CN104212626B - A method of with subcritical fluid extraction cape jasmine oil - Google Patents
A method of with subcritical fluid extraction cape jasmine oil Download PDFInfo
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Abstract
The present invention discloses a kind of method with subcritical fluid extraction cape jasmine oil.First cape jasmine fruit pretreatment of raw material, and note amount puts into extractor；Then it checks extractor air-tightness, is 1:4 by solid-liquid mass ratio, leached liquefied butane input extractor with delivery pump, every tank carries out level Four leaching extraction, every grade of extraction time is two hours, second and third, level Four extract liquor respectively enter upper level extraction and use, first order extract liquor separates；First order extract liquor enters evaporator and carries out reduction vaporization precipitation, and cape jasmine crude oil is made, then cape jasmine crude oil is refined into finished product.The method of the present invention, can cape jasmine oil in high efficiency extraction cape jasmine fruit raw material, low energy consumption, and pollution-free, quality is high, will not especially destroy natural thermal sensitivity, oxidizable active constituent in cape jasmine oil.
Description
Technical field
It is specifically a kind of to use subcritical fluid extraction Cape jasmine the invention belongs to extract the method for effective component from plant material
The method of seed oil.
Background technique
Rich in cape jasmine oil in cape jasmine fruit, oil content is 17.6% close to soybean, its fatty acid composition of cape jasmine oil is more single
One, predominantly linoleic acid.Linoleic acid is one of essential fatty acid, cannot be synthesized in human body, it is necessary to absorb from food；
Linoleic acid can prevent atherosclerosis, reduce the content of blood lipid and serum total cholesterol, the anti-improper solidification of Hemostatic Oral Liquid, softening
Blood vessel, expansion artery increase blood circulation, adjust the endocrine system of heart aging, and activating microcirculation and removing stasis medicinal restores neural function indirectly
Can, to hypertension, the cardiovascular diseases such as coronary heart disease are had a better effect.In addition, linoleic acid can also make skin exquisiteness, therefore there is U.S. flesh
The title of acid.Therefore, Europe, the United States, Deng state have developed the margarine of high linoleic acid type in recent years, and this not only adds the battalion of food
It supports, while beauty can also be played the role of and prevented and cured diseases.Gardenia Seed Oil is through works such as saponification, acidification, acetone solution, freezing and crystallizings
Skill can also produce meet medical standards linoleic acid it is rigid.
Instantly, there are more than 20 families in the producer of domestic production cape jasmine oil.Most of producers are simply equipped, and production technology is fallen
Afterwards.Most of product that they are produced is medicinal extract and liquid, pulvis it is of poor quality, it is difficult to participate in the competition of international market, therefore more
Number production cape jasmine oil producers all in halt production, partly stop production or change the line of production state, domestic cape jasmine oil yield is only at 120~150 tons/year
Between.And since the country is far below western developed country to cape jasmine oil nutritive value cognition degree, people are directly influenced to cape jasmine
The consumption of oil specializes in research and promotes cape jasmine oil in European and American developed countries all about the special scientific research institution of cape jasmine oil
Scientific and technological content, and the science and technology strength of cape jasmine oil is put into since China lacks in China and cape jasmine reasonable utilization rate is low, because
This cape jasmine oil is in a disadvantageous position always in China's grease industry, and there are no form powerful industry.But in recent years, disappearing with people
Take consciousness and behavior and multinomial selection is turned to by individual event selection, cape jasmine oil is just gradually approved and favored by the majority of consumers.
Currently, having infusion process, percolation, decocting method, reflux extraction, continuous time in terms of the refinement method of cape jasmine oil
Flow extraction method, steam distillation method, sublimed method, ultrasonic extraction and supercritical CO2The processes such as fluids extraction.Wherein,
Infusion process, percolation, decocting method, the extracting power of reflux extraction and continuous circumfluence extraction method are strong, and selectivity is strong, but is extracting
It takes, in separation process, technological temperature requires more than 50 DEG C or more, easily causes " thermal sensitivity " effective component in cape jasmine oil different degrees of
Decomposition or denaturation so that product occur it is time biochemical；In addition, the lipophylic organic solvents that they are used extract product produced
In dissolvent residual it is high, reduce the quality of product, and the organic solvent that can be chosen belongs to inflammable thing, the safety of production process more
Hidden danger is difficult to eliminate.Steam distillation method and sublimed method affect the application field of this method since its specific aim is too strong, not by
It is widely popularized；Ultrasonic extraction has larger improvement to Conventional processing methods, has preferable economy and extensive adaptability,
But still it can not overcome or be avoided completely using inflammable organic solvent.It now appear that supercritical CO2Fluids extraction is current
Ideal process has extracting power strong, and recovery rate is high, and selectivity is strong, the advantages such as superior product quality, but CO2
It must can carry out extraction processing under the superelevation pressure condition of 25MPa or more, high pressure limit equipment dischargeable capacity
Amplification, also constrain the technology intermediate production in industrial applications.
Summary of the invention
Traditional method for extracting cape jasmine oil when low efficiency, safety is poor, cape jasmine oil quality is poor, low output aiming at the problem that,
It, can be in high efficiency extraction cape jasmine fruit raw material the purpose of the present invention is to provide a kind of method with subcritical fluid extraction cape jasmine oil
Cape jasmine oil, low energy consumption, pollution-free, and quality is high, will not especially destroy natural thermal sensitivity in cape jasmine oil, oxidizable activity at
Point.
A kind of method with subcritical fluid extraction cape jasmine oil of the present invention, comprising the following steps:
(1) cape jasmine fruit raw material successively carried out impurity elimination, remove stone, broken, softening, pressure embryo pretreatment, and will be pretreated
Cape jasmine fruit raw material note amount puts into extractor；
(2) it checks extractor air-tightness, is 1:4 by solid-liquid mass ratio, with delivery pump by liquid after ensuring that air-tightness is good
State butane input extractor is leached；
(3) every tank carries out level Four leaching extraction, every grade of extraction time is two hours, and extractor is when carrying out leaching extraction
Pressure is 0.3-0.7MPA, and extraction temperature is 30 ~ 38 DEG C, second and third, level Four extract liquor respectively enter upper level extraction and use, the
Level-one extract liquor is separated；
(4) first order extract liquor enters evaporator and carries out reduction vaporization precipitation, and cape jasmine crude oil is made, while opening compression
Machine recycles gaseous solvent butane, and compression condensation is liquid, returns to butane solvent tank；
(5) after fourth stage extraction, compressor, vacuum pump are opened, and the steam of 0.05MPa is passed through into extractor,
Residual solvent butane in the cape jasmine dregs of rice is recycled, compression condensation is liquid, returns to butane solvent tank；
(6) the degreasing cape jasmine dregs of rice are drawn off out of extractor, and cleans extractor；
(7) refining treatment is carried out to cape jasmine crude oil, refining treatment is successively aquation alkali refining, dehydration, decoloration, deodorization, crystallization
Filtering, eventually becomes finished product；In aquation alkali refining, amount of water is 2.5-3 times of peptization material content in cape jasmine oil, starts to stir
Speed is 55-65r/ minute, when peptization material particle is formed, is controlled at 15-25r/ minutes, when peptization material particle coagulates
Poly- to stop stirring in when being clearly separated state, oil temperature is 38 DEG C or so when adding water, and final temperature control is at 45 DEG C or so, quiescent setting
5-6 hours.
Further, the cape jasmine fruit raw material is broken, and degree of grinding is 45 ~ 60 mesh.
Further, the decolorization uses, carclazyte and wooden carbon.
Further, the deodorising process is deodorized 6-8 hours under the conditions of vacuum degree-0.01Mpa, 40 DEG C.
By adopting the above-described technical solution, the diffusion of molecule enhances in the presence of butane is with subcritical fluids state,
Mass transfer velocity is accelerated, to the permeability and solvability of low pole and apolar substance in the natural products in cape jasmine fruit raw material
It significantly improves.Thus, extraction of the above-mentioned subcritical fluids particularly suitable for volatile oil, grease or liposoluble constituent in natural products.
It is extracted under subcritical environment, does not destroy that cape jasmine oil heat-sensitive ingredients, purpose object are complete, be considered as environmentally protective, have a extensive future
One change property technology.
Subcritical fluids are mainly liquefied butane.The solvent boiling point is -0.5 DEG C, is at normal temperatures and pressures gas, after pressurization
For liquid.The basic principle of the technique is: under room temperature and certain pressure (0.3MPa -0.7MPa), with subcritical fluids adverse current
Cape jasmine raw material material embryo is extracted, so that the solvent under reduced pressure in miscella and the dregs of rice is gasified, the solvent gas after gasification is using compression
It is recycled after machine condensing liquid.
A kind of method with subcritical fluid extraction cape jasmine oil of the present invention has the advantage that
A. Residual oil is residual molten less than 50ppm less than 1.5% in the dregs of rice after extracting.
B. molten consumption is low, and ton material consumption is molten to be less than 6kg.
C. it is not required to steam, only 90 DEG C of hot water, opposite No. six solvents can saving heat energy 70%.
D. three-waste free pollution in production belongs to environment-friendly engineering.
E. room temperature extracts, low temperature (less than 30 DEG C) precipitation, does not destroy to the heat-sensitive substance in the dregs of rice and oil.
F. invest small, production cost is low, and operating pressure is less than 0.7MPa, and security performance is high.
G. subcritical fluids source is wide, and price is low, and each oil gas field, oil plant have butane product.
H. the technology and equipment are fexible unit, can process various materials using the equipment: as cape jasmine oil, capsicum are red
Element, Chinese medicine, fragrance, safflower seed oil etc..
Therefore, subcritical cape jasmine oil abstraction technique is a kind of separation of the efficient low-consume Environmental Safety with broad prospect of application
Extractive technique.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the method with subcritical fluid extraction cape jasmine oil of the present invention.
Specific embodiment
Referring to Fig. 1, a method of with subcritical fluid extraction cape jasmine oil, comprise the following steps that
(1) cape jasmine fruit raw material successively carried out impurity elimination, remove stone, broken, softening, pressure embryo pretreatment, and will be pretreated
Cape jasmine fruit raw material note amount puts into extractor；
(2) it checks extractor air-tightness, is 1:4 by solid-liquid mass ratio, with delivery pump by liquid after ensuring that air-tightness is good
State butane input extractor is leached；
(3) every tank carries out level Four leaching extraction, every grade of extraction time is two hours, and extractor is when carrying out leaching extraction
Pressure is 0.3-0.7MPA, and extraction temperature is 30 ~ 38 DEG C, second and third, level Four extract liquor respectively enter upper level extraction and use, the
Level-one extract liquor is separated；
(4) first order extract liquor enters evaporator and carries out reduction vaporization precipitation, and cape jasmine crude oil is made, while opening compression
Machine recycles gaseous solvent butane, and compression condensation is liquid, returns to butane solvent tank；
(5) after fourth stage extraction, compressor, vacuum pump are opened, and the steam of 0.05MPa is passed through into extractor,
Residual solvent butane in the cape jasmine dregs of rice is recycled, compression condensation is liquid, returns to butane solvent tank；
(6) the degreasing cape jasmine dregs of rice are drawn off out of extractor, and cleans extractor；
(7) refining treatment is carried out to cape jasmine crude oil, refining treatment is successively aquation alkali refining, dehydration, decoloration, deodorization, crystallization
Filtering, eventually becomes finished product.
Wherein, the cape jasmine fruit raw material is broken, and degree of grinding is 45 ~ 60 mesh.
Wherein, the aquation alkali refining is divided into aquation and alkali refining, and aquation is: using the hydrophily of peptization material, using one
The electrolyte solutions such as quantitative hot water or diluted alkaline, salt are added in hot oil insoluble impurities in grease is promoted to agglomerate under stiring
Precipitation and separation.The factor for influencing degumming mainly has temperature, amount of water and mixing speed etc..Add coolant-temperature gage low or coolant-temperature gage is added to be higher than
Oil temperature all emulsifies to some extent, therefore in hydration process, it is necessary to hot water be added and be equal to or higher than cape jasmine in water temperature
It is added when oil temperature.Amount of water excessively will also result in emulsification, and cause trouble to subsequent dehydration, own when amount of water is very few
Glue soluble substance all coagulative precipitation and cannot be difficult to separate, best amount of water can be determined by little sample testing.Mixing speed mistake
Fastly, glue soluble substance is not easy to agglomerate, and even if cohesion and sedimentation time it is longer, but when mixing speed is too low glue soluble substance and
Water cannot come into full contact with, and degumming purpose is not achieved.Amount of water in the present invention is peptization material content 2.5-3 in cape jasmine oil
Times, starting mixing speed is 55-65r/ minute, and when peptization material particle is formed, control worked as glue at 15-25r/ minutes
Molten material particle cohesion stops stirring in when being clearly separated state, and oil temperature is 38 DEG C or so when adding water, and final temperature controls on 45 DEG C of left sides
The right side, quiescent setting 5-6 hours；The purpose of alkali refining is: the free fatty acid in removing cape jasmine crude oil increases the transparency of oil,
Smoke point is reduced, oxidation deterioration is prevented.Alkali refining is the committed step of cape jasmine oil refinement, and the quality of alkali refining effect directly affects refined oil
The height of quality.Alkali refining is actually the process of an acid-base neutralization, and basic principle is occurred using lye and free fatty acid
Neutralization reaction forms the alkali metal salt of fatty acid, thus separated with grease, and while acid-base neutralization forming salt precipitating, it will
Phosphatide, protein, viscose glue, pigment in grease etc. remove.Caustic dosage, concentration of lye plus the alkali uniformity are to influence to subtract refining again
Principal element adds alkali excessive, and oil soap increases, and easily causes dry phenomenon；Caustic dosage is inadequate, easily causes neat soap meticulous, and precipitating number is small
When oil soap do not separate still.And concentration of lye is excessively dilute, and moisture content is excessive, and Yi Yinqi grease emulsifying adds alkali unevenly to easily cause part
Excessively, whole pot oil alkali number is insufficient for saponification.Meanwhile also there are correlativity in oil alkali refining initial temperature and alkali refining effect, sedimentation time.
Wherein, it decolourizes, decoloration process is batch production, is suitble to the de- of various edible oil materials qualified after aquation alkali refining
Color process.(1) ingredient requirement: moisture≤0.5%, phosphorous≤20ppm contain soap≤0.3%.(2) auxiliary material requirement: carclazyte: food grade,
It can be according to the quality requirement for Bu Tong determining carclazyte of the kind and quality of cape jasmine oil.Activated carbon: food grade, mostly wooden carbon.
Wherein, deodorization refers to that malodor components process is referred to as to be deodorized in removal Gardenia Seed Oil.The purpose of deodorization is oil removing
Expect that hydrolysis occurs in storage, producing process, aoxidizes product generated (ketone, aldehyde for itself special composition and triglyceride
And free fatty acid, sulfur-containing compound etc.), and in refining process, alkali refining oil cleans brought alkali taste scent and leaching
Remaining solvent of crude oil etc. causes the had special odor of grease out.The basic principle of deodorization: under certain vacuum, glycerol is utilized
The difference of three acid esters and volatility is water vapour by the way that in the grease containing malodor components, generation vapour-liquid surface is contacted, and water
Steam is saturated by the malodor components of volatilization, and by the evolution of the ratio of its partial pressure, to achieve the purpose that stink in abjection oil.?
Vacuum degree-0.01Mpa, it is deodorized 6-8 hours under the conditions of 40 DEG C.
Cape jasmine oil physical and chemical property determining:
By legal conventional method to by the appearance of cape jasmine oil produced by the invention, smell, index of refraction, density, acid value, iodine
Value, saponification number and peroxide value etc. are measured, and measurement result is shown in Table 1.
1 cape jasmine oil physicochemical property of table
GC/MS analysis, the preparation of fatty acid methyl ester, using transesterification are formed by Gardenia Seed Oil fat acid produced by the invention
Method: weighing 0.2g oil sample, is transferred in 10ml volumetric flask, adds 1ml ether-normal hexane (2:1) solution, adds 0.5mol/L hydrogen
Potassium oxide-methanol solution, shakes up, and stands 30 minutes, adds water to scale, and supernatant liquor is taken to carry out GC/MS measurement；Determination condition:
Instrument: U.S. HP5988A type GC/MS combined instrument.Chromatographic column: SE-59 quartz capillary column (25m,0.2mm), column temperature
60-280 DEG C, 10 DEG C/min of temperature programming, 280 DEG C of temperature of vaporization chamber, carrier gas He, electron bombardment ionization source, electric flux 70eV, ion
Change power supply 300, resolution ratio 500；Measurement result: by the standard in PBM search library in resulting mass spectrometric data and computer
Spectrum is compareed, and the composition of grease is identified.The peak area of total ion chromatogram is normalized, then can obtain each rouge
The relative amount of fat acid.It, which measures analysis, the results are shown in Table 2.
2 Gardenia Seed Oil fat acid main component of table
。
Claims (4)
1. a kind of method with subcritical fluid extraction cape jasmine oil, it is characterized in that comprising the following steps that
(1) cape jasmine fruit raw material successively carried out impurity elimination, remove stone, broken, softening, pressure embryo pretreatment, and by pretreated cape jasmine
Fruit raw material note amount puts into extractor；
(2) it checks extractor air-tightness, is 1:4 by solid-liquid mass ratio, with delivery pump by liquid fourth after ensuring that air-tightness is good
Alkane input extractor is leached；
(3) every tank carries out level Four leaching extraction, and every grade of extraction time is two hours, pressure of the extractor when carrying out leaching extraction
For 0.3-0.7MPA, extraction temperature is 30 ~ 38 DEG C, second and third, level Four extract liquor respectively enter upper level extraction and use, the first order
Extract liquor is separated；
(4) first order extract liquor enters evaporator and carries out reduction vaporization precipitation, and cape jasmine crude oil is made, while opening compressor,
Gaseous solvent butane is recycled, compression condensation is liquid, returns to butane solvent tank；
(5) after fourth stage extraction, compressor, vacuum pump are opened, and the steam of 0.05MPa is passed through into extractor, recycling
Residual solvent butane in the cape jasmine dregs of rice, compression condensation are liquid, return to butane solvent tank；
(6) the degreasing cape jasmine dregs of rice are drawn off out of extractor, and cleans extractor；
(7) refining treatment being carried out to cape jasmine crude oil, refining treatment is successively aquation alkali refining, dehydration, decoloration, deodorization, crystallizes filtering,
Eventually become finished product；In the aquation alkali refining, amount of water is 2.5-3 times of peptization material content in cape jasmine oil, starts stirring speed
Degree is 55-65r/ minute, when peptization material particle is formed, is controlled at 15-25r/ minutes, when the cohesion of peptization material particle
When in being clearly separated state, stop stirring, oil temperature is 38 DEG C or so when adding water, and final temperature control is at 45 DEG C or so, quiescent setting 5-
6 hours.
2. a kind of method with subcritical fluid extraction cape jasmine oil as described in claim 1, it is characterized in that: the cape jasmine fruit is former
Material is broken, and degree of grinding is 45 ~ 60 mesh.
3. a kind of method with subcritical fluid extraction cape jasmine oil as described in claim 1, it is characterized in that: the decolorization
It uses, carclazyte and wooden carbon.
4. a kind of method with subcritical fluid extraction cape jasmine oil as described in claim 1, it is characterized in that: described be deodorized
Journey is deodorized 6-8 hours under the conditions of vacuum degree-0.01Mpa, 40 DEG C.
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| CN105001991A (en) * | 2015-06-15 | 2015-10-28 | 中国林业科学研究院林产化学工业研究所 | Ledum palustre extractive with sterilization function and preparing method and application thereof |
| CN105132184B (en) * | 2015-09-11 | 2019-07-09 | 中国林业科学研究院林产化学工业研究所 | A kind of method of subcritical abstraction and molecular distillation coupling preparation cape jasmine flower essential oil |
| CN105112155A (en) * | 2015-09-11 | 2015-12-02 | 福建恒康生态农业发展有限公司 | Preparation method of high-quality cape jasmine seed oil rich in linoleic acid |
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| CN110117512B (en) * | 2019-06-06 | 2022-06-03 | 浙江骄栀科技有限公司 | Automatic gardenia oil extraction production line |
| CN110591810A (en) * | 2019-06-06 | 2019-12-20 | 浙江骄栀科技有限公司 | Gardenia oil extraction process |
| CN110343564A (en) * | 2019-07-19 | 2019-10-18 | 湖北聿津生物科技有限公司 | A kind of method that cape jasmine oil is extracted in continuous phase transistion |
| CN110357935B (en) * | 2019-07-19 | 2023-02-14 | 湖北聿津生物科技有限公司 | Method for extracting geniposide and yellow pigment step by step through continuous phase change |
| CN115851380A (en) * | 2023-02-28 | 2023-03-28 | 云南云科特色植物提取实验室有限公司 | Saussurea lappa volatile oil and preparation method and application thereof |
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Address after: Nanyang City, Henan province Tanghe County 473000 Zan Gang Xiang Gang Liu Industrial Park Applicant after: Terry biological Polytron Technologies Inc, Nanyang Address before: Nanyang City, Henan province Tanghe County 473000 Zan Gang Xiang Gang Liu Industrial Park Applicant before: NANYANG TERRY BIOLOGICAL PRODUCTS CO., LTD. |
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