CN103382414A - Method for supercritical extraction of alpha-linolenic acid - Google Patents
Method for supercritical extraction of alpha-linolenic acid Download PDFInfo
- Publication number
- CN103382414A CN103382414A CN201210133201XA CN201210133201A CN103382414A CN 103382414 A CN103382414 A CN 103382414A CN 201210133201X A CN201210133201X A CN 201210133201XA CN 201210133201 A CN201210133201 A CN 201210133201A CN 103382414 A CN103382414 A CN 103382414A
- Authority
- CN
- China
- Prior art keywords
- extraction
- alpha
- linolenic acid
- product
- injected
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method for supercritical extraction of alpha-linolenic acid. The method comprises the following steps of 1, carrying out extraction on linseed oil by liquid CO2 as a supercritical solvent at an extraction reactor temperature of 25-40 DEG C under the pressure of 1.01*10<7>-1.82*10<7>Pa for 1-2.5h, wherein a use ratio of the linseed oil to the liquid CO2 is 1: 1.8-3 and stainless steel balls having diameters of 0.2-0.5mm are used as dispersants and mass of the stainless steel balls is 5-10% of the total mass of the extraction system, 2, carrying out separation by a separator, and 3, carrying out rectification by a horizontal vacuum rectification device at a normal temperature at a vacuum degree of 30-90kPa to product the alpha-linolenic acid having purity of 92.4-98.6%.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of method of supercritical extraction alpha-linolenic acid.
Background technology
In recent years, along with people to the attention of health and the raising of quality of life, research and understanding to alpha-linolenic acid are progressively deepened, research discovery alpha-linolenic acid can be regulated immunity system, have reducing blood-fat, reduce blood viscosity, delay body aging, the function such as cancer-resisting, be the necessary lipid acid of human body.Alpha-linolenic acid is not medicine, and existing in edible oil is a kind of food, is a kind of healthcare products and be made into capsule.Mostly the health care product is the fish oil of animal class in the market, and pathways metabolism is not fully aware of, and alpha-linolenic acid is safer to brain, and it is to produce the favourable composition of human body such as DHA by liver metabolism, absorbs abundant.
At present, study morely to the extraction of alpha-linolenic acid both at home and abroad, as, adopt the level Four molecular distillation, obtain the alpha-linolenic acid of purity 82.3%, very high but processing condition require, be difficult to realize in masses' technique; Adopting perilla seed is the extraction process of raw material, pass through ten three step process such as filtration, saponification, washing, urea clathration, extraction, molecular distillation, very complicated; Adopt the envelope agent to extract alpha-linolenic acid, also need column chromatography, efficiency ratio is lower, complex process, performance accuracy require more high.
In the extraction process of alpha-linolenic acid, purification step finally relates to the purity of product, and in existing method, the reasonable general employing vacuum distilling of effect, make vacuum distilling gas in tower, makes filler carry out the vapour-liquid contact mass transfer by column plate and reaches the component separation.But it exists the contradiction of separating effect and Pressure Drop, and the separating effect that wants to obtain just needs many stage number or high packing layer, thereby produces large Pressure Drop, so that causes heat sensitive material to decompose or autohemagglutination.Therefore, research high-purity alpha-linolenic acid extraction process tool is of great significance.
Rectification step in the present invention has adopted horizontal vacuum rectifying tower equipment, utilizes the rational internals that can realize that repeatedly part vaporization combines with condensation, avoids the concentration back-mixing, has improved separating effect, has realized the separating-purifying of high-purity alpha-linolenic acid.
Summary of the invention
The object of the invention is to overcome shortcomings and deficiencies of the prior art, a kind of method of extracting alpha-linolenic acid from oleum lini is provided.
Technical scheme of the present invention is: take oleum lini as raw material, utilize supercutical fluid as the solvent extraction alpha-linolenic acid, be comprised of following steps.
1, supercritical extraction
CO
2Be a kind of inactive gas, safety performance is good, can effectively prevent oxidation and the decomposition of heat-sensitive substance,, selects with CO for this reason
2(liquid state) can improve linolenic biological activity effectively as supercritical solvent.With oleum lini and CO
2(liquid state) is injected in the extractive reaction still with 1:1.8 ~ 3, and extractive reaction still temperature is 25～40 ℃, and pressure is 1.01 * l0
7～1.82 * l0
7Pa utilizes Stainless Steel Ball to be dispersion agent, and size is diameter 0.2～0.5mm, and add-on is total mass 5～10%, and extraction time is 1～2.5 hour, is extracted product 1.
2, separator separates
The extraction product 1 that obtains is injected into carries out CO in separator
2Emptying or recovery separate, and are extracted product 2.
3, horizontal vacuum rectifying
The extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, normal temperature, vacuum tightness is 30-90kPa, finally obtains high-purity alpha-linolenic acid, purity 92.4 ~ 98.6%.
Alpha-linolenic acid of the present invention has good beneficial effect, product purity can reach 92.4 ~ 98.6%, has very strong physics biological activity, human body easily absorbs, easily utilizes, have good balance the body physiological function, reduce blood lipid level, suppress the effect of the cardiovascular disordeies such as thrombosis and anti-heart disorder, under normal temperature, the preservation of energy long period, do not have additive and chemical residual.
Embodiment
It is below specific embodiment.
Embodiment 1:
Get oleum lini and liquid CO
2, both (oleum lini and liquid CO
2) blending ratio is 1:1.8, is injected into preheating temperature and is in the extractive reaction still of 40 ℃, adding quality is that total mass 10%, diameter are the Stainless Steel Ball of 0.5mm, regulating extractive reaction still pressure is 1.82 * l0
7Pa, under abundant agitation condition, extraction is 1.5 hours, is extracted product 1.The extraction product 1 that obtains is injected into separator, separates, isolate CO
2Be extracted product 2.The extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, carries out separating-purifying under normal temperature, 90kPa condition, obtain purity and be 94.6% alpha-linolenic acid product.
Embodiment 2:
Get oleum lini and liquid CO
2, both (oleum lini and liquid CO
2) blending ratio is 1:2.2, is injected into preheating temperature and is in the extractive reaction still of 35 ℃, adding quality is that total mass 9%, diameter are the Stainless Steel Ball of 0.5mm, regulating extractive reaction still pressure is 1.82 * l0
7Pa, under abundant agitation condition, extraction is 1.5 hours, is extracted product 1.The extraction product 1 that obtains is injected into separator, separates, isolate CO
2Be extracted product 2.The extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, carries out separating-purifying under normal temperature, 50kPa condition, obtain purity and be 96.3% alpha-linolenic acid product.
Embodiment 3:
Get oleum lini and liquid CO
2, both (oleum lini and liquid CO
2) blending ratio is 1:2.2, is injected into preheating temperature and is in the extractive reaction still of 38 ℃, adding quality is that total mass 10%, diameter are the Stainless Steel Ball of 0.5mm, regulating extractive reaction still pressure is 1.80 * l0
7Pa, under abundant agitation condition, extraction is 2.5 hours, is extracted product 1.The extraction product 1 that obtains is injected into separator, separates, isolate CO
2Be extracted product 2.The extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, carries out separating-purifying under normal temperature, 30kPa condition, obtain purity and be 98.6% alpha-linolenic acid product.
Embodiment 4:
Get oleum lini and liquid CO
2, both (oleum lini and liquid CO
2) blending ratio is 1:2.2, is injected into preheating temperature and is in the extractive reaction still of 25 ℃, adding quality is that total mass 10%, diameter are the Stainless Steel Ball of 0.5mm, regulating extractive reaction still pressure is 1.80 * l0
7Pa, under abundant agitation condition, extraction is 2.5 hours, is extracted product 1.The extraction product 1 that obtains is injected into separator, separates, isolate CO
2Be extracted product 2.The extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, carries out separating-purifying under normal temperature, 30kPa condition, obtain purity and be 93.7% alpha-linolenic acid product.
Claims (2)
1. a method that relates to the supercritical extraction alpha-linolenic acid, is characterized in that the method is comprised of following steps: (1) supercritical extraction: with CO
2(liquid state) is as supercritical solvent, with oleum lini and CO
2(liquid state) is injected in the extractive reaction still with 1:1.8 ~ 3, and extractive reaction still temperature is 25～40 ℃, and pressure is 1.01 * l0
7～1.82 * l0
7Pa utilizes Stainless Steel Ball to be dispersion agent, and size is diameter 0.2～0.5mm, and add-on is total mass 5～10%, and extraction time is 1～2.5 hour, is extracted product 1; (2) separator separates: the extraction product 1 that obtains is injected into carries out CO in separator
2Emptying or recovery separate, and are extracted product 2; (3) horizontal vacuum rectifying: the extraction product 2 that obtains is injected in the horizontal vacuum rectifier unit, finally obtains alpha-linolenic acid, purity 92.4 ~ 98.6%.
2. the method for supercritical extraction alpha-linolenic acid according to claim 1, is characterized in that, described horizontal vacuum rectifier unit, and the rectifying condition is normal temperature, vacuum tightness is 30-90kPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210133201XA CN103382414A (en) | 2012-05-03 | 2012-05-03 | Method for supercritical extraction of alpha-linolenic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210133201XA CN103382414A (en) | 2012-05-03 | 2012-05-03 | Method for supercritical extraction of alpha-linolenic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103382414A true CN103382414A (en) | 2013-11-06 |
Family
ID=49490350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210133201XA Pending CN103382414A (en) | 2012-05-03 | 2012-05-03 | Method for supercritical extraction of alpha-linolenic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103382414A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744235A (en) * | 2015-02-28 | 2015-07-01 | 陈学沛 | Process for preparing alpha-linolenic acid |
| CN115261051A (en) * | 2022-06-24 | 2022-11-01 | 重庆工商大学 | Extraction method and equipment for oil-based drilling cuttings |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211615A (en) * | 1998-08-17 | 1999-03-24 | 清华大学 | Method for extracting linolenic acid from linseed oil |
| CN1237618A (en) * | 1999-05-13 | 1999-12-08 | 潘泰安 | Fruit seed oil obtained by supercritical CO2 extraction and its product |
| CN1317556A (en) * | 2001-04-24 | 2001-10-17 | 哈尔滨市应用技术研究所 | Process for extracting oenothera seed oil with CO2 |
| CN101812044A (en) * | 2010-05-17 | 2010-08-25 | 天津大学 | Method and system for extracting and separating natural VE from plant oil deodorizing distillate |
-
2012
- 2012-05-03 CN CN201210133201XA patent/CN103382414A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211615A (en) * | 1998-08-17 | 1999-03-24 | 清华大学 | Method for extracting linolenic acid from linseed oil |
| CN1237618A (en) * | 1999-05-13 | 1999-12-08 | 潘泰安 | Fruit seed oil obtained by supercritical CO2 extraction and its product |
| CN1317556A (en) * | 2001-04-24 | 2001-10-17 | 哈尔滨市应用技术研究所 | Process for extracting oenothera seed oil with CO2 |
| CN101812044A (en) * | 2010-05-17 | 2010-08-25 | 天津大学 | Method and system for extracting and separating natural VE from plant oil deodorizing distillate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744235A (en) * | 2015-02-28 | 2015-07-01 | 陈学沛 | Process for preparing alpha-linolenic acid |
| CN115261051A (en) * | 2022-06-24 | 2022-11-01 | 重庆工商大学 | Extraction method and equipment for oil-based drilling cuttings |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103695182B (en) | Method for supercritical extraction of linolenic acid | |
| CN101987809A (en) | Production technology for extracting purified lycopene from tomato waste residue | |
| CN105087166A (en) | Method for extracting Jasminum sambac essential oil | |
| CN103396303A (en) | Method for separating and purifying eicosapentaenoic acid and docosahexaenoic acid from micro-algal oil or fish oil | |
| CN102718774B (en) | Method for preparing artemisinin | |
| CN103382414A (en) | Method for supercritical extraction of alpha-linolenic acid | |
| CN103012351B (en) | A kind of purifying technique of natural VE | |
| CN107540683A (en) | A kind of method of knapsack reaction and rectification device production anhydrosugar alcohol | |
| CN102775327A (en) | Composite oxidizer and method for preparing high efficiency liquid chromatography eluate acetonitrile by using same | |
| CN102702122B (en) | Method for preparing tetrazine by oxidizing dihydro tetrazine | |
| CN103865642B (en) | A kind of preparation method of non-solvent high purity DHA algal oil | |
| CN107382708A (en) | A kind of extracting method of medium chain fatty acid caproic acid | |
| CN101353294A (en) | Separation and purification method of high-content resveratrol | |
| CN101103805B (en) | Industrial producing method for extracting fatty compound from melissa pollen | |
| CN103772255A (en) | Method for extracting beta-carotene from algae by low-molecule organic matters/inorganic salt aqueous two-phase extraction | |
| CN105713721A (en) | Method for concentrating DHA and EPA in fish oil | |
| CN102816054A (en) | Environment-friendly method for preparing adipic acid by catalytic oxidation | |
| CN102660378B (en) | Method for extracting natural coenzyme Q10 by using palm residue | |
| CN103965155B (en) | A kind of preparation process of natural VE | |
| CN105195206B (en) | Alkali modification molecular sieve prepares the application of CLA catalysts as corn oil conjugation | |
| CN105131059B (en) | A method of extracting geniposide from cape jasmine | |
| CN103265572B (en) | A kind of method adopted containing carboxyl/polyhydroxyl solvents extraction separation purification phosphatidylcholine | |
| CN105646342B (en) | A kind of method of quinoline in extraction and separation quinoline-biphenyl-naphthalene mixtures | |
| CN103103063B (en) | Technology for producing distilled wine by use of grape skin residue | |
| CN108047014B (en) | Method for extracting and separating coenzyme Q10 by using ionic liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131106 |