CN1676502A - Solanesol refining method - Google Patents
Solanesol refining method Download PDFInfo
- Publication number
- CN1676502A CN1676502A CNA2004100222338A CN200410022233A CN1676502A CN 1676502 A CN1676502 A CN 1676502A CN A2004100222338 A CNA2004100222338 A CN A2004100222338A CN 200410022233 A CN200410022233 A CN 200410022233A CN 1676502 A CN1676502 A CN 1676502A
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- CN
- China
- Prior art keywords
- buddhist nun
- eggplant buddhist
- nun alcohol
- jie
- extraction
- 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.)
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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
Abstract
This invention provides a solanesol refining method, including pre-treatment of solanesol crude cream with zymolysis and alkali saponification, and making eater key formed from solanesol and organic acid break off. Its characteristics also include: supercritical extraction purifying, decompressing separation purifying, modified extraction purifying. This invention greatly simplifies the refining procedure and improves the yield of products in order to lower the cost and overcomes many weak points of present techniques, and greatly decreases the exhaustion of industrial residues to aim the low cost, high efficiency, scalization and environmental protection. It is a method with high industrial value.
Description
Technical field
The present invention relates to a kind of preparation method of eggplant Buddhist nun alcohol, especially a kind of process for purification of eggplant Buddhist nun alcohol.
Technical background
Eggplant Buddhist nun alcohol is synthesizing coenzyme Q
10And vitamin K
2Main intermediate, also be the important intermediate of making anti-allergy agent, anti-ulcerative drug, hypolipidemic, anticarcinogen etc.Be present in mostly in animal viscera and the plant leaf, especially the content in tobacco is higher.At present, the production method of high-purity solanesol mostly adopts various column chromatography methods, is the method for a kind of purifying solanesol of 00123921 as the disclosed application number of Chinese patent literature.There is following shortcoming in these methods: 1, industrial scale is little, and production efficiency is not high.If calculate to produce 10 tons of elaboration year, then need a huge column chromatography system.2, the solvent-oil ratio in the production process is bigger, and operating process is numerous and diverse, causes production cost too high.3, the number of dropouts of eggplant Buddhist nun alcohol is big in the production process, and yield is undesirable.4, in a large number with an organic solvent, reduce the safety coefficient of product.Therefore, be necessary prior art is improved.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of cost low, product yield height, technological process is simple, and is pollution-free, the eggplant Buddhist nun alcohol process for purification of easily accomplishing scale production.
The present invention adopts super Jie's CO 2 fluid abstraction technique that faces, by changing pressure, temperature and adding fluid properties-correcting agent, the thick cream of eggplant Buddhist nun alcohol after the saponification processing is carried out stage extraction, at first the impurity stage extraction is come out, and then eggplant Buddhist nun alcohol extracted, so just can obtain highly purified eggplant Buddhist nun alcohol.The method that the present invention proposes has overcome many shortcomings of previous methods, is a kind of method that has industrial value.
The concrete technical scheme that realizes the object of the invention is: a kind of process for purification of eggplant Buddhist nun alcohol comprises and adopts enzymolysis or alkali soapization that the thick cream of eggplant Buddhist nun alcohol is carried out pre-treatment that the ester bond that the pure and mild organic acid of eggplant Buddhist nun is formed disconnects, and it is characterized in that also comprising following process steps:
Supercritical extraction removal of impurities: in through the thick cream of pretreated eggplant Buddhist nun alcohol, with per minute 1-100m
3Flow feed the super CO 2 fluid that faces Jie's state, in extracting pressure is 7.37Mpa-16Mpa, extraction temperature is 32 ℃--under 80 ℃, extracted 5 minutes-24 hours, the extracting substances that makes molecular weight and polarity in the thick cream be lower than eggplant Buddhist nun alcohol is come out and is flowed out with super Jie's CO 2 fluid that faces;
Decompression separation removal of impurities: to above-mentioned super Jie's of the facing CO 2 fluid of separating that is rich in extract, be decompressed to below the 7Mpa, make carbonic acid gas return the conventional gas state, thereby the material of extraction is separated out, the normality carbonic acid gas becomes the liquefaction attitude through condensation, reaches supercritical state after compressed again, the heat exchange and recycles;
Modification abstraction impurity removal: in through the thick cream of pretreated eggplant Buddhist nun alcohol, feed super Jie's CO 2 fluid that faces, simultaneously by the super weight percent of Jie's carbon-dioxide flow scale of construction or the 0.01-5% interpolation properties-correcting agent of volume percent of facing, to change fluidic polarity, modification extraction 5 minutes-24 hours, thus with polarity greater than the extracting substances of eggplant Buddhist nun alcohol, separate;
Extraction eggplant Buddhist nun alcohol: in extracting pressure is 10Mpa-80Mpa, and extraction temperature is under 32-180 ℃, and the thick cream through above-mentioned twice abstraction impurity removal is carried out 5 minutes-24 hours extraction, gets high-load eggplant Buddhist nun alcohol elaboration.
Described properties-correcting agent is a kind of in water, methyl alcohol, ethanol, acetone, sherwood oil, hexane, ethyl acetate, the methyl acetate or their mixture.
The method that the present invention proposes has been simplified the treating process of eggplant Buddhist nun alcohol greatly; improved product yield; thereby reduced cost; many shortcomings of existing technology have been overcome; and greatly alleviated the discharging of industry three expenses; having reached the purpose that low cost, high-level efficiency, mass-producing, environmental protection are produced, is a kind of method that has industrial value.
Description of drawings
Fig. 1 is the inventive method equipment therefor and process flow sheet.
Among the figure, 1 is receiver, and 2 is compressor, and 3 is interchanger, and 4 is extractor, and 5 is separating tank, and 6 is condenser, and 7 are properties-correcting agent interpolation pump.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, is not limited thereto but hold within the present invention.
Embodiment 1
The thick cream of the eggplant Buddhist nun that 1, will extract from tobacco leaf alcohol is put into the saponification jar, is being heated under 80 ℃ and the intense stirring condition, adds the 10%KOH aqueous solution and carries out saponification and handled 30 minutes, emits water layer after the end, keeps oil reservoir, thick cream is saponified;
2, will open interchanger 3 through in the pure thick 10 kilograms of extractors 4 of packing into of cream of the eggplant Buddhist nun that saponification is handled, regulating Heating temperature is 50 ℃, opens compressor 2, with per minute 30m
3Flow feed the super CO 2 fluid that faces Jie's state to extractor 4, make extractor 4 internal pressures reach 14Mpa, open reducing valve, the extracting substances that makes molecular weight and polarity in the phase cream be lower than eggplant Buddhist nun alcohol is come out and is flowed into separating tank 5 with super Jie's CO 2 fluid that faces, decompression back extract is separated out, the pressure of separating tank 5 maintains 4MPa, supercritical co is become enter condenser 6 after gaseous carbon dioxide is separated out extract, and flow back to receiver 1 after in condenser 6, constantly being liquefied, compressed machine 2 is squeezed into extractor again, this process continues 2 hours, opens the separating tank bleed valve, and extract is released;
3, feed super when facing Jie's CO 2 fluid again to extractor 4 by compressor 2, open properties-correcting agent and add pump 7, in extractor 4, squeeze into concentration and be 95% methyl alcohol, the amount of squeezing into is super 1% of Jie's CO 2 fluid flow that faces, continue extraction 2 hours, thus with polarity greater than the extracting substances of eggplant Buddhist nun alcohol, separate, close properties-correcting agent afterwards and add pump 7, open the bleed valve of separating tank 5, release the mixture of methyl alcohol and extract;
4, close reducing valve, the pressure that makes extractor 4 is opened reducing valve again for being upgraded to 24Mpa, and this moment, the precipitate in separating tank 5 was an eggplant Buddhist nun alcohol, and this process continues 1 hour, emits the extract in the separating tank 5---and eggplant Buddhist nun alcohol product, the purity that records product is 95%.
Embodiment 2
1, this process is with embodiment 1;
2, will open interchanger 3 through in the pure thick 10 kilograms of extractors 4 of packing into of cream of the eggplant Buddhist nun that saponification is handled, regulating Heating temperature is 80 ℃, opens compressor 2, with per minute 100m
3Flow feed the super CO 2 fluid that faces Jie's state to extractor 4, make extractor 4 internal pressures reach 16Mpa, open reducing valve, the extracting substances that makes molecular weight and polarity in the thick cream be lower than eggplant Buddhist nun alcohol is come out and is flowed into separating tank 5 with super Jie's CO 2 fluid that faces, decompression back extract is separated out, the pressure of separating tank 5 maintains 4MPa, make supercritical co become gaseous carbon dioxide and enter condenser 6, and flow back to receiver 1 after in condenser 6, constantly being liquefied, compressed machine 2 is squeezed into extractor again, this process continues 2 hours, opens the separating tank bleed valve, and extract is released;
3, feed super when facing Jie's CO 2 fluid again to extractor 4 by compressor 2, open properties-correcting agent and add pump 7, squeeze into pure water to extractor 4, the amount of squeezing into is super 0.01% of Jie's CO 2 fluid flow that faces, continue extraction 2 hours, thus with polarity greater than the extracting substances of eggplant Buddhist nun alcohol, separate, close properties-correcting agent afterwards and add pump 7, open the bleed valve of separating tank 5, release the mixture of water and extract;
4, close reducing valve, the pressure that makes extractor 4 is opened reducing valve again for being upgraded to 24Mpa, and this moment, the precipitate in separating tank 5 was an eggplant Buddhist nun alcohol, and this process continues 1 hour, emits the extract in the separating tank 5---and eggplant Buddhist nun alcohol product, the purity that records product is 93%.
Embodiment 3
1, saponification process is with embodiment 1;
2, will open interchanger 3 through in the pure thick 10 kilograms of extractors 4 of packing into of cream of the eggplant Buddhist nun that saponification is handled, regulating Heating temperature is 40 ℃, opens compressor 2, with per minute 10m
3Flow feed the super CO 2 fluid that faces Jie's state to extractor 4, make extractor 4 internal pressures reach 75Mpa, open reducing valve, the extracting substances that makes molecular weight and polarity in the thick cream be lower than eggplant Buddhist nun alcohol is come out and is flowed into separating tank 5 with super Jie's CO 2 fluid that faces, decompression back extract is separated out, the pressure of separating tank 5 maintains 5Pma, make supercritical co become gaseous carbon dioxide and enter condenser 6, and flow back to receiver 1 after in condenser 6, constantly being liquefied, compressed machine 2 is squeezed into extractor again, this process continues 4 hours, opens the separating tank bleed valve, and extract is released;
3, feed super when facing Jie's CO 2 fluid again to extractor 4 by compressor 2, open properties-correcting agent and add pump 7, in extractor 4, squeeze into concentration and be 80% acetone, the amount of squeezing into is super 5% of Jie's CO 2 fluid flow that faces, continue extraction 4 hours, thus with polarity greater than the extracting substances of eggplant Buddhist nun alcohol, separate, close properties-correcting agent afterwards and add pump 7, open the bleed valve of separating tank 5, release the mixture of acetone and extract;
4, close reducing valve, the pressure that makes extractor 4 is opened reducing valve again for being upgraded to 40Mpa, and this moment, the precipitate in separating tank 5 was an eggplant Buddhist nun alcohol, and this process continues 4 hours, emits the extract in the separating tank 5---and eggplant Buddhist nun alcohol product, the purity that records product is 96%.
Claims (2)
1, a kind of process for purification of eggplant Buddhist nun alcohol comprises and adopts enzymolysis or alkali soapization that the thick cream of eggplant Buddhist nun alcohol is carried out pre-treatment, and the ester bond that the pure and mild organic acid of eggplant Buddhist nun is formed disconnects, and it is characterized in that also comprising following process steps:
Supercritical extraction removal of impurities: in through the thick cream of pretreated eggplant Buddhist nun alcohol, with per minute 1-100m
3Flow feed the super CO 2 fluid that faces Jie's state, in extracting pressure is 7.37Mpa-16Mpa, extraction temperature is 32 ℃--under 80 ℃, extracted 5 minutes-24 hours, the extracting substances that makes molecular weight and polarity in the thick cream be lower than eggplant Buddhist nun alcohol is come out and is flowed out with super Jie's CO 2 fluid that faces;
Decompression separation removal of impurities: to above-mentioned super Jie's of the facing CO 2 fluid of separating that is rich in extract, be decompressed to below the 7Mpa, make carbonic acid gas return the conventional gas state, thereby the material of extraction is separated out, the normality carbonic acid gas becomes the liquefaction attitude through condensation, reaches supercritical state after compressed again, the heat exchange and recycles;
Modification abstraction impurity removal: in through the thick cream of pretreated eggplant Buddhist nun alcohol, feed super Jie's CO 2 fluid that faces, simultaneously by the super weight percent of Jie's carbon-dioxide flow scale of construction or the 0.01-5% interpolation properties-correcting agent of volume percent of facing, to change fluidic polarity, modification extraction 5 minutes-24 hours, thus with polarity greater than the extracting substances of eggplant Buddhist nun alcohol, separate;
Extraction eggplant Buddhist nun alcohol: in extracting pressure is 10Mpa-80Mpa, and extraction temperature is under 32-180 ℃, and the thick cream through above-mentioned twice abstraction impurity removal is carried out 5 minutes-24 hours extraction, gets high-load eggplant Buddhist nun alcohol elaboration.
2, method according to claim 1 is characterized in that described properties-correcting agent is a kind of in water, methyl alcohol, ethanol, acetone, sherwood oil, hexane, ethyl acetate, the methyl acetate or their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100222338A CN1676502A (en) | 2004-04-03 | 2004-04-03 | Solanesol refining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100222338A CN1676502A (en) | 2004-04-03 | 2004-04-03 | Solanesol refining method |
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| Publication Number | Publication Date |
|---|---|
| CN1676502A true CN1676502A (en) | 2005-10-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2004100222338A Pending CN1676502A (en) | 2004-04-03 | 2004-04-03 | Solanesol refining method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408310A (en) * | 2011-10-25 | 2012-04-11 | 广东省食品工业研究所 | Method for preparing high-purity solanesol by utilizing prepared opium paste |
| CN104072336A (en) * | 2014-06-06 | 2014-10-01 | 山东中烟工业有限责任公司 | Process for extracting solanesol |
| CN105767302A (en) * | 2016-03-07 | 2016-07-20 | 马占平 | Preparation method of camellia nitidissima nectar |
| US10405571B2 (en) | 2015-06-26 | 2019-09-10 | Altria Client Services Llc | Compositions and methods for producing tobacco plants and products having altered alkaloid levels |
-
2004
- 2004-04-03 CN CNA2004100222338A patent/CN1676502A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408310A (en) * | 2011-10-25 | 2012-04-11 | 广东省食品工业研究所 | Method for preparing high-purity solanesol by utilizing prepared opium paste |
| CN102408310B (en) * | 2011-10-25 | 2013-10-30 | 广东省食品工业研究所 | Method for preparing high-purity solanesol by utilizing prepared opium paste |
| CN104072336A (en) * | 2014-06-06 | 2014-10-01 | 山东中烟工业有限责任公司 | Process for extracting solanesol |
| US10405571B2 (en) | 2015-06-26 | 2019-09-10 | Altria Client Services Llc | Compositions and methods for producing tobacco plants and products having altered alkaloid levels |
| CN105767302A (en) * | 2016-03-07 | 2016-07-20 | 马占平 | Preparation method of camellia nitidissima nectar |
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