CN1107110C - Supercritical carbon dioxide extraction process of grape seed oil and cyanine oligomer - Google Patents
Supercritical carbon dioxide extraction process of grape seed oil and cyanine oligomer Download PDFInfo
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- CN1107110C CN1107110C CN99111574A CN99111574A CN1107110C CN 1107110 C CN1107110 C CN 1107110C CN 99111574 A CN99111574 A CN 99111574A CN 99111574 A CN99111574 A CN 99111574A CN 1107110 C CN1107110 C CN 1107110C
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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
The present invention relates to a method for extracting grape seed oil and a procyanidine oligomer by supercritical carbon dioxide, which comprises two steps: in the first step, grape seed oil is extracted under the conditions of the pressure of 25 to 29MPa and the temperature of 60 DEG C of an extraction kettle by control; in the second step, a modifying agent is added to an extracting agent, namely carbon dioxide, wherein the modifying agent comprises 70 parts of acetone and 30 parts of water, and the rate of the CO2 to the modifying agent is from 4 to 1 by quantity. The yields of two products extracting procyanidine both reach 15% and 14%. The carbon dioxide and the modifying agent of the steps can be used circularly to generate no pollution to the environment, which changes the traditional organic solvent method with pollution.
Description
The present invention relates to a kind of method of extracting cyanine oligomer from Semen Vitis viniferae, particularly a kind of supercritical co extracts the method for cyanine oligomer from Semen Vitis viniferae.
Raisin seed oil is present in Semen Vitis viniferae and the Pericarpium Vitis viniferae, and cyanine oligomer (Oligamer of ProanthCynidine, OPC) then extensively be present in the leaf and seed of plant, as Ginkgo Leaf, tealeaves, especially with the abundantest in Semen Vitis viniferae and the skin, and Semen Vitis viniferae and the Pi Ze waste of vinify industry normally.Up to this point, the method of extracting cyanine oligomer from Semen Vitis viniferae and skin remains organic solvent method, this method is not only extracted the flow process complexity, mass consumption organic solvent again, energy consumption height and serious environment pollution, the residual organic solvent that excess is arranged in the product particularly has influence on the purposes of product.
The object of the present invention is to provide a kind of supercritical co to extract the method for cyanine oligomer from Semen Vitis viniferae, product purity height, extraction yield height, environmental nonpollution, energy consumption are hanged down and are its characteristics.
Embodiment of the present invention are as follows: (consulting schema 1) is total in two steps: the first step, extract raisin seed oil earlier.To clean oven dry and be crushed to granularity is the charging basket that 20-40 purpose Semen Vitis viniferae is put into extraction kettle (1), open and send into preheater (11) and enter extraction kettle (1) after the fresh CO2 of high-pressure pump (10) suction enters high-pressure pump (10) by condenser (7), control extraction kettle (1) internal pressure is that 27 ± 2MPa, temperature are 60 ℃, extracted 2-4 hour, temperature is 0 ℃ in condenser (7) tubulation, the CO2 logistics of extraction back is heated to 65 ℃ through well heater (2), collect raisin seed oil in two series connection separators (3,4), the CO2 logistics is passed through condenser (7) again and is circulated.
Second step: extract cyanine oligomer.Start properties-correcting agent pump (9) in extraction after 2-4 hour, with the properties-correcting agent in the properties-correcting agent groove (8), be acetone: water is that 70: 30 properties-correcting agent also enters preheater (11), the amount ratio that CO2 logistics and properties-correcting agent behind the raisin seed oil were extracted in control is 4: 1, pressure is 22-25MPa, temperature is 60 ℃, after the extraction, enters another two placed in-line separators of group (5,6) behind the CO2 logistics process well heater (2) and isolates cyanine oligomer.
Advantage of the present invention is that technical process is simple and reliable, and raisin seed oil purity is more than 97% and yield reaches 15%, and cyanine oligomer purity is that yield is up to 14% more than 95%.
Below preference be described in detail in conjunction with 1 couple of the present invention of schema, but do not mean that and limit the scope of the invention.
Example 1: with 6 kilograms of cleaned oven dry and be crushed to 40 purpose Semen Vitis viniferaes and place 10 liters extraction kettle (1) barrel, start high-pressure pump (10), with fresh CO
2, be pressurized to 27 ± 2Mpa through condenser (7) suction, be heated to 60 ℃ through preheater (11) and send into extraction kettle (1), have the CO of raisin seed oil
2Logistics enters well heater (2) after coming out from extraction kettle (1), and controlled temperature is 65 ℃ and enters two placed in-line separators (3,4), emits raisin seed oil from the separator bottom: CO
2Come out in top after condenser (7) condenses to about 0 ℃ from separator (3,4) in logistics, enters high-pressure pump (10) again, and so, cycling extraction 3 hours is emitted 0.18 kilogram from separator (3,4), and yield is 15%.
Then, start properties-correcting agent pump (9), properties-correcting agent is acetone and water, and ratio is 70: 30, is 1: 4 properties-correcting agent and CO with throughput ratio
2Squeeze into preheater (11) after the mixing, the pressure of control extraction kettle (1) is 25 ± 2MPa, temperature is 58 ± 2 ℃, the temperature of preheater (11) is 60 ℃, it is 65 ℃ well heater (2) that material comes out through temperature from extraction kettle (1), and two placed in-line separators (5,6), emit cyanine oligomer liquid, CO from separator (5,6) bottom
2Gas enters condenser (7) through separator (5,6) top, and so cycling extraction is 2 hours; Emit cyanine oligomer from separator (5,6) bottom 0.24 kilogram, yield is 4%.
And then startup properties-correcting agent pump (9), with the properties-correcting agent in the properties-correcting agent groove (8), be acetone with the water ratio be that 70: 30 properties-correcting agent is extracted out in that preheater (11) is preceding mixes with the CO2 logistics (its measure than be 1: 4) and squeezed into preheater (11) simultaneously, this moment, extraction kettle (1) control pressure was 25 ± 2MPa, temperature is 58 ± 2 ℃, preheater (11) temperature is 60 ℃, heater via (2) after the CO2 logistics is come out from extraction kettle (1), be heated to 65 ℃ of temperature, through two placed in-line separators (5,6), from separator (5,6) bottom emits cyanine oligomer, and the CO2 logistics of coming out from separator (5,6) top enters condenser (7) again, so cycling extraction is 2 hours, emit 0.12 kilogram of cyanine oligomer from separator (5,6) bottom, yield is 14%.
Through gas chromatographic analysis raisin seed oil purity is 97.3%, is 96.5% through liquid-phase chromatographic analysis cyanine oligomer purity.
Example 2, when removing extraction of oil from grape seeds, the CO of the pressure-controlling of extraction kettle (10) during at 25 ± 2MPa with at the extracting procyanidins oligopolymer
2Flow and properties-correcting agent (acetone: the water ratio is 70: 30) amount is than being outside 4: 1, and all the other conditions are constant, gets 0.17 kilogram of raisin seed oil, and purity is 97.2%, yield 14.8%; 0.11 kilogram of cyanine oligomer, purity are 95.5%, yield 13.8%.
Claims (1)
1, a kind of supercritical co extracts the method for cyanine oligomer from Semen Vitis viniferae, it is characterized in that: altogether in two steps:
The first step, extract raisin seed oil:
With granularity is the charging basket that 20-40 purpose Semen Vitis viniferae is put into extraction kettle (1), and extraction conditions is 60 ℃ of pressure 27 ± 2MPa, temperature, extracts 2-4 hour; In two series connection separators (3,4), collect raisin seed oil, CO
2Gas passes through condenser (7) again and circulates.
In second step, extract cyanine oligomer:
After extraction 2-4 hour, start properties-correcting agent pump (9), with properties-correcting agent and CO
2Semen Vitis viniferae behind the extraction extraction oil, properties-correcting agent is acetone and water, ratio is 70: 30, properties-correcting agent and CO
2Throughput ratio be 1: 4, the condition that pressure 22-25MPa, temperature are 60 ℃, after extraction was finished, isolating purity at another two placed in-line separators of group (5,6) was 96.5% cyanine oligomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99111574A CN1107110C (en) | 1999-08-18 | 1999-08-18 | Supercritical carbon dioxide extraction process of grape seed oil and cyanine oligomer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99111574A CN1107110C (en) | 1999-08-18 | 1999-08-18 | Supercritical carbon dioxide extraction process of grape seed oil and cyanine oligomer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1241623A CN1241623A (en) | 2000-01-19 |
| CN1107110C true CN1107110C (en) | 2003-04-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN99111574A Expired - Fee Related CN1107110C (en) | 1999-08-18 | 1999-08-18 | Supercritical carbon dioxide extraction process of grape seed oil and cyanine oligomer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384832C (en) * | 2005-07-18 | 2008-04-30 | 天津大学 | Method of extracting proto anthocyanidin by supercritical extraction grape seed oil and resin absorption |
| WO2011147989A1 (en) | 2010-05-28 | 2011-12-01 | Finzelberg Gmbh & Co. Kg | Process for the preparation of an enriched extract from grape vine plant leaves |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111068C (en) * | 2000-07-27 | 2003-06-11 | 上海北医大生物科技有限公司 | Strong anti-oxidative composite capsule of grape seed extract OPC and its producing method |
| CN1311063C (en) * | 2005-06-17 | 2007-04-18 | 长沙桑霖生物科技有限公司 | Method for extracting spine grape seed oil from spine grape seeds |
| CN101199689B (en) * | 2007-12-24 | 2012-04-18 | 浙江省中药研究所有限公司 | Grape chrysanthemum capsule and preparing method thereof |
| CN101787010B (en) * | 2010-03-16 | 2012-05-23 | 浙江大学 | Method for extracting oligo proanthocyanidin from grape seeds |
| CN102224923B (en) * | 2011-04-26 | 2012-08-08 | 乌鲁木齐富润东方生物科技有限公司 | Preparation method of modified apple polyphenol |
| CN103193751A (en) * | 2013-03-27 | 2013-07-10 | 吉首大学 | Method for continuously extracting active ingredients from grape seeds |
| CN108795563A (en) * | 2018-06-29 | 2018-11-13 | 成都纺织高等专科学校 | A kind of supercritical CO2The method of extraction of oil from grape seeds |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145400A (en) * | 1995-09-11 | 1997-03-19 | 贵州省生物资源超临界流体萃取研究开发中心 | Method of extracting perilla plant oil by using super-critical CO2 |
| JPH09221484A (en) * | 1996-02-14 | 1997-08-26 | Kikkoman Corp | Production of proanthocyanidin |
-
1999
- 1999-08-18 CN CN99111574A patent/CN1107110C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145400A (en) * | 1995-09-11 | 1997-03-19 | 贵州省生物资源超临界流体萃取研究开发中心 | Method of extracting perilla plant oil by using super-critical CO2 |
| JPH09221484A (en) * | 1996-02-14 | 1997-08-26 | Kikkoman Corp | Production of proanthocyanidin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384832C (en) * | 2005-07-18 | 2008-04-30 | 天津大学 | Method of extracting proto anthocyanidin by supercritical extraction grape seed oil and resin absorption |
| WO2011147989A1 (en) | 2010-05-28 | 2011-12-01 | Finzelberg Gmbh & Co. Kg | Process for the preparation of an enriched extract from grape vine plant leaves |
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| Publication number | Publication date |
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| CN1241623A (en) | 2000-01-19 |
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