CN103483358B - A kind of supercritical CO 2extraction print chinaberry produces the method for the former medicine of print chinaberry - Google Patents
A kind of supercritical CO 2extraction print chinaberry produces the method for the former medicine of print chinaberry Download PDFInfo
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- CN103483358B CN103483358B CN201310480938.3A CN201310480938A CN103483358B CN 103483358 B CN103483358 B CN 103483358B CN 201310480938 A CN201310480938 A CN 201310480938A CN 103483358 B CN103483358 B CN 103483358B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D519/00—Heterocyclic compounds containing more than one system of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring system not provided for in groups C07D453/00 or C07D455/00
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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
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- 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
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Abstract
The invention discloses a kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry.The efficiency solving existing preparation method is lower, and cost is higher, and the problem that in product, Azadirachtin Cotent is not high.The present invention includes following steps: (1) gets the raw materials ready, (2) extraction, (3) crystallization, (4) recrystallization, Azadirachtin Cotent >=20% in the product finally prepared; Can be enhanced productivity while being lowered into product cost by the present invention, and obtained product Azadirachtin Cotent is high, thus the demand of growing nimbin raw medicine can be met.
Description
Technical field
The present invention is specifically related to a kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry.
Background technology
Print chinaberry system Meliaceae Melia arbor, extensively plants in tropical and subtropical region.Originate in Burma and India, have distribution and plantation in more than 70 countries, maximum with Asian countries's output such as India.Print in the fruit of chinaberry, seed, kind core, branch, leaf, bark and resin and all contain active substance, but with seed more so.So far, found 100 multiple compounds in print chinaberry, have at least 70 kinds of compounds to have biological activity, they are diterpenes, triterpenes, five triterpeness and non-terpenoid.Be mainly margosa tree element, melianotriol and nimbin etc., these extracts have food refusal to insect, interference is laid eggs, interference insect variation, make it cannot change in quality for adult, repellent larva and the effect that suppresses it to grow and reach desinsection object.Nimbin is that a class isolates the strongest active compound from print chinaberry, and it belongs to tetracyclic triterpenes.And Chinese patent ZL01108503.7, there is following defect in it: (1) production efficiency is lower, be difficult to the demand meeting growing nimbin raw medicine industry, (2) in production process, energy consumption is comparatively large, makes product cost higher, makes its competitive power not high, (3) existing carbon dioxide abstraction is used to print chinaberry production print chinaberry medicinal extract content not high, impurity phase is to more, and product is stable not, there is certain risk and problem for production formulation products.
Summary of the invention
The object of the present invention is to provide a kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and the efficiency solving existing preparation method is lower, and cost is higher, and the problem that in product, Azadirachtin Cotent is not high.
The present invention is achieved through the following technical solutions:
A kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, the chloroform of 95%, wherein the flow of carbonic acid gas and the weight ratio of neem kernel are 100 ~ 200:1, and carbonic acid gas and chloroform weight ratio are 100:6 ~ 8;
(2) extract: neem kernel is placed in extraction plant, be 2 ~ 24.9Mpa at pressure, temperature is that under 30 ~ 60 DEG C of conditions, the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio extracts, extraction time is 2 ~ 5 hours, both obtains paste;
(3) crystallization: paste is transferred in crystallization kettle, now paste Azadirachtin Cotent is 10%, adds acetone and makes it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 DEG C of conditions, now obtains the nimbin crystal that Azadirachtin Cotent is 15%;
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3 ~ 5, heats to 55 DEG C and makes it to dissolve completely, progressively be cooled to 1 ~ 5 DEG C again, still intercrystalline is separated out, and goes out still and filters, crystal is then fine work nimbin, content >=20%.
Further, the specifically implementation method of described step (2) is as follows: neem kernel is placed in one-level extraction kettle, be 2 ~ 24.9Mpa at pressure, temperature is under 30 ~ 60 DEG C of conditions, the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio carries out one-level extraction, and the time is 1 ~ 2 hour; Extraction liquid passes into primary separator, is 2 ~ 7Mpa at pressure, and temperature is isolate paste solution and waste residue under 30 ~ 40 DEG C of conditions; Paste solution is passed into secondary extraction, the time is 0.5 ~ 2 hour, and secondary extract is passed into second-stage separator, is 2 ~ 7Mpa at pressure, and temperature is under 30 ~ 50 DEG C of conditions, is separated, obtains paste by second-stage separator; Whole extraction time is 2 ~ 5 hours.
In order to reduce production cost, described secondary extract also comprises carbonic acid gas and chloroform by the isolated material of second-stage separator; Wherein carbonic acid gas again carries chloroform and enters in one-level extraction kettle and carry out next round extraction after condensation, compression.Carbon dioxide recovery can utilize by this step, has saved production cost greatly.
Preferred as one, flow and the neem kernel weight ratio of the middle carbonic acid gas of described step (1) are 150:1, and carbonic acid gas and chloroform weight ratio are 100:6.
Or in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 100:1, and carbonic acid gas and chloroform weight ratio are 100:8.
Or in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 200:1, and carbonic acid gas and chloroform weight ratio are 100:7.
In addition, in described step (2), pressure is 24.9Mpa, and temperature is 50 DEG C.
The present invention has the following advantages and beneficial effect:
(1) chloroform selected by entrainment agent of the present invention, and do not use the entrainment agents such as traditional methyl alcohol, ethanol, thus improve leaching effect, its reason is that methyl alcohol, ethanol etc. are relatively poor to the solvability of nimbin, leaching effect is very not good, after applicant puts into practice for a long time and tests, find to use chloroform respond well as entrainment agent, effect improves about 10%.
(2) The inventive method achieves carbon dioxide recycling, improve raw-material rate of utilization, reduce energy consumption, thus reduce production cost.
(3) method of the present invention carries out specific crystallization and re-crystallization step to the paste obtained, thus improves the content of nimbin in product.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, the chloroform of 95%, wherein the flow of carbonic acid gas and the weight ratio of neem kernel are 150:1, and carbonic acid gas and chloroform weight ratio are 100:6.
(2) extract: neem kernel being placed in one-level extraction kettle, is 24.9Mpa at pressure, and temperature is under 50 DEG C of conditions, and the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio carries out one-level extraction, and the time is 1.5 hours; Extraction liquid passes into primary separator, is 5Mpa at pressure, and temperature is isolate paste solution and waste residue under 40 DEG C of conditions; Paste solution is passed into secondary extraction, time is 1.5 hours, secondary extract is passed into second-stage separator, be 5Mpa at pressure, temperature is under 50 DEG C of conditions, isolates paste, chloroform and carbonic acid gas by second-stage separator, and carbonic acid gas again carries chloroform after condensation, compression to carry out one-level extraction kettle and carry out next round extraction, to realize carbon dioxide recycling, namely complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now paste Azadirachtin Cotent is 10%, adds acetone and makes it to dissolve, and the add-on of acetone being advisable in submergence, acetone is evaporated to dry under 55 DEG C of conditions, now obtains the nimbin crystal that Azadirachtin Cotent is 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:4, heats to 55 DEG C and makes it to dissolve completely, progressively be cooled to 1 DEG C again, still intercrystalline is separated out, and goes out still and filters, crystal is then fine work nimbin, content >=20%.
Then detect, if less than index, then recrystallization again, knows and meets index.Finally lucifuge is only needed to pack.
Embodiment 2
A kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, the chloroform of 95%, wherein the flow of carbonic acid gas and the weight ratio of neem kernel are 100:1, and carbonic acid gas and chloroform weight ratio are 100:7.
(2) extract: neem kernel being placed in one-level extraction kettle, is 20Mpa at pressure, and temperature is under 30 DEG C of conditions, and the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio carries out one-level extraction, and the time is 2 hours; Extraction liquid passes into primary separator, is 2Mpa at pressure, and temperature is isolate paste solution and waste residue under 30 DEG C of conditions; Paste solution is passed into secondary extraction, time is 1 hour, secondary extract is passed into second-stage separator, be 2Mpa at pressure, temperature is under 30 DEG C of conditions, isolates paste, chloroform and carbonic acid gas by second-stage separator, and carbonic acid gas again carries chloroform after condensation, compression to carry out one-level extraction kettle and carry out next round extraction, to realize carbon dioxide recycling, namely complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now paste Azadirachtin Cotent is 10%, adds acetone and makes it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 DEG C of conditions, now obtains the nimbin crystal that Azadirachtin Cotent is 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3, heats to 55 DEG C and makes it to dissolve completely, progressively be cooled to 3 DEG C again, still intercrystalline is separated out, and goes out still and filters, crystal is then fine work nimbin, content >=20%.
Then detect, if less than index, then recrystallization again, until meet index.Finally lucifuge is only needed to pack.
Embodiment 3
A kind of supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, the chloroform of 95%, wherein the flow of carbonic acid gas and the weight ratio of neem kernel are 200:1, and carbonic acid gas and chloroform weight ratio are 100:8.
(2) extract: neem kernel being placed in one-level extraction kettle, is 2Mpa at pressure, and temperature is under 40 DEG C of conditions, and the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio carries out one-level extraction, and the time is 1 hour; Extraction liquid passes into primary separator, is 7Mpa at pressure, and temperature is isolate paste solution and waste residue under 35 DEG C of conditions; Paste solution is passed into secondary extraction, time is 2 hours, secondary extract is passed into second-stage separator, be 7Mpa at pressure, temperature is under 40 DEG C of conditions, isolates paste, chloroform and carbonic acid gas by second-stage separator, and carbonic acid gas again carries chloroform after condensation, compression to carry out one-level extraction kettle and carry out next round extraction, to realize carbon dioxide recycling, namely complete a circulation.The whole cycling extraction time is 4 hours.
(3) crystallization: paste is transferred in crystallization kettle, now paste Azadirachtin Cotent is 10%, adds acetone and makes it to dissolve, and the add-on of acetone is different can be advisable in submergence, acetone is evaporated to dry under 55 DEG C of conditions, now obtains the nimbin crystal that Azadirachtin Cotent is 15%.
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:5, heats to 55 DEG C and makes it to dissolve completely, progressively be cooled to 5 DEG C again, still intercrystalline is separated out, and goes out still and filters, crystal is then fine work nimbin, content >=20%.
Then detect, if less than index, then recrystallization again, until meet index.Finally lucifuge is only needed to pack.
Should be noted that, above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although with reference to above-described embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: still can modify to the present invention or equivalent replacement, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (7)
1. a supercritical CO
2extraction print chinaberry produces the method for the former medicine of print chinaberry, it is characterized in that, comprises the following steps:
(1) get the raw materials ready: get the neem kernel after pulverizing, CO 2 fluid, the chloroform of 95%, wherein the flow of carbonic acid gas and the weight ratio of neem kernel are 100 ~ 200:1, and carbonic acid gas and chloroform weight ratio are 100:6 ~ 8;
(2) extract: neem kernel is placed in extraction plant, be 2 ~ 24.9Mpa at pressure, temperature is under 30 ~ 60 DEG C of conditions, the carbonic acid gas passing into the above-critical state carrying chloroform by the flow of the carbonic acid gas of above-mentioned weight ratio and neem kernel extracts, extraction time is 2 ~ 5 hours, both obtains paste;
(3) crystallization: paste is transferred in crystallization kettle, now paste Azadirachtin Cotent is 10%, and add acetone and make it to dissolve, acetone is evaporated to dry under 55 DEG C of conditions, now obtains the nimbin crystal that Azadirachtin Cotent is 15%;
(4) recrystallization: add tetracol phenixin in above-mentioned nimbin crystal, the weight ratio of nimbin crystal and tetracol phenixin is 1:3 ~ 5, heats to 55 DEG C and makes it to dissolve completely, progressively be cooled to 1 ~ 5 DEG C again, still intercrystalline is separated out, and goes out still and filters, crystal is then fine work nimbin, content >=20%.
2. a kind of supercritical CO according to claim 1
2extraction print chinaberry produces the method for the former medicine of print chinaberry, it is characterized in that, the specifically implementation method of described step (2) is as follows: neem kernel is placed in one-level extraction kettle, be 2 ~ 24.9Mpa at pressure, temperature is under 30 ~ 60 DEG C of conditions, the carbonic acid gas passing into the above-critical state carrying chloroform by above-mentioned weight ratio carries out one-level extraction, and the time is 1 ~ 2 hour; Extraction liquid passes into primary separator, is 2 ~ 7Mpa at pressure, and temperature is isolate paste solution and waste residue under 30 ~ 40 DEG C of conditions; Paste solution is passed into secondary extraction, the time is 0.5 ~ 2 hour, and secondary extract is passed into second-stage separator, is 2 ~ 7Mpa at pressure, and temperature is under 30 ~ 50 DEG C of conditions, is separated, obtains paste by second-stage separator; Whole extraction time is 2 ~ 5 hours.
3. a kind of supercritical CO according to claim 2
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and it is characterized in that, described secondary extract also comprises carbonic acid gas and chloroform by the isolated material of second-stage separator; Wherein carbonic acid gas again carries chloroform and enters in one-level extraction kettle and carry out next round extraction after condensation, compression.
4. a kind of supercritical CO according to claim 1
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 150:1, and carbonic acid gas and chloroform weight ratio are 100:6.
5. a kind of supercritical CO according to claim 1
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 100:1, and carbonic acid gas and chloroform weight ratio are 100:8.
6. a kind of supercritical CO according to claim 1
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and it is characterized in that, in described step (1), the flow of carbonic acid gas and the weight ratio of neem kernel are 200:1, and carbonic acid gas and chloroform weight ratio are 100:7.
7. a kind of supercritical CO according to claim 1
2extraction print chinaberry produces the method for the former medicine of print chinaberry, and it is characterized in that, in described step (2), pressure is 24.9Mpa, and temperature is 50 DEG C.
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Citations (4)
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| CN1373132A (en) * | 2002-02-08 | 2002-10-09 | 云南中科生物产业有限公司 | Process for supercritical extracting nimbin |
| CN1389465A (en) * | 2001-06-06 | 2003-01-08 | 成都绿金生物科技有限责任公司 | Supercritical fluid extraction process of nim to produce mimbin extract |
| CN101029276A (en) * | 2006-03-03 | 2007-09-05 | 中国林业科学研究院资源昆虫研究所 | Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed |
| CN101857603A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院地球化学研究所 | Multi-stage countercurrent extraction method for azadirachtin |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389465A (en) * | 2001-06-06 | 2003-01-08 | 成都绿金生物科技有限责任公司 | Supercritical fluid extraction process of nim to produce mimbin extract |
| CN1373132A (en) * | 2002-02-08 | 2002-10-09 | 云南中科生物产业有限公司 | Process for supercritical extracting nimbin |
| CN101029276A (en) * | 2006-03-03 | 2007-09-05 | 中国林业科学研究院资源昆虫研究所 | Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed |
| CN101857603A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院地球化学研究所 | Multi-stage countercurrent extraction method for azadirachtin |
Non-Patent Citations (2)
| Title |
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| 新工艺萃取印楝素及机理初探;赵淑英等;《山东化工》;20091231;第38卷(第10期);第4-6、11页 * |
| 李永红.印楝(Azadirachta indica)种仁中印楝素的提取及其杀虫活性研究.《中国优秀硕士学位论文全文数据库(硕士)农业科技辑》.2003,(第02期),第16页. * |
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