CN1398844A - Nervonic acid extracting and purifying production process - Google Patents
Nervonic acid extracting and purifying production process Download PDFInfo
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- CN1398844A CN1398844A CN02136802A CN02136802A CN1398844A CN 1398844 A CN1398844 A CN 1398844A CN 02136802 A CN02136802 A CN 02136802A CN 02136802 A CN02136802 A CN 02136802A CN 1398844 A CN1398844 A CN 1398844A
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- extraction
- selacholeic acid
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- selacholeic
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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
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Abstract
A production process of extracting and purifying nervonic acid includes supercritical CO2 extraction of Youguo fruit to obtain coarse nervonic acid existing in the form of glyceride; further converting the coarse nervonic acid existing in the form of glyceride into coarse nervonic acid existing in the free form; and emulsifying separation with an emulsifier to obtain high-purity nervonic acid. The said technological process is simple and has no environmental pollution, low operation temperature, low cost and high purity and yield of nervonic acid product; and may be used in industrial production.
Description
Technical field
The present invention relates to extraction, the purifying production process of a kind of production method of Selacholeic acid, particularly a kind of Selacholeic acid.
Technical background
Selacholeic acid is a kind of monounsaturated fatty acids of long-chain, mainly the form with sphingoglycolipid and sphingophospholipid is present in the white fat of human brain, in the biosynthesizing of myelin, play an important role, foreign study shows, Selacholeic acid has a significant effect to treatment demyelination (adrenoleukodystrophy disease, multiple sclerosis); We have carried out animal and human's body test-meal test to Selacholeic acid, show that Selacholeic acid has tangible promotion brain development, improve the effect of memory, but, in present Selacholeic acid production research, its separating technology adopts traditional saponification, acidifying, the technical process that purifies, this technology is used to the separation and Extraction of general lipid acid for a long time in fact, because its technology is outmoded, cause environmental pollution again, and solvent loss is big, purity is low, at the bottom of the yield and the cost height, be applied in the production of Selacholeic acid, be difficult to form produce in batches, can not produce the market advantage, can't satisfy people's lives and market demand to this product, and its synthesis technique complexity is easy to generate harmful by product in the building-up process, is difficult to separate, so, also all can't realize suitability for industrialized production at home and abroad.
Summary of the invention
Purpose foot of the present invention provides a kind of technology simple for the deficiency that solves above-mentioned technology, and free from environmental pollution, service temperature is low, effective ingredient Selacholeic acid purity height, yield height, the extraction of the Selacholeic acid that cost is low, purifying production process.
In order to achieve the above object, extraction, the purifying production process of the Selacholeic acid that the wood invention is designed, be that the oil fruit of will pulverize at first makes the thick Selacholeic acid that glyceride form exists by the CO2 supercritical extraction, the thick Selacholeic acid that glyceride form is existed transforms the thick Selacholeic acid that free form exists again, separates obtaining the high purity Selacholeic acid then by the emulsification partition method with emulsifying agent.At this, in the CO2 supercritical extraction, can use ethanol or normal hexane to do entrainment agent, directly use the overcritical equipment of CO2, by controlled temperature at 80 ℃-120 ℃, pressure under the 18-27Mpa condition, extraction makes the thick Selacholeic acid that glyceride form exists.The process that the described thick Selacholeic acid that glyceride form is existed transforms the thick Selacholeic acid of free form existence can be the thick Selacholeic acid that glyceride form exists to be added the sodium hydroxide ethanolic soln fully react, react with dilution heat of sulfuric acid then, make it fully transform the thick Selacholeic acid that free form exists, make itself and solution separating.Described emulsification partition method is that the emulsifying agent that adds in the thick Selacholeic acid that free form exists is Sodium dodecylbenzene sulfonate and ionogen and water, and controlled temperature is at 45 ℃-50 ℃, and high speed centrifugation separation then, crystallization, drying make the high purity Selacholeic acid.Its ionogen can be sal epsom or sodium-chlor.At this, the first-selected ethanol of described entrainment agent, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.The first-selected sal epsom of ionogen in the emulsification partition method, controlled temperature is at 45 ℃; Can certainly be sodium-chlor.
Supercritical extraction is to utilize the fluid under the supercritical state to be extraction agent, effective constituent from liquid or solid in the Chinese medicine ability is also carried out isolating method, CO2 becomes the first-selected supercutical fluid that uses of supercritical extraction because of the moderate characteristics of itself nontoxic, no burn into critical condition, in the supercritical extraction process, use entrainment agent, add solvent when promptly extracting with excellent dissolution performance, as ethanol, acetone etc., not only improve and keep the selectivity of extraction, and improve the solubleness of difficult volatile solute.
Use CO2 supercritical extraction Selacholeic acid, 1, operating restraint is wide, be convenient to regulate; 2, selectivity is good, can change the density of supercritical CO 2, thereby change its dissolving power to material by control pressure and temperature, extracts Selacholeic acid targetedly; 3, service temperature is low, can extract near under the room temperature condition, especially is suitable for the extraction of thermo-sensitivity composition, and extraction process is airtight, carry out continuously, has got rid of the possibility of meeting atmospheric oxidation and seeing photoresponse, and extract is stablized; 4, separate a step and finish from being extracted into, extraction back CO2 does not residue in the extract; 5, CO2 is cheap and easy to get, and can be recycled.
The emulsification partition method is utilize saturated lipid acid and unsaturated fatty acids fusing point in the mixed fatty acid different, adds emulsifying agent, ionogen, water, and controls suitable temperature, makes it to carry out liquid liquid and separates.Because saturated lipid acid and unsaturated fatty acids fusing point is different in the mixed fatty acid, carry out subzero treatment, make its temperature lower than saturated fatty acid, than unsaturated fatty acids height, make the saturated fatty acid xln, it is microgranular to be dispersed solids through Mechanical Crushing, at this moment, unsaturated fatty acids still is in a liquid state, be attached on the crystal surface of saturated fatty acid, whole mixed fatty acid is congee shape thing, therein, add synthermal tensio-active agent (Sodium dodecylbenzene sulfonate) aqueous solution and stir, contact surface is constantly increased, the saturated fatty acid solia particle is wetted, reduced the sticking power of liquid unsaturated fatty acids to the solia particle surface of saturated fatty acid, and make it break away from the solia particle surface, and at this moment Ye Tai unsaturated fatty acids just becomes many small dropletss and is scattered in the aqueous solution, and the solia particle of saturated fatty acid is separated being suspended in the aqueous solution of while also.Separate with supercentrifuge, because the proportion difference obtains the heavy phase that light phase that is made of unsaturated fatty acids and the water phase surfactant mixture that is suspending the saturated fatty acid solia particle constitute respectively.
The extraction of the resulting Selacholeic acid of the present invention, purifying production process, in extraction, purge process, realized the combination of supercritical fluid extraction and emulsification partition method, it is simple to have technology, free from environmental pollution, service temperature is low, effective ingredient Selacholeic acid purity height, the yield height, low cost and other advantages, it is to realizing the Selacholeic acid suitability for industrialized production, satisfies people's lives and market the demand of this product is had very active operation significance.
Embodiment
The present invention is further described by the following embodiment.
Embodiment 1
With the oil fruit that 300KG pulverizes, use normal hexane to do entrainment agent, with the overcritical equipment of CO2, under the condition of 90 ℃ of temperature and pressure 27Mpa, extract, make about thick Selacholeic acid glyceryl ester 130KG.Sodium hydroxide ethanolic soln with 10% fully reacts, then with the reaction of 25% dilution heat of sulfuric acid, make it fully be converted into the thick Selacholeic acid that free form exists, make itself and solution separating, add an amount of Sodium dodecylbenzene sulfonate, sodium-chlor, water then, and control suitable temperature at 50 ℃, high speed centrifugation separation, crystallization, drying, make 48.6KG purity and be 95.2% Selacholeic acid product, the rate of recovery reaches 89% embodiment 2
With the oil fruit that 500KG pulverizes, use ethanol to do entrainment agent, with the overcritical equipment of CO2, under the condition of 90 ℃ of temperature and pressure 27Mpa, extract, make about thick Selacholeic acid glyceryl ester 220KG.Sodium hydroxide ethanolic soln with 8% fully reacts, then with the reaction of 30% dilution heat of sulfuric acid, make it fully be converted into the thick Selacholeic acid that free form exists, make itself and solution separating, add an amount of Sodium dodecylbenzene sulfonate, sal epsom, water then, and control suitable temperature at 45 ℃, high speed centrifugation separation, crystallization, drying, make 75KG purity and be 96% Selacholeic acid product, the rate of recovery reaches 90%.
Claims (11)
1, a kind of extraction of Selacholeic acid, purifying production process, it is characterized in that the oil fruit of will pulverize at first makes the thick Selacholeic acid that glyceride form exists by the CO2 supercritical extraction, the thick Selacholeic acid that glyceride form is existed transforms the thick Selacholeic acid that free form exists again, separates obtaining the high purity Selacholeic acid then by the emulsification partition method with emulsifying agent.
2, the extraction of Selacholeic acid according to claim 1, purifying production process, it is characterized in that in the CO2 supercritical extraction, use ethanol or normal hexane to do entrainment agent, directly with the overcritical equipment of CO2, by controlled temperature at 80 ℃-120 ℃, pressure under the 18-27Mpa condition, extraction makes the thick Selacholeic acid that glyceride form exists.
3, the extraction of Selacholeic acid according to claim 1 and 2, purifying production process, it is characterized in that the process that the described thick Selacholeic acid that glyceride form is existed transforms the thick Selacholeic acid of free form existence is the thick Selacholeic acid that glyceride form exists to be added the sodium hydroxide ethanolic soln fully react, react with dilution heat of sulfuric acid then, make it fully transform the thick Selacholeic acid that free form exists, make itself and solution separating.
4, the extraction of Selacholeic acid according to claim 1 and 2, purifying production process, it is characterized in that described emulsification partition method is that the emulsifying agent that adds is Sodium dodecylbenzene sulfonate and ionogen and water in the thick Selacholeic acid that free form exists, and controlled temperature is at 45 ℃-50 ℃, and high speed centrifugation separation then, crystallization, drying make the high purity Selacholeic acid.
5, the extraction of Selacholeic acid according to claim 3, purifying production process, it is characterized in that described emulsification partition method is that the emulsifying agent that adds is Sodium dodecylbenzene sulfonate and ionogen and water in the thick Selacholeic acid that free form exists, and controlled temperature is at 45 ℃-50 ℃, and high speed centrifugation separation then, crystallization, drying make the high purity Selacholeic acid.
6, the extraction of Selacholeic acid according to claim 1 and 2, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.
7, the extraction of Selacholeic acid according to claim 3, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.
8, the extraction of Selacholeic acid according to claim 4, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.Ionogen in the described emulsification partition method is a sal epsom, and controlled temperature is at 45 ℃.
9, the extraction of Selacholeic acid according to claim 5, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.Ionogen in the described emulsification partition method is a sal epsom, and controlled temperature is at 45 ℃.
10, the extraction of Selacholeic acid according to claim 4, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.Ionogen in the described emulsification partition method is a sodium-chlor.
11, the extraction of Selacholeic acid according to claim 5, purifying production process is characterized in that described entrainment agent is an ethanol, during extraction controlled temperature at 90 ℃, pressure at 27Mpa.Ionogen in the described emulsification partition method is a sodium-chlor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN02136802A CN1398844A (en) | 2002-09-04 | 2002-09-04 | Nervonic acid extracting and purifying production process |
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| CN02136802A CN1398844A (en) | 2002-09-04 | 2002-09-04 | Nervonic acid extracting and purifying production process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429217B (en) * | 2008-11-27 | 2012-11-28 | 中国科学院山西煤炭化学研究所 | Phospholipid type nervonic acid and method for producing the same |
| CN105037133A (en) * | 2015-08-17 | 2015-11-11 | 浙江大学 | Method of extracting nervonic acid from malania oleifera |
| CN107343650A (en) * | 2017-06-13 | 2017-11-14 | 浙江亚林生物科技股份有限公司 | It is a kind of to be applied to adrenal gland brain protein malnutrition and the nutritional oil and preparation of old dementia patients and application |
| CN107353199A (en) * | 2017-08-10 | 2017-11-17 | 王显权 | The method of Malania Oleifera Oil separating-purifying nervonic acid |
| CN108863764A (en) * | 2018-07-20 | 2018-11-23 | 李明龙 | A kind of improvement memory improves the nervonic acid piece preparation method of sleep quality |
-
2002
- 2002-09-04 CN CN02136802A patent/CN1398844A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429217B (en) * | 2008-11-27 | 2012-11-28 | 中国科学院山西煤炭化学研究所 | Phospholipid type nervonic acid and method for producing the same |
| CN105037133A (en) * | 2015-08-17 | 2015-11-11 | 浙江大学 | Method of extracting nervonic acid from malania oleifera |
| CN107343650A (en) * | 2017-06-13 | 2017-11-14 | 浙江亚林生物科技股份有限公司 | It is a kind of to be applied to adrenal gland brain protein malnutrition and the nutritional oil and preparation of old dementia patients and application |
| CN107353199A (en) * | 2017-08-10 | 2017-11-17 | 王显权 | The method of Malania Oleifera Oil separating-purifying nervonic acid |
| CN108863764A (en) * | 2018-07-20 | 2018-11-23 | 李明龙 | A kind of improvement memory improves the nervonic acid piece preparation method of sleep quality |
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