CN1373132A - Process for supercritical extracting nimbin - Google Patents
Process for supercritical extracting nimbin Download PDFInfo
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- CN1373132A CN1373132A CN02113360A CN02113360A CN1373132A CN 1373132 A CN1373132 A CN 1373132A CN 02113360 A CN02113360 A CN 02113360A CN 02113360 A CN02113360 A CN 02113360A CN 1373132 A CN1373132 A CN 1373132A
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- nimbin
- cosolvent
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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
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Abstract
A process for supercritical extracting nimbin from the seed kernel, bark, leaf and twigs of nim includes extracting at 30-60 deg.c and 24.8-31 MPa for 120-280 min by concentrated CO2 and cosolvent, e.g. methanol, ethanol, acetone, ethyl acetate, etc, while discharging the extract continuously, preheating, cyclone separating at 30-60 deg.C and 15.5-21.7 MPa, depressurizing in a sealed container, drying and grinding.
Description
Technical field
The present invention relates to adopt super critical CO 2 technology from neem kernel, branch, bark, leaf, to extract the technology of nimbin.
Background technology
The seal chinaberry more and more is subjected to people's attention as a kind of " can solve the tree of global problems ", and nimbin has superior efficacy such as anti-inflammatory, sterilization, antipruritic, insect protected as the most effective activeconstituents wherein.Be applied to aspects such as agricultural chemicals, medicine, daily-use chemical industry more and more.Not only technical process is long but traditional solvent method extracts nimbin, and solvent consumption is big, and yield is low, the cost height, and environment polluted harm humans health.
Summary of the invention
The object of the present invention is to provide a kind of technology that adopts super critical CO 2 technology from neem kernel, bark, branch, leaf, to extract nimbin, it is according to stagnation point and the at high temperature easy characteristics that decomposition take place of nimbin in carbonic acid gas, adopt carbonic acid gas as supercutical fluid, with organic solvent, as methyl alcohol, ethanol, acetone, ethyl acetate, trichloromethane, methylene dichloride etc. is cosolvent, under supercritical state, neem kernel, bark, branch, leaf are extracted, obtain the higher nimbin of content; In spissated carbonic acid gas, add quantitative cosolvent, can improve the solubleness of nimbin, simultaneously the rate of recovery that also can corresponding raising nimbin.
Purpose of the present invention is implemented by following technical solution:
The technology of supercritical extracting nimbin, it is a raw material with neem kernel, bark, branch, leaf etc., it is characterized in that following these steps to extract nimbin:
A, extraction kettle will be put into after the raw material pulverizing, is that concentrated carbonic acid gas and the cosolvent of 9.8～10.3MPa extracts it with temperature at-10～10 ℃, pressure, 30～60 ℃ of extraction temperature, pressure are 24.8～31Mpa, keep said temperature and pressure 120～280 minutes, and constantly discharge extraction liquid;
B, extraction liquid separate after preheating, and it is 15.5～21.7Mpa that separation temperature is controlled at 30～60 ℃, pressure;
C, the isolating composition that is extracted make pressure reduce to normal pressure again through entering the step-down container of sealing after the cyclonic separation;
D, collection separate the product that obtains, and through super-dry, grinding, promptly obtain being rich in the product of nimbin.
Described cosolvent is organic solvents such as methyl alcohol, ethanol, acetone, ethyl acetate, trichloromethane, methylene dichloride, and the cosolvent add-on is 1～60 times of raw material.
The concentrated carbonic acid gas flow rate that adds is 1500～2500kg/hr, and the flow rate of cosolvent is 50～150kg/hr.
Compared with prior art, the present invention adopts super critical CO 2 technology to extract nimbin from neem kernel, bark, branch, leaf, replace traditional solvent extration, avoided a large amount of uses and the consequent defective of organic solvent, as toxicity, pollution, inflammable, leakage etc.Through 120～280 minutes cycling extraction, obtain effective constituent, enforcement of the present invention has improved production efficiency greatly; it is short to have flow process, and less energy consumption does not pollute; the product purity height of producing, the characteristics that economic worth is high, and environment protection played positive effect.
Description of drawings: Fig. 1 is a process flow diagram of the present invention.
Below in conjunction with embodiment the present invention is further described, but protection scope of the present invention is not limited to embodiment.
In the nimbin extraction process as shown in the figure, Liquid carbon dioxide is stored in storage tank R
1In, the control tank temperature is-10～10 ℃, and pressure is 9.8～10.3MPa, and the carbonic acid gas flow rate is controlled at 1500～2500kg/hr, through being heated to extraction temperature by separating preheater E3 behind the circulate carbon dioxide water cooler E2 under the pumping of high-pressure pump P1;
The supercutical fluid that adds cosolvent enters extraction kettle A
1, A
2, 30～60 ℃ of control extraction kettle temperature, pressure is 24.8～31Mpa, the cosolvent flow rate is 50～150kg/hr;
Separate preheater E from the extraction liquid process that is rich in activeconstituents that extraction kettle is discharged
4Heating enters separator V
1In separate, the control separator temperature is 30～60 ℃, pressure is 15.5～21.7MPa, is extracted the cyclonic separator V of composition through two parallel connections after the separation
2, V
3Enter the step-down container V of two sealings
4, V
5, make pressure reduce to normal pressure;
Cosolvent is through recirculation cooler E
5, E
6With circulating solvent moisture eliminator X
1After get back to solvent tank V
6In, by solvent cycle pump P
2Get back to extraction kettle.
From separator V
1Middle carbonic acid gas of discharging is through carbon dioxide recovery compressor C
1With circulate carbon dioxide water cooler E
1, get back to carbon dioxide storage tank R
1In, by vacuum pump P
3To solvent tank V
6Middle supplementing solvent.
Collect and separate the product that obtains,, promptly obtain being rich in the product of nimbin through super-dry, grinding.
Embodiment:
Embodiment 1
Carry out cold press after 500 kilograms of neem seeds are peeled off and handle, reclaim most nim oil, obtain the nim oil cake and put into extraction kettle for 200 kilograms.The extraction kettle temperature is controlled at 50 ℃, separator temperature is controlled at 40 ℃, the Liquid carbon dioxide tank temperature is controlled at-10～10 ℃, extraction kettle pressure is 28.9MPa, and separator pressure is 18.6MPa, and the Liquid carbon dioxide pressure of storage tank is 10.3MPa, cycling extraction through 200 minutes, acquisition contains the multiphase mixture of cosolvent, solute and other heavier solids components, reclaims cosolvent for recycling through vacuum distilling then, concentrates 2.45 kilograms of products that obtain containing 30% nimbin.
Embodiment 2
Carrying out cold press after 450 kilograms of neem seeds are peeled off handles, obtain the nim oil cake and put into extraction kettle for 178 kilograms, the extraction kettle temperature is controlled at 53 ℃, separator temperature is controlled at 42 ℃, the temperature of Liquid carbon dioxide storage tank is-10～10 ℃, extraction kettle pressure is 30.7MPa, separator pressure 19.4MPa, the Liquid carbon dioxide pressure of storage tank is 10.1MPa, cycling extraction through 170 minutes, acquisition contains cosolvent, the multiphase mixture of solute and other heavier solids components reclaims cosolvent (for recycling) through vacuum distilling then, concentrates 2.21 kilograms of products that obtain containing 30% nimbin.
Embodiment 3
To put into extraction kettle after the pulverizing of 500 kilograms of seal neem barks, the extraction kettle temperature is controlled at 48 ℃, and separator temperature is controlled at 45 ℃, uses high-pressure pump P
1Liquid carbon dioxide is sent into extraction kettle, extraction kettle pressure is 27MPa, separator pressure 16MPa, the Liquid carbon dioxide pressure of storage tank is 9.8MPa, cycling extraction through 180 minutes, acquisition contains the multiphase mixture of cosolvent, solute and other heavier solids components, reclaims cosolvent (for recycling) through vacuum distilling then, concentrates 0.49 kilogram of the product that obtains containing 5% nimbin.
Embodiment 4
Put into extraction kettle after will printing 480 kilograms of pulverizing of chinaberry leaf, control extraction kettle temperature is 50 ℃, separator temperature is 40 ℃, the Liquid carbon dioxide tank temperature is-10～10 ℃, extraction kettle pressure is 25MPa, separator pressure is 15MPa, the Liquid carbon dioxide pressure of storage tank is 10.3MPa, cycling extraction through 230 minutes, acquisition contains the multiphase mixture of cosolvent, solute and other heavier solids components, reclaim cosolvent (for recycling) through vacuum distilling then, concentrate 0.54 kilogram of the product that obtains containing 5% nimbin.
Claims (3)
1, a kind of process for supercritical extracting nimbin, it is a raw material with neem kernel, bark, branch, leaf etc., it is characterized in that following these steps to extract nimbin:
A, extraction kettle will be put into after the raw material pulverizing, is that concentrated carbonic acid gas and the cosolvent of 10.3MPa extracts it with temperature at-10～10 ℃, pressure, 30～60 ℃ of extraction temperature, pressure are 24.8～31Mpa, keep said temperature and pressure 120～280 minutes, and constantly discharge extraction liquid;
B, extraction liquid separate after preheating, and it is 15.5～21.7Mpa that separation temperature is controlled at 30～60 ℃, pressure;
C, the isolating composition that is extracted make pressure reduce to normal pressure again through entering the step-down container of sealing after the cyclonic separation;
D, collection separate the product that obtains, and through super-dry, grinding, promptly obtain being rich in the product of nimbin
2, technology according to claim 1 is characterized in that: cosolvent is organic solvents such as methyl alcohol, ethanol, acetone, ethyl acetate, trichloromethane, methylene dichloride, and the cosolvent add-on is 1～60 times of raw material.
3, technology according to claim 1 is characterized in that: spissated carbonic acid gas flow rate is 1500～2500kg/hr, and the flow rate of cosolvent is 50～150kg/hr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021133603A CN1158928C (en) | 2002-02-08 | 2002-02-08 | Process for supercritical extracting nimbin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021133603A CN1158928C (en) | 2002-02-08 | 2002-02-08 | Process for supercritical extracting nimbin |
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| Publication Number | Publication Date |
|---|---|
| CN1373132A true CN1373132A (en) | 2002-10-09 |
| CN1158928C CN1158928C (en) | 2004-07-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021133603A Expired - Fee Related CN1158928C (en) | 2002-02-08 | 2002-02-08 | Process for supercritical extracting nimbin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102696696A (en) * | 2012-06-11 | 2012-10-03 | 四川农业大学 | Grass meal granular formulation for controlling rodent pests in grassland and preparation method as well as application thereof |
| CN103483358A (en) * | 2013-10-15 | 2014-01-01 | 成都绿金生物科技有限责任公司 | Method for producing neem crude drug by extracting neem with supercritical CO2 |
| CN108938724A (en) * | 2018-08-24 | 2018-12-07 | 云南希康生物科技有限公司 | A kind of neem leaf extract and its preparation process, application |
| CN113056568A (en) * | 2018-08-31 | 2021-06-29 | 德克萨斯大学体系董事会 | Neem compositions and methods for treating cancer |
-
2002
- 2002-02-08 CN CNB021133603A patent/CN1158928C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102696696A (en) * | 2012-06-11 | 2012-10-03 | 四川农业大学 | Grass meal granular formulation for controlling rodent pests in grassland and preparation method as well as application thereof |
| CN103483358A (en) * | 2013-10-15 | 2014-01-01 | 成都绿金生物科技有限责任公司 | Method for producing neem crude drug by extracting neem with supercritical CO2 |
| CN103483358B (en) * | 2013-10-15 | 2015-08-05 | 成都绿金生物科技有限责任公司 | A kind of supercritical CO 2extraction print chinaberry produces the method for the former medicine of print chinaberry |
| CN108938724A (en) * | 2018-08-24 | 2018-12-07 | 云南希康生物科技有限公司 | A kind of neem leaf extract and its preparation process, application |
| CN108938724B (en) * | 2018-08-24 | 2021-06-18 | 云南希康生物科技有限公司 | Neem leaf extract and preparation process and application thereof |
| CN113056568A (en) * | 2018-08-31 | 2021-06-29 | 德克萨斯大学体系董事会 | Neem compositions and methods for treating cancer |
| EP3844312A4 (en) * | 2018-08-31 | 2022-06-22 | Board of Regents, The University of Texas System | Compositions of azadirachta indica and methods of treating cancer |
| EP3843764A4 (en) * | 2018-08-31 | 2022-08-03 | Board of Regents, The University of Texas System | Compositions of azadirachta indica and methods of treating cancer |
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| Publication number | Publication date |
|---|---|
| CN1158928C (en) | 2004-07-28 |
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