395458A (en) * | 2015-12-15 | 2016-03-16 | 上海相宜本草化妆品股份有限公司 | Herbal composition and application thereof |
| CN105754570A (en) * | 2016-03-24 | 2016-07-13 | 中国石油大学(华东) | Supercritical CO2 microemulsion formed by anionic-nonionic amphoteric surfactant |
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