CN109627157A - The method of alpha-linolenic acid is purified in a kind of linseed oil - Google Patents
The method of alpha-linolenic acid is purified in a kind of linseed oil Download PDFInfo
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- CN109627157A CN109627157A CN201811620009.7A CN201811620009A CN109627157A CN 109627157 A CN109627157 A CN 109627157A CN 201811620009 A CN201811620009 A CN 201811620009A CN 109627157 A CN109627157 A CN 109627157A
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- linolenic acid
- linseed oil
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to a kind of methods that alpha-linolenic acid is purified in linseed oil, belong to natural materials purification field.The method of alpha-linolenic acid is purified in the linseed oil the following steps are included: carrying out supercritical extract to linseed oil obtains extract；Decompression separation is carried out to extract and obtains just alpha-linolenic acid processed；Molecular distillation is carried out to just alpha-linolenic acid processed and obtains alpha-linolenic acid.This method is easy to operate, and energy efficiency is pollution-free, can significantly promote the refining effect of alpha-linolenic acid in linseed oil, linolenic acid content is purified to 90% or more.
Description
Technical field
The present invention relates to natural materials to extract field, and the side of alpha-linolenic acid is purified in particular to a kind of linseed oil
Method.
Background technique
Flax is the annual herb plant of flax family (Linaceae), linum, is most ancient one of long-term cropping, all over China
All there is cultivation, is especially to contain with the Inner Mongol, Gansu, Shaanxi and Shanxi.It is a kind of good oil crops, is widely used in oil
Rouge industry, linseed oil unsaturated fatty acid containing volume can effectively prevent the diseases such as hyperlipemia, atherosclerosis.Its institute
Have in position, the fat content of linseed is most, therefore multi-purpose linseed extracts linseed oil.
Alpha-linolenic acid can be extracted in linseed oil, had the effects that improve intelligence, antithrombotic, liver protection, be people
One of necessary nutrient, there is important meaning to the health of human body, and preparation also has many therapeutic effects medically, flax
The alpha-linolenic acid content in linseed oil that seed oil extract goes out is 50% or so, is unable to satisfy demand of the people to its purity, because
This needs further purification alpha-linolenic acid, for preparing alpha-linolenic acid derived product.
Given this special to propose the application.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that alpha-linolenic acid is purified in linseed oil, and this method is easy to operate,
Energy efficiency is pollution-free, can significantly promote the refining effect of alpha-linolenic acid in linseed oil, linolenic acid content is purified to
90% or more.
The present invention solves its technical problem and adopts the following technical solutions to realize:
The present invention proposes a kind of method that alpha-linolenic acid is purified in linseed oil, comprising the following steps:
Supercritical extract is carried out to linseed oil and obtains extract；
Decompression separation is carried out to extract and obtains just alpha-linolenic acid processed；
Molecular distillation is carried out to just alpha-linolenic acid processed and obtains alpha-linolenic acid.
The beneficial effect that the method for alpha-linolenic acid is purified in the linseed oil that the embodiment of the present invention proposes is:
The embodiment of the present invention is simple and efficient by using the coherent combination of supercritical extract, decompression separation and molecular distillation
Mode of operation so that the refining effect of alpha-linolenic acid is significantly promoted in linseed oil, and residual without chemical solvent in the process
It stays, energy conservation and environmental protection.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The method that alpha-linolenic acid is purified in the linseed oil of the embodiment of the present invention is specifically described below.
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
Supercritical extract is carried out to linseed oil and obtains extract.
Specifically, take linseed oil that extractant is added as raw material, alpha-linolenic acid must be contained by then carrying out supercritical extract
Extract.The method of supercritical extract can effectively extract alpha-linolenic acid in linseed oil, because it is using overcritical
The solvability of fluid separates mixture with the relationship of the density of institute extraction of substance, therefore in suitable temperature and pressure
In the case where, the alpha-linolenic acid of very high purity and the mixture of extractant can be extracted, it is only necessary to remove the alpha-linolenic acid and extraction
Take the extractant in the mixture of agent that the alpha-linolenic acid of very high purity can be obtained.On the other hand, supercritical extract overall process is not
With organic solvent, therefore the absolutely not remaining vehicle substance of extract, to prevent depositing for the object that is harmful to the human body in extraction process
With the pollution to environment, ensure that the pure natural property of extraction.
Further, extractant is carbon dioxide, is inactive gas, using it as extractant, in extraction process
It will not be chemically reacted with the substance in linseed oil, will not influence the quality of alpha-linolenic acid, and it belongs to non-flammable gases,
Tasteless, odorless, nontoxic, safety is very good；On the other hand, carbon dioxide gas is cheap, and purity is high is easy to produce, and
It can be used in production with repetitive cycling, to significantly reduce cost.
Further, the volume ratio of linseed oil and carbon dioxide is 1:2-4, and the ratio is in the extraction for guaranteeing alpha-linolenic acid
The dosage for reducing carbon dioxide while adequacy as far as possible, avoids the waste of extractant, extracted to further reduced
The cost of journey.
Further, during supercritical extract, extracting pressure is 160-190 atmospheric pressure, extraction temperature 70-90
℃.In supercritical extract, pressure and temperature influences it significantly, to be embodied in, and the solvent strength of supercritical fluid depends on
The temperature and pressure of extraction, i.e. change pressure and temperature, so that it may the different component in linseed oil be pressed molten in extractant
The size of Xie Du successively extracts, while can also play the role of separation.Wherein, the variation of temperature is embodied in influence extraction
The density of agent and two factors of vapour pressure of solute influence extracting pressure indirectly, in the common of specific temperature and specified pressure
Under effect, required component can be just extracted.In the present embodiment, extracting pressure is 160-190 atmospheric pressure, extraction temperature 70-
90 DEG C, which can efficiently and quickly extract the alpha-linolenic acid in linseed oil under conditions of pressure.
Further, extraction time is 1-1.5 hours, which can guarantee the adequacy of extraction, makes linseed
Alpha-linolenic acid in oil is fully extracted as far as possible, to increase the usage amount of raw material.
S2, separation；
Decompression separation is carried out to extract and obtains just alpha-linolenic acid processed.Since the extractant in step S1 is carbon dioxide, because
This can effectively be separated extract with extractant using the method for decompression separation.
Specifically, decompression separation step includes first order decompression separation and second level decompression separation, obtains above-mentioned extraction
The extract containing alpha-linolenic acid pass sequentially through first order decompression separation and second level decompression separation, thus by extract
Alpha-linolenic acid separates to obtain first alpha-linolenic acid processed.It is that decompression excessively leads to carbon dioxide in order to prevent using two-stage decompression separation
Bumping occurs, first passes through the first pole decompression separation alpha-linolenic acid processed at the beginning of as buffering and obtaining a part, then subtract by the second pole
Pressure separation thoroughly obtains just alpha-linolenic acid processed, this method ensure that ensure that the effect of separation while the safety of experiment.
Further, the pressure of the first pole decompression separation is 5-7MPa, and temperature is 35-50 DEG C.The separating pressure and temperature
It can be effectively prevented carbon dioxide generation bumping while guaranteeing that carbon dioxide is separated with extract, and be able to maintain point
Stabilization from process, to reduce the damage to experimental facilities.
Further, the pressure of second level decompression separation is 3-5MPa, and temperature is 32-40 DEG C.In the first pole decompression separation
On the basis of, which can improve separative efficiency and effect under the premise of keeping separating and stablize with temperature.
Further, the time of decompression separation is 30-50 minutes, to guarantee isolated completeness.
S3, distillation；
Molecule steaming is carried out to the first alpha-linolenic acid processed that above-mentioned first pole decompression separation and the second pole decompression separation are extracted
Evaporate to obtain alpha-linolenic acid.α-the flax extracted can further be purified using the method for molecular distillation on the basis of decompression separation
The purity of acid, other liquid impurities mixed in supercritical extract step is further separated with alpha-linolenic acid, thus further
Purification obtains the alpha-linolenic acid of high-purity.
Further, vapo(u)rizing temperature is 20-25 DEG C, pressure 0.08-0.15MPa.The temperature with can be effective under pressure
Ground separates alpha-linolenic acid with other liquid impurities, so that purification obtains the alpha-linolenic acid of high-purity.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
It is 160 atmospheric pressure in extracting pressure, under conditions of extraction temperature is 90 DEG C, according to the ratio of volume ratio 1:2 to Asia
Carbon dioxide is added in flaxseed oil and carries out supercritical extract 1.5 hours obtaining extract.
S2, separation；
So that above-mentioned extract is passed sequentially through the first pole decompression separation and obtains just α-flax processed respectively with the second pole decompression separation
Acid, wherein the pressure of the first pole decompression separation is 5MPa, and temperature is 50 DEG C, and the pressure of second level decompression separation is 3MPa, temperature
It is 40 DEG C, the time of decompression separation is 30 minutes.
S3, distillation；
It is 25 DEG C in temperature, under conditions of pressure is 0.08MPa, to above-mentioned first pole decompression separation and the decompression point of the second pole
Alpha-linolenic acid is obtained from obtained first alpha-linolenic acid progress molecular distillation processed is extracted.
Embodiment 2
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
It is 190 atmospheric pressure in extracting pressure, under conditions of extraction temperature is 70 DEG C, according to the ratio of volume ratio 1:4 to Asia
Carbon dioxide is added in flaxseed oil and carries out supercritical extract 1 hour obtaining extract.
S2, separation；
So that above-mentioned extract is passed sequentially through the first pole decompression separation and obtains just α-flax processed respectively with the second pole decompression separation
Acid, wherein the pressure of the first pole decompression separation is 7MPa, and temperature is 35 DEG C, and the pressure of second level decompression separation is 5MPa, temperature
It is 32 DEG C, the time of decompression separation is 50 minutes.
S3, distillation；
It is 20 DEG C in temperature, under conditions of pressure is 0.15MPa, to above-mentioned first pole decompression separation and the decompression point of the second pole
Alpha-linolenic acid is obtained from obtained first alpha-linolenic acid progress molecular distillation processed is extracted.
Embodiment 3
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
It is 170 atmospheric pressure in extracting pressure, under conditions of extraction temperature is 85 DEG C, according to the ratio of volume ratio 2:5 to Asia
Carbon dioxide is added in flaxseed oil and carries out supercritical extract 1.3 hours obtaining extract.
S2, separation；
So that above-mentioned extract is passed sequentially through the first pole decompression separation and obtains just α-flax processed respectively with the second pole decompression separation
Acid, wherein the pressure of the first pole decompression separation is 5.5MPa, and temperature is 45 DEG C, and the pressure of second level decompression separation is 3.5MPa,
Temperature is 38 DEG C, and the time of decompression separation is 35 minutes.
S3, distillation；
It is 23 DEG C in temperature, under conditions of pressure is 0.10MPa, to above-mentioned first pole decompression separation and the decompression point of the second pole
Alpha-linolenic acid is obtained from obtained first alpha-linolenic acid progress molecular distillation processed is extracted.
Embodiment 4
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
It is 180 atmospheric pressure in extracting pressure, under conditions of extraction temperature is 75 DEG C, according to the ratio of volume ratio 2:7 to Asia
Carbon dioxide is added in flaxseed oil and carries out supercritical extract 1.2 hours obtaining extract.
S2, separation；
So that above-mentioned extract is passed sequentially through the first pole decompression separation and obtains just α-flax processed respectively with the second pole decompression separation
Acid, wherein the pressure of the first pole decompression separation is 6.5MPa, and temperature is 37 DEG C, and the pressure of second level decompression separation is 4.8MPa,
Temperature is 35 DEG C, and the time of decompression separation is 48 minutes.
S3, distillation；
It is 22 DEG C in temperature, under conditions of pressure is 0.12MPa, to above-mentioned first pole decompression separation and the decompression point of the second pole
Alpha-linolenic acid is obtained from obtained first alpha-linolenic acid progress molecular distillation processed is extracted.
Embodiment 5
The method of alpha-linolenic acid is purified in a kind of linseed oil provided in an embodiment of the present invention comprising following steps:
S1, extraction；
It is 180 atmospheric pressure in extracting pressure, under conditions of extraction temperature is 80 DEG C, according to the ratio of volume ratio 1:2 to Asia
Carbon dioxide is added in flaxseed oil and carries out supercritical extract 1 hour obtaining extract.
S2, separation；
So that above-mentioned extract is passed sequentially through the first pole decompression separation and obtains just α-flax processed respectively with the second pole decompression separation
Acid, wherein the pressure of the first pole decompression separation is 6MPa, and temperature is 40 DEG C, and the pressure of second level decompression separation is 4MPa, temperature
It is 35 DEG C, the time of decompression separation is 40 minutes.
S3, distillation；
It is 23 DEG C in temperature, under conditions of pressure is 0.11MPa, to above-mentioned first pole decompression separation and the decompression point of the second pole
Alpha-linolenic acid is obtained from obtained first alpha-linolenic acid progress molecular distillation processed is extracted.
Comparative example 1
Difference with embodiment 5 is, does not carry out molecular distillation.
Comparative example 2
Difference with embodiment 5 is, prepares alpha-linolenic acid using the method for enzyme hydrolysis and molecular distillation.
Comparative example 3
Difference with embodiment 5 is, in step S1, extraction temperature is 30 DEG C, and extracting pressure is 140 atmospheric pressure.
Comparative example 4
Difference with embodiment 5 is, is directly 3-5MPa, the decompression that temperature is 32-40 DEG C by pressure in step S2
Separation.
Comparative example 5
Difference with embodiment 5 is, in step S3, vapo(u)rizing temperature is 18 DEG C, pressure 0.5MPa.
Test example 1
The purity of alpha-linolenic acid made from method to embodiment 1-5 and comparative example 1-5 detects, testing result ginseng
It is shown in Table 1.
The purity of 1 alpha-linolenic acid of table
As shown in Table 1, in linseed oil provided by the invention purify alpha-linolenic acid method refining effect much higher than pair
The refining effect of the method for ratio 1-5, wherein pass through the comparison of comparative example 1-2 and embodiment 5, it can be seen that the present invention provides
Linseed oil in purify alpha-linolenic acid method selected by can successively effectively increase purification between step and step
Effect is able to demonstrate that by the comparison of comparative example 3-5 and embodiment 5: during 1. supercritical extracts, extracting pressure is
160-190 atmospheric pressure, extraction temperature, which is 70-90 DEG C, efficiently and quickly to be extracted the alpha-linolenic acid in linseed oil
Come, the DNA purity of alpha-linolenic acid can be dramatically increased under this condition；2. using first order decompression separation and the second level is passed sequentially through
The separate mode of decompression separation, and the pressure of the first pole decompression separation is limited as 5-7MPa, temperature is 35-50 DEG C, the second level
The pressure of decompression separation is 3-5MPa, and temperature is 32-40 DEG C, can further increase refining effect；3. vapo(u)rizing temperature is 20-25
DEG C, pressure is that the molecular distillation condition of 0.08-0.15MPa can effectively be such that alpha-linolenic acid separates with other liquid impurities, from
And increase the purification purity of alpha-linolenic acid.
To sum up, the method that alpha-linolenic acid is purified in linseed oil provided in an embodiment of the present invention, by using overcritical
The coherent mode of operation being simple and efficient combined of extraction, decompression separation and molecular distillation, so that alpha-linolenic acid in linseed oil
Refining effect significantly promoted, and in the process without chemical solvent remain, energy conservation and environmental protection；Further by limiting overcritical extraction
Temperature, the pressure and other parameters taken enhance the effect of extraction, and by setting first order decompression separation and for decompression separation
Second depressurized separation, ensure that the effect that ensure that separation while the safety of experiment, further be subtracted by limiting the first order
The temperature and pressure of pressure separation and second level decompression separation, improve separating effect, so that alpha-linolenic acid in linseed oil again
Refining effect significantly promoted, 90% or more can be reached.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. purifying the method for alpha-linolenic acid in a kind of linseed oil, which comprises the following steps:
Supercritical extract is carried out to linseed oil and obtains extract；
Decompression separation is carried out to the extract and obtains just alpha-linolenic acid processed；
Molecular distillation is carried out to the alpha-linolenic acid just processed and obtains alpha-linolenic acid.
2. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the overcritical extraction
It takes in step, extractant is carbon dioxide.
3. purifying the method for alpha-linolenic acid in linseed oil according to claim 2, which is characterized in that the overcritical extraction
It takes in step, the volume ratio of the linseed oil and the carbon dioxide is 1:2-4.
4. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the overcritical extraction
It takes in step, extracting pressure is 160-190 atmospheric pressure.
5. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the overcritical extraction
It takes in step, extraction temperature is 70-90 DEG C.
6. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the overcritical extraction
It takes in step, extraction time is 1-1.5 hours.
7. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the decompression separation
Step includes first order decompression separation and second level decompression separation, the extract pass sequentially through the first order decompression separation with
The second level decompression separation.
8. purifying the method for alpha-linolenic acid in linseed oil according to claim 7, which is characterized in that the first order subtracts
Pressing isolated pressure is 5-7MPa, and temperature is 35-50 DEG C.
9. purifying the method for alpha-linolenic acid in linseed oil according to claim 7, which is characterized in that the second level subtracts
Pressing isolated pressure is 3-5MPa, and temperature is 32-40 DEG C.
10. purifying the method for alpha-linolenic acid in linseed oil according to claim 1, which is characterized in that the molecule steams
It evaporates in step, vapo(u)rizing temperature is 20-25 DEG C, pressure 0.08-0.15MPa.
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Cited By (1)
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| CN110105197A (en) * | 2019-05-23 | 2019-08-09 | 河南农业大学 | A kind of overcritical method of purification and its application of pharmaceutical woody alpha-linolenic acid |
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