CN1216065C - Solvent extraction process of oryzanol - Google Patents
Solvent extraction process of oryzanol Download PDFInfo
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- CN1216065C CN1216065C CN 02135610 CN02135610A CN1216065C CN 1216065 C CN1216065 C CN 1216065C CN 02135610 CN02135610 CN 02135610 CN 02135610 A CN02135610 A CN 02135610A CN 1216065 C CN1216065 C CN 1216065C
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Abstract
The present invention relates to a production method for extracting oryzanol by a solvent method. Firstly, the physical refining is carried out for pretreated bran oil to eliminate free fatty acid in the oil, and alkaline methanol is added in the refined bran oil for continuous counter-current extraction; the extracted methanol mother liquid is acidified, so that oryzanol is separated by crystallization to obtain oryzanol. By the present invention, the yield of refined oil can be raised to 60 to 65% from 50 to 55%, and the oryzanol yield can be raised to 60 to 70 % from 35 to 40%. Simultaneously, the production method can reduce methanol dosage without the generation of alkali refined oil footings, no lipoid and no black lipid acid are discharged during the oryzanol extraction, and environments basically can not be polluted.
Description
Technical field
The invention belongs to thiaminogen and produce the field.
Background technology
Thiaminogen is the mixture of ring jackfruit alcohols ferulic acid ester and sterols ferulic acid ester, and it extensively is present in the cereal grass seed, is the accompaniment of lipid.The content of thiaminogen in the rice bran layer is generally 0.3～0.5%.Rice bran is when squeezing system oil, and thiaminogen is dissolved in the oil, and then mixed oil is taken out of during solvent extraction legal system oil.Hair oil extracted from rice husks two-story valley dimension cellulose content is about 1.8～2.5%.Though (as Fructus Maydis oil, wheatgerm oil, oleum lini, vegetable seed wet goods) all contains thiaminogen in a lot of vegetables oil,, be not worth so that there is industry to extract, so thiaminogen all extracts from the hair Rice pollard oil so far because its content is very low.Thiaminogen is mainly used in pharmacy.Thiaminogen starts from the eighties of last century sixties as pharmaceutical prod in the use of China, all from Japanese import.Under the still underdeveloped situation of China's economy at that time, for the import thiaminogen, only the sick total institute of Shanghai Spirit will spend twenties0000 dollars foreign exchange every year.For this reason, country organizes relevant R﹠D institutions such as Shanghai, Zhejiang to carry out the development and research of thiaminogen in sixties end, finished lab scale research in June, 70, finished middle trial production the March year July 1st again, carried out May in the same year summing up and identified, July respectively in Shanghai, the two places, Zhejiang put into serial production, and have promptly finished the development and research of thiaminogen, have formed first cover production method---the fatty acid distillation method of enrichment of domestic thiaminogen.The technical process of this method as shown in Figure 1.
Though this method has been produced the qualified product of thiaminogen, but still exist following shortcoming:
1, method complexity, production cycle are long.Begin to need 15 operation stepss altogether, five days production cycles from Rice pollard oil to producing thiaminogen.2, thiaminogen, Rice pollard oil yield are low.The thiaminogen recovery rate only is about 15%, and refining Rice pollard oil yield is 50～55% when hair oil extracted from rice husks acid value 25～30mgKOH/g.
Because the many disadvantages of aforesaid method, constituted jointly improvement group by institute of Zhejiang grain section, Shanghai grease research department and The Big Red Gate, Beijing You Chang in August, 1973, in Zhejiang, the two places, Shanghai have carried out lab scale, going into operation simultaneously in improve one's methods, Zhejiang in Beijing in 1 year, three ground, Shanghai, has formed the alkali-soluble acid analysis method of using till today.Improve one's methods and compare characteristics such as having method is simple, constant product quality with former fatty acid distillation method, and obtain in 1978 national science conference award.The technical process of this method as shown in Figure 2.Though this improved alkali-soluble acid analysis method is compared with former fatty acid distillation method bigger progress has been arranged, the thiaminogen recovery rate also only reaches 30～35%, and refining of crude rice bran oil rate and former method are suitable substantially.Because being arranged, slubbing alkali refining, the molten filtration of alkali and three operations of Methanol Recovery discharge waste materials such as oil foot, lipoid and black acid in alkali-soluble acid analysis method production method, these waste materials are processed into useful lipid acid also needs to consume a large amount of mineral acids, alkali, can cause certain environmental pollution.
Summary of the invention
The object of the present invention is to provide the production method of the high solvent extraction thiaminogen of a kind of yield.
For achieving the above object, the present invention adopts following technical scheme: a kind of production method of solvent extraction thiaminogen, it is characterized in that, at first the rice bran crude oil is carried out pre-treatment, pretreated oil extracted from rice husks is carried out physical refining to remove free lipid acid in the oil, add alkaline methanol in the oil extracted from rice husks after refining and carry out continuous countercurrent extraction, add acid in the methanol mother liquor after extraction wherein contained thiaminogen crystallization is separated out, get thiaminogen after the separation.
After isolating thiaminogen, it is further washed and negative pressure drying, with the purity of further raising thiaminogen.
Described pre-treatment comprise take off cured, come unstuck, decolouring, filtration step, the temperature of taking off in the cured step is 0～30 ℃, the temperature in the step of coming unstuck is 30～90 ℃, the temperature in the decolouring step is 60～150 ℃.
In the add-on of counter-current extraction step neutral and alkali methyl alcohol is 1.5～8 times of oil mass, and extraction temperature is 10～50 ℃, and extraction times is 2～8 times, and the time is 5～60 minutes.
Temperature in the physical refining step is 220～280 ℃, absolute pressure 10～500Pa, and the physical refining time is 3～60 minutes, the oil extracted from rice husks acid value after the refining is below 0.6.
PH value is 3～7 in the acid out step, and added acid is hydrochloric acid, phosphoric acid or citric acid, and temperature is 10～50 ℃, and the time is 1～4 hour.
Oil extracted from rice husks after the extraction is through washing, the drying Rice pollard oil that gets product after removing residual solvent.
The present invention is applied to physical refining deacidification method in the thiaminogen production method first, avoided the soap stock that alkali refining produces in the current methods to make thiaminogen loss about 20%, owing to adopt physical refining deacidification method that the more existing alkali-soluble acid analysis method of yield of refining Rice pollard oil is had increased significantly, the essential oil yield brings up to 60～65% by original 50～55%, the thiaminogen unit cost production is reduced greatly, finished product (thiaminogen in the unit raw material, the refining Rice pollard oil) goes out rate and be greatly improved, limited raw material is utilized fully than alkali-soluble acid analysis method.The present invention is a solvent with the alkaline methanol, takes the multiple-effect counter-current extraction to produce thiaminogen, has reduced methanol usage, and methanol usage be oily heavy 2～8 times, makes the yield of thiaminogen bring up to 60～70% by 35～40% of current methods.The present invention does not have the alkali refining oil foot and produces owing to adopted physical refining deacidification method when oil refining, and the thiaminogen extraction does not have lipoid and black acid to discharge yet, and can not pollute environment basically.
Description of drawings
Fig. 1 is a process flow sheet of producing thiaminogen in the prior art with the fatty acid distillation method of enrichment;
Fig. 2 is a process flow sheet of producing thiaminogen in the prior art with the alkali-soluble acid analysis method.
Embodiment
The rice bran crude oil at first removes contained wax in the oil, 0～30 ℃ of temperature.Come unstuck then, 30～90 ℃ of temperature, aquation is removed phosphatide.Degummed oil adds gac or carclazyte adsorption bleaching, 60～150 ℃ of temperature, and oil extracted from rice husks must decolour after the filtration.Remove free lipid acid in the oil, 220～280 ℃ of temperature, absolute pressure 10～500Pa, 3～60 minutes time through physical refining.Oil extracted from rice husks acid value behind the physical refining reaches below 0.6.Oil extracted from rice husks after concise is added alkaline methanol carry out continuous countercurrent extraction, the alkaline methanol add-on is 1.5～8 times of oil mass, and temperature is 10～50 ℃, and extraction times is 2～8 times.Time is 5～60 minutes.Oil extracted from rice husks after the extraction removes through washing, drying and residually obtains the rice finished product oil extracted from rice husks after molten.Contain thiaminogen in the methanol mother liquor after the extraction, in mother liquor, add acid the thiaminogen crystallization is separated out, get thick thiaminogen after the separation.Can add hydrochloric acid, phosphoric acid, citric acid etc. in the acid out, pH value is 3～7, and temperature is 10～50 ℃, and the time is 1～4 hour.Thick thiaminogen gets smart thiaminogen through washing, vacuum-drying.The total recovery rate of smart thiaminogen can be up to 60～70%.Purity can reach more than 98%, reaches the high-quality drug standard.Waste liquor behind the acid out reclaims methyl alcohol and can be recycled.
Claims (7)
1, a kind of production method of solvent extraction thiaminogen, it is characterized in that, at first the rice bran crude oil is carried out pre-treatment, pretreated oil extracted from rice husks is carried out physical refining to remove free lipid acid in the oil, add alkaline methanol in the oil extracted from rice husks after refining and carry out continuous countercurrent extraction, add acid in the methanol mother liquor after extraction wherein contained thiaminogen crystallization is separated out, get thiaminogen after the separation.
2, the method for claim 1 is characterized in that, after isolating thiaminogen, it is further washed and negative pressure drying.
3, method as claimed in claim 1 or 2, it is characterized in that, described pre-treatment comprise take off cured, come unstuck, decolouring, filtration step, the temperature of taking off in the cured step is 0～30 ℃, temperature in the step of coming unstuck is 30～90 ℃, and the temperature in the decolouring step is 60～150 ℃.
4, method as claimed in claim 1 or 2 is characterized in that, is 1.5～8 times of oil mass in the add-on of counter-current extraction step neutral and alkali methyl alcohol, and extraction temperature is 10～50 ℃, and extraction times is 2～8 times, and the time is 5～60 minutes.
5, method as claimed in claim 1 or 2 is characterized in that, the temperature in the physical refining step is 220～280 ℃, absolute pressure 10～500Pa, and the physical refining time is 3～60 minutes, the oil extracted from rice husks acid value after the refining is below 0.6.
6, method as claimed in claim 1 or 2 is characterized in that, pH value is 3～7 in the acid out step, and added acid is hydrochloric acid, phosphoric acid or citric acid, and temperature is 10～50 ℃, and the time is 1～4 hour.
7, method as claimed in claim 1 or 2 is characterized in that, the oil extracted from rice husks after the extraction is through washing, the drying Rice pollard oil that gets product after removing residual solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135610 CN1216065C (en) | 2002-09-27 | 2002-09-27 | Solvent extraction process of oryzanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135610 CN1216065C (en) | 2002-09-27 | 2002-09-27 | Solvent extraction process of oryzanol |
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| CN1485330A CN1485330A (en) | 2004-03-31 |
| CN1216065C true CN1216065C (en) | 2005-08-24 |
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| CN 02135610 Expired - Fee Related CN1216065C (en) | 2002-09-27 | 2002-09-27 | Solvent extraction process of oryzanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI715503B (en) * | 2020-06-04 | 2021-01-01 | 台灣中油股份有限公司 | Method for preparing oryzanol |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103525545A (en) * | 2013-10-21 | 2014-01-22 | 江苏丹绿食品股份有限公司 | Manufacturing process of rice essential oil |
| CN103694300B (en) * | 2013-12-10 | 2015-09-30 | 苏州谷力生物科技有限公司 | A kind of method extracting thiaminogen from chaff dregs of rice waste grease |
| CN105131073A (en) * | 2015-07-27 | 2015-12-09 | 中国科学院长春应用化学研究所 | Combined production method of extraction of oryzanol and squalene from rice bran directly |
| US20220162258A1 (en) * | 2020-07-29 | 2022-05-26 | Cpc Corporation, Taiwan | Method for Obtaining Gamma-Oryzanol |
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2002
- 2002-09-27 CN CN 02135610 patent/CN1216065C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI715503B (en) * | 2020-06-04 | 2021-01-01 | 台灣中油股份有限公司 | Method for preparing oryzanol |
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| CN1485330A (en) | 2004-03-31 |
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