CN103588617A - Extraction method for high purity octacosanol from rice bran - Google Patents

Extraction method for high purity octacosanol from rice bran Download PDF

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Publication number
CN103588617A
CN103588617A CN201210298843.5A CN201210298843A CN103588617A CN 103588617 A CN103588617 A CN 103588617A CN 201210298843 A CN201210298843 A CN 201210298843A CN 103588617 A CN103588617 A CN 103588617A
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China
Prior art keywords
wax
extraction
rice bran
policosanol
refining
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Pending
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CN201210298843.5A
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Chinese (zh)
Inventor
龙蕾
安海燕
史洁
魏志杰
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Tianjin Naer Biotechnology Co Ltd
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Tianjin Naer Biotechnology Co Ltd
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Priority to CN201210298843.5A priority Critical patent/CN103588617A/en
Publication of CN103588617A publication Critical patent/CN103588617A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
    • C07C29/92—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound by a consecutive conversion and reconstruction
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides an extraction method for high purity octacosanol from rice bran. According to the method, the SF-CO2 extraction technology is used to extract grease and wax in rice bran, ultrasonic hydrolysis is employed for refining of bran wax, alcohol-acid separation is carried out by using a transesterification method, and the molecular distillation technology and high vacuum fractionation are utilized for refining and purification of octacosanol. The extraction method for octacosanol from rice bran is characterized by comprising the following steps: extracting grease and wax in rice bran by using the SF-CO2 extraction technology; refining bran wax through ultrasonic hydrolysis; carrying out alcohol-acid separation by using the transesterification method; refining octacosanol by using the molecular distillation technology and high vacuum fractionation; and preparing an octacosanol product with purity of more than 95%. The method has good application prospects.

Description

In a kind of rice bran, extract the extracting method of high purity policosanol
(1) technical field:
The invention provides a kind of method of extracting high purity policosanol from rice bran, utilize SF-CO 2grease and wax in abstraction technique extraction rice bran, adopt ultrasonic wave hydrolysis to carry out the refining of chaff wax, then carry out alkyd separation with ester-interchange method, and application molecular distillation technique and high-vacuum fractionation are refined the method for purifying to policosanol.
(2) background technology:
Rice bran is a kind of highly beneficial food resource with being worth, wherein containing abundant grease and wax.Chaff wax is the main raw material source of extracting high-carbon fatty alcohol, has abundant policosanol, and it is the natural product with remarkable anti-fatigue effect.
SF-CO 2extraction has increasingly extensive application in fields such as food, makeup, the extraction of medical active ingredient of natural plant and oil soil.In the process of extraction, the ultrasonic wave hydrolysis that the present invention uses, ester-interchange method separation, application molecular distillation technique and high-vacuum fractionation technology are all up-to-date industrial technologies, are described as best process means.
(3) summary of the invention:
The method of extracting policosanol at the rice bran that the object of the present invention is to provide a kind of the best, wherein adopts SF-CO 2refining, the ester-interchange method that in extraction rice bran, chaff wax is carried out in grease and wax, ultrasonic wave hydrolysis carries out that alkyd is separated, application molecular distillation technique and high-vacuum fractionation are refined policosanol.Extracting method percentage extraction of the present invention is high, obviously improve product quality, successfully solved the hydrolysis difficult problem of chaff wax, under Ultrasonic Conditions, transesterification reaction is strengthened, shortened the reaction times, having reduced distillation number of times, improved reaction product yield and policosanol content, is a kind of extracting method with applications well prospect.
Technical scheme of the present invention: a kind of rice bran of the best extracts the method for policosanol, it is characterized in that adopting grease and wax, ultrasonic wave technology for hydrolyzing in supercritical liquid extraction technique extraction rice bran carry out chaff wax refining, alkyd is separated, molecular distillation technique and high-vacuum fractionation technology are refined policosanol, has obtained the more than 95% high purity policosanol of purity.
Above-mentioned said extraction policosanol method is: that in extraction rice bran, grease and wax adopt is SF-CO 2extraction, hydrolysis carry out chaff wax refining employing be ultrasonic wave hydrolysis, alkyd is separated, and what adopt is ester-interchange method, what distillation technique and fractionation refine employing to policosanol is molecular distillation technique and high-vacuum fractionation.
Rice bran extract the method for policosanol, it is characterized in that it comprises the following steps:
1) SF-CO 2grease and wax in extraction rice bran: adopt extracting pressure 40～60MPa, 35～45 ℃ of extraction temperature, extraction time 40～60min.
2) the refining of chaff wax carried out in ultrasonic wave hydrolysis: take a certain amount of 1) in grease and wax be placed in beaker, after add appropriate distilled water and alkali lye, ultrasound probe is placed in to beaker and reacts certain hour, measure its percent hydrolysis;
The above-mentioned said reaction times is 40-60min.
3) ester-interchange method carries out alkyd separation: adopt sonochemistry transesterify, from 2) extract high-carbon fatty alcohol mixture in refining rice bran wax, strict control extracted temperature, solvent species, solvent ratio, extraction time;
Above-mentioned ultrasonic power 150～250W, 50～70 ℃ of temperature of reaction, ceryl alcohol is than 1: 9～11, reaction times 5～7h, catalyst levels 1～2%.
4) application molecular distillation technique and high-vacuum fractionation are refined policosanol: first will carry out the pre-treatment of fatty alcohol acetylation method, then add in Distallation systm.In fractionation by distillation process, thin film evaporation actuator temperature is 160～180 ℃, and molecular distillation actuator temperature is 200～220 ℃.
5) preparation of high purity policosanol.
Superiority of the present invention is: 1, extracting method percentage extraction is high, obviously improves product quality; 2, successfully solved the hydrolysis difficult problem of chaff wax; 3, under Ultrasonic Conditions, transesterification reaction is strengthened; 4, shorten the reaction times, reduced distillation number of times, improved separation efficiency, greatly shortened disengaging time; 5, improve product quality, have a extensive future; It is a kind of extracting method with applications well prospect.
(4) embodiment:
Rice bran extract the method for policosanol, adopt grease and wax, hydrolysis in extraction rice bran carry out chaff wax refining, alkyd is separated, distillation technique and fractionation are refined policosanol.
This extracting method main process is as follows:
1) SF-CO 2grease and wax in extraction rice bran: adopt extracting pressure 50MPa, 40 ℃ of extraction temperature, extraction time 50min.
2) the refining of chaff wax carried out in ultrasonic wave hydrolysis: take a certain amount of 1) in grease and wax be placed in beaker, after add appropriate distilled water and alkali lye, ultrasound probe is placed in to beaker and reacts 50min, measure its percent hydrolysis.
3) ester-interchange method carries out alkyd separation: adopt sonochemistry transesterify, from 2) extract high-carbon fatty alcohol mixture in refining rice bran wax, ultrasonic power 200W wherein, 60 ℃ of temperature of reaction, ceryl alcohol is than 1: 10, reaction times 6h, catalyst levels 1.5%.
4) application molecular distillation technique and high-vacuum fractionation are refined policosanol: first will carry out the pre-treatment of fatty alcohol acetylation method, then add in Distallation systm.In fractionation by distillation process, thin film evaporation actuator temperature is 170 ℃, and molecular distillation actuator temperature is 210 ℃.
5) adopting high-vacuum fractionation technology to prepare purity is 99.2% policosanol.
Superiority of the present invention is: 1, improve percentage extraction more than 10%, obviously improve product quality; 2, successfully solved the hydrolysis difficult problem of chaff wax; 3,, under Ultrasonic Conditions, ester interchanged prod yield has increased more than 9%; 4, shorten the reaction times, reduced distillation number of times, improved separation efficiency more than 8%, greatly shortened disengaging time; 5, having obtained highly purified policosanol, is a kind of extracting method with applications well prospect.

Claims (3)

1. the invention provides a kind of method of extracting high purity policosanol from rice bran, utilize SF-CO 2grease and wax in abstraction technique extraction rice bran, adopt ultrasonic wave hydrolysis to carry out the refining of chaff wax, then carry out alkyd separation with ester-interchange method, and application molecular distillation technique and high-vacuum fractionation are refined the method for purifying to policosanol.
2. according to the said extraction policosanol of claim 1 method, be: that in extraction rice bran, grease and wax adopt is SF-CO 2extraction, hydrolysis carry out chaff wax refining employing be ultrasonic wave hydrolysis, alkyd is separated, and what adopt is ester-interchange method, it is to apply molecular distillation technique and high-vacuum fractionation that distillation technique and fractionation refine what adopt to policosanol.
3. according to a kind of said method of extracting policosanol from rice bran of claim 2, it is characterized in that it comprises the following steps:
1) SF-CO 2grease and wax in extraction rice bran: adopt extracting pressure 40～60MPa, 35～45 ℃ of extraction temperature, extraction time 40～60min.
2) the refining of chaff wax carried out in ultrasonic wave hydrolysis: take a certain amount of 1) in grease and wax be placed in beaker, after add appropriate distilled water and alkali lye, ultrasound probe is placed in to beaker and reacts certain hour.Measure its percent hydrolysis;
The above-mentioned said reaction times is 40-60min.
3) ester-interchange method carries out alkyd separation: adopt sonochemistry transesterify, from 2) extract high-carbon fatty alcohol mixture in refining rice bran wax, strict control extracted temperature, solvent species, solvent ratio, extraction time;
Above-mentioned ultrasonic power 150～250W, 50～70 ℃ of temperature of reaction, ceryl alcohol is than 1: 9～11, reaction times 5～7h, catalyst levels 1～2%.
4) application molecular distillation technique and high-vacuum fractionation are refined policosanol: first will carry out the pre-treatment of fatty alcohol acetylation method, then add in Distallation systm.In fractionation by distillation process, thin film evaporation actuator temperature is 160～180 ℃, and molecular distillation actuator temperature is 200～220 ℃.
5) preparation of high purity policosanol.
CN201210298843.5A 2012-08-16 2012-08-16 Extraction method for high purity octacosanol from rice bran Pending CN103588617A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210298843.5A CN103588617A (en) 2012-08-16 2012-08-16 Extraction method for high purity octacosanol from rice bran

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210298843.5A CN103588617A (en) 2012-08-16 2012-08-16 Extraction method for high purity octacosanol from rice bran

Publications (1)

Publication Number Publication Date
CN103588617A true CN103588617A (en) 2014-02-19

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106306301A (en) * 2016-08-19 2017-01-11 鸿进商贸有限公司 Candy product and preparation method thereof
CN108358757A (en) * 2018-04-17 2018-08-03 叶盛权 The extracting method of n-octacosanol in a kind of seawater rice
CN109180426A (en) * 2018-06-28 2019-01-11 益倍（常州）生物医药科技有限公司 A kind of preparation method of rice bran higher aliphatic
CN112225638A (en) * 2020-09-28 2021-01-15 浙江得乐康食品股份有限公司 Process for extracting octacosanol from rice bran wax

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106306301A (en) * 2016-08-19 2017-01-11 鸿进商贸有限公司 Candy product and preparation method thereof
CN108358757A (en) * 2018-04-17 2018-08-03 叶盛权 The extracting method of n-octacosanol in a kind of seawater rice
CN109180426A (en) * 2018-06-28 2019-01-11 益倍（常州）生物医药科技有限公司 A kind of preparation method of rice bran higher aliphatic
CN112225638A (en) * 2020-09-28 2021-01-15 浙江得乐康食品股份有限公司 Process for extracting octacosanol from rice bran wax

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Application publication date: 20140219