CN1091107C - Method for raising natural vitamin E concentrate transparency and fluidity - Google Patents
Method for raising natural vitamin E concentrate transparency and fluidity Download PDFInfo
- Publication number
- CN1091107C CN1091107C CN99125744A CN99125744A CN1091107C CN 1091107 C CN1091107 C CN 1091107C CN 99125744 A CN99125744 A CN 99125744A CN 99125744 A CN99125744 A CN 99125744A CN 1091107 C CN1091107 C CN 1091107C
- Authority
- CN
- China
- Prior art keywords
- natural
- concentrate
- transparency
- enriched material
- temperature
- 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.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for increasing the transparency and the fluidity of natural vitamin E concentrate. After organic solvents, such as ketone, alcohol, hydrocarbon, etc., are mixed with natural VE concentrate according to certain proportion and are dissolved at the temperature of 30 DEG C to 80 DEG C, the temperature is slowly reduced to 10 DEG C to 25 DEG C below zero; after standing is carried out for 10 to 60 hours, the mixture of the organic solvents and the natural VE concentrate is filtered, and after the solvents are evaporated by the decompression of mother liquid, the natural VE is obtained. The present invention has the advantages of simple process, clarifying and transparent natural VE, high fluidity and obviously increased content. The method can not only remove impurities in the natural VE concentrate, but also remove impurities in the methyl ester mixture during the cold separation stage of pretreatment of raw materials, and the method adapts to industrialized production.
Description
Technical field:
The present invention relates to improve natural VE (VE) concentrate transparency and mobile method, relate in particular to solvent method and remove impurity such as higher fatty acid fat in the natural VE, thereby improve natural VE concentrate transparency and mobile technology, belong to the separation engineering technical field.
Background technology:
Natural VE has many important physical functions, and human body is had no side effect, and the security of life-time service is far above synthetic VE, and therefore, in industries such as food, dietary supplements and makeup, natural VE is subjected to consumers in general's favor as functional additive.In the prior art, the preparation of natural VE mainly is to adopt technology such as vacuum distilling, molecular distillation to extract concentrated obtaining from the processed side product of refined vegetable oil.Its general technological process is: raw material → esterification → esterification product → cold analysis → filtration → sterols separated → filtrate (esterification mixture) → vacuum distilling or molecular distillation → natural VE enriched material.But it is very poor with mobile property of natural VE enriched material and transparency that existing extraction concentration technique obtains.According to publication number CN1074217A, the natural VE enriched material product that CN1034367A obtains is opaque at normal temperatures, just begins to solidify, do not flow under 22 ℃, has a strong impact on natural VE product quality and use.Cause VE enriched material product opaque, easily curing, immobilising major cause are because in the course of processing, some materials such as high-grade aliphatic ester that have than high-solidification point still are present in the natural VE product.In the cold analysis process of raw materials pretreatment, because mixtures of methyl esters zero pour height, the cold analysis temperature can not be too low, generally at 5～10 ℃, thereby makes the bigger materials such as high-grade aliphatic ester of solubleness still be retained in the mixtures of methyl esters, because these materials and VE have close boiling point, therefore, when vacuum distilling or molecular distillation, these materials are distilled out with VE, open very difficult the branch with VE, thereby influence the quality of natural VE.Like this, because the existence of these impurity, one side can not effectively improve the content of natural VE, on the other hand, makes the natural VE enriched material just be muddy, opaque, mobile poor, easily curing at normal temperatures.
Summary of the invention:
The objective of the invention is at above-mentioned the deficiencies in the prior art, a kind of method of improving mobile property of natural VE enriched material and transparency and can improving natural VE content simultaneously is provided, makes it simple, production cost is low, not needing increases facility investment in addition, is applicable to suitability for industrialized production.
For realizing such purpose, present method adopts a kind of organic solvent, according to the dissolubility difference of materials such as VE and high-grade aliphatic ester in solvent, promptly according to VE a temperature range can be arbitrarily and solvent miscible, and the materials such as high-grade aliphatic ester in the VE enriched material can be miscible with solvent in the high temperature section of this temperature range, and, carry out separating of materials such as VE and high-grade aliphatic ester in low-temperature zone unmixing and the characteristic separated out of precipitation.The organic solvent that the present invention adopts can be ketone, alcohols and hydro carbons and their mixture, preferably low-carbon (LC) ketone, low-carbon alcohol and lower carbon number hydrocarbons.
Preferred acetone or alcohol of the present invention or hexane, with the ratio of natural VE enriched material in 1: 1～6: 1, under 30 ℃～80 ℃ (being preferably 40 ℃～60 ℃), behind the mixed dissolution, slowly reduce the temperature to 10 ℃～-25 ℃, left standstill 10～70 hours, then, by the conventional filtration method mother liquor and precipitation are separated, mother liquor obtains the natural VE of clear after decompression steams solvent, it does not solidify under 0 ℃, good fluidity.In addition, on original basis, VE content can improve 5～15 percentage points.In treating processes,, then help filtering if cooling temperature is lower, time of repose is long.
The present invention also is applicable to the raw materials pretreatment process, i.e. the separating of materials such as high-grade aliphatic ester in the mixtures of methyl esters that raw material and methyl alcohol reaction finishes and carries out obtaining after the sterols separated.With solvent and mixtures of methyl esters at a certain temperature, after miscible by a certain percentage, slowly reduce temperature, species precipitate such as high-grade aliphatic ester are separated out, after with ordinary method mother liquor and precipitation being separated then, again the mixtures of methyl esters that obtains is carried out underpressure distillation or molecular distillation.
The present invention is simple, and is effective, and the natural VE that obtains clear still under 0 ℃ does not solidify, good fluidity, and also VE content can improve 5～15 percentage points.Technological operation of the present invention is easy, need not drop into new equipment, production cost is low, be not only applicable to remove the impurity such as high-grade aliphatic ester that are present in the natural VE enriched material, also be applicable to the impurity of removing in the mixtures of methyl esters that obtains in the cold analysis stage of raw materials pretreatment process such as high-grade aliphatic ester, can suitability for industrialized production.
Embodiment:
Below by specific embodiment technical scheme of the present invention and the effect that reaches thereof are further described.
Embodiment 1: solidify under the room temperature flow, opaque, VE content is 41.0% natural VE enriched material 100 grams, according to a conventional method with 200 gram acetone be heated to 40 ℃ miscible after, slowly be cooled to 0 ℃, leave standstill suction filtration after 24 hours, mother liquor and precipitation are separated, must precipitate 15 grams, after the mother liquor decompression steams acetone, get VE enriched material 76 grams, VE content 47.5%, the rate of recovery 88.0%, this VE enriched material does not solidify good fluidity at 0 ℃ of following clear.
Embodiment 2: solidify under the room temperature flow, opaque, VE content is 52.0% natural VE enriched material 100 grams, according to a conventional method with 300 gram acetone be heated to 45 ℃ miscible after, slowly be cooled to-15 ℃, leave standstill suction filtration after 54 hours, mother liquor and precipitation are separated, must precipitate 18 grams, after the mother liquor decompression steams acetone, get VE enriched material 73 grams, VE content 66.0%, the rate of recovery 92.6%, this VE enriched material does not solidify good fluidity at 0 ℃ of following clear.
Embodiment 3: solidify under the room temperature flow, opaque, VE content is 42.0% natural VE enriched material 100 grams, according to a conventional method with 300 gram ethanol be heated to 55 ℃ miscible after, slowly be cooled to-10 ℃, leave standstill suction filtration after 50 hours, mother liquor and precipitation are separated, must precipitate 17 grams, after the mother liquor decompression steams ethanol, get VE enriched material 73 grams, VE content 53.0%, the rate of recovery 92.1%, this VE enriched material does not solidify good fluidity at 0 ℃ of following clear.
Claims (2)
1, a kind of natural vitamin E concentrate transparency and mobile method of improving, it is characterized in that adopting organic solvent-acetone or ethanol, with the ratio of natural VE enriched material in 1: 1～6: 1, behind 30 ℃～80 ℃ following mixed dissolutions, slowly reduce the temperature to 10 ℃～-25 ℃, leave standstill 10～70 hours after-filtration, mother liquor and precipitation are separated, mother liquor obtains natural VE after decompression steams solvent.
2, a kind of as said raising natural vitamin E concentrate transparency of claim 1 and mobile method, the mixed dissolution temperature that it is characterized in that solvent and natural VE enriched material is 40 ℃～60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99125744A CN1091107C (en) | 1999-12-24 | 1999-12-24 | Method for raising natural vitamin E concentrate transparency and fluidity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99125744A CN1091107C (en) | 1999-12-24 | 1999-12-24 | Method for raising natural vitamin E concentrate transparency and fluidity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1263096A CN1263096A (en) | 2000-08-16 |
| CN1091107C true CN1091107C (en) | 2002-09-18 |
Family
ID=5284154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99125744A Expired - Fee Related CN1091107C (en) | 1999-12-24 | 1999-12-24 | Method for raising natural vitamin E concentrate transparency and fluidity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1091107C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012351B (en) * | 2012-09-03 | 2015-09-02 | 宁波大红鹰生物工程股份有限公司 | A kind of purifying technique of natural VE |
| CN105585552B (en) * | 2014-11-13 | 2018-06-26 | 丰益(上海)生物技术研发中心有限公司 | A kind of decoloration purification process of vitamin E |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034367A (en) * | 1987-09-17 | 1989-08-02 | 清华大学 | The technology of separating VE from foots of refining vegetable oil |
| JPH02264721A (en) * | 1989-04-05 | 1990-10-29 | Tama Seikagaku Kk | Production of powdery vitamin e |
| JPH0570793A (en) * | 1991-09-10 | 1993-03-23 | Nissei Baadeishie Kk | Granular lipid composition |
| CN1074217A (en) * | 1993-01-14 | 1993-07-14 | 清华大学 | From the vegetable oil refining by product, extract the novel process of vitamin-E and sterol |
| JPH10298074A (en) * | 1997-04-25 | 1998-11-10 | Grelan Pharmaceut Co Ltd | Composition containing vitamins |
-
1999
- 1999-12-24 CN CN99125744A patent/CN1091107C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034367A (en) * | 1987-09-17 | 1989-08-02 | 清华大学 | The technology of separating VE from foots of refining vegetable oil |
| JPH02264721A (en) * | 1989-04-05 | 1990-10-29 | Tama Seikagaku Kk | Production of powdery vitamin e |
| JPH0570793A (en) * | 1991-09-10 | 1993-03-23 | Nissei Baadeishie Kk | Granular lipid composition |
| CN1074217A (en) * | 1993-01-14 | 1993-07-14 | 清华大学 | From the vegetable oil refining by product, extract the novel process of vitamin-E and sterol |
| JPH10298074A (en) * | 1997-04-25 | 1998-11-10 | Grelan Pharmaceut Co Ltd | Composition containing vitamins |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1263096A (en) | 2000-08-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7572376B2 (en) | Process for producing 1,3-propanediol | |
| CN1837201A (en) | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea | |
| CN107216252B (en) | Preparation method of high-content Omega-3 fatty acid ethyl ester | |
| CN105038948A (en) | Supercritical extraction method of grape seed oil | |
| CN1206245C (en) | Algae extracting process | |
| CN1091107C (en) | Method for raising natural vitamin E concentrate transparency and fluidity | |
| CN1064951C (en) | Method for refining long-chain bibasic acid | |
| CN1305882C (en) | Technique for producing soya bean lecithin | |
| CN111534374B (en) | Method for improving content of nutrient components of grease and grease refining system for method | |
| CN101417917B (en) | Method for preparing high-purity all-trans lycopene crystal | |
| CN103012351A (en) | Technology for purifying natural vitamin E | |
| CN103787864A (en) | Method for extracting DHA (Docosahexaenoic acid) from marine microalgae fermentation liquor | |
| CN108164415B (en) | Method for completely separating EPA and DHA from fish oil | |
| CN111072469A (en) | Method for extracting natural nervonic acid | |
| CN110627802B (en) | Method for extracting sesame lignan from by-product generated in sesame oil production | |
| CN108753455A (en) | A method of extracting high-purity linseed oil using molecularly distilled | |
| CN105349252A (en) | Method for separating high-purity rice bran crude oil from rice bran | |
| CN115028530A (en) | Extraction process of long-chain dicarboxylic acid and long-chain dicarboxylic acid product | |
| CN101747657A (en) | Industrial method for improving quality of capsicum red pigment | |
| CN1789236A (en) | Purification method of 15N-L-arginine | |
| CN110550608A (en) | Method for purifying biological sulfur | |
| CN107557148B (en) | Method for extracting crude shrimp sauce from Antarctic krill | |
| CN112646663B (en) | Method for enriching, separating and purifying linoleic acid in sunflower seed oil | |
| CN115715559B (en) | Method for enriching DHA in grease | |
| CN116751110A (en) | Method for extracting inositol from inositol mother liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |