CN102138960A - Novel extraction process of dalbergiae oil through super (sub) critical carbon dioxide - Google Patents
Novel extraction process of dalbergiae oil through super (sub) critical carbon dioxide Download PDFInfo
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- CN102138960A CN102138960A CN2010101048226A CN201010104822A CN102138960A CN 102138960 A CN102138960 A CN 102138960A CN 2010101048226 A CN2010101048226 A CN 2010101048226A CN 201010104822 A CN201010104822 A CN 201010104822A CN 102138960 A CN102138960 A CN 102138960A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000605 extraction Methods 0.000 title claims abstract description 33
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 23
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000284 extract Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003795 desorption Methods 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 6
- 238000000638 solvent extraction Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001256 steam distillation Methods 0.000 description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 description 3
- 239000000341 volatile oil Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000657528 Dalbergia odorifera Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
本发明涉及以超(亚)临界二氧化碳技术萃取降香油的新工艺。文献曾报道超临界二氧化碳携带乙醇夹带剂萃取降香油的工艺，夹带剂难以去除，后续处理比较麻烦，影响产品质量。本发明提供了一种无需用夹带剂且萃取效率高的方法。通过优化萃取温度、压力、时间及二氧化碳流速，得到好的工艺条件，其中萃取温度为20-55℃，萃取压力为20-35MPa，解析釜温度为40-60℃，压力为6-12MPa，萃取时间1-2h，二氧化碳流量为20-40L/h，所得萃出物收率为1.28％，高于文献报道萃取率(1.05％)。本发明采用超(亚)临界二氧化碳流体萃取速度快、收率高，是一种高效、节能、安全无毒、对环境无污染的萃取方法。The invention relates to a new process for extracting balsamic oil with super (sub)critical carbon dioxide technology. It has been reported in the literature that supercritical carbon dioxide carries an ethanol entrainer to extract balsamic oil. The entrainer is difficult to remove, and the follow-up treatment is cumbersome, which affects product quality. The invention provides a method without entrainer and high extraction efficiency. By optimizing the extraction temperature, pressure, time and flow rate of carbon dioxide, good process conditions are obtained. The extraction temperature is 20-55°C, the extraction pressure is 20-35MPa, the temperature of the desorption tank is 40-60°C, and the pressure is 6-12MPa. The time is 1-2h, the flow rate of carbon dioxide is 20-40L/h, and the yield of the obtained extract is 1.28%, which is higher than the extraction rate (1.05%) reported in the literature. The invention adopts super (sub)critical carbon dioxide fluid to extract fast and high yield, and is an extraction method with high efficiency, energy saving, safety, non-toxicity and no pollution to the environment.
Description
Technical field
The invention belongs to and adopt super (Asia) critical carbon dioxide fluid from the Chinese medicine Lignum Dalbergiae Odoriferae, to extract the new technology of Lignum Dalbergiae Odoriferae oil.
Background technology
Lignum Dalbergiae Odoriferae is the dry duramen of leguminous plant Lignum Dalbergiae Odoriferae wingceltis Dalbergia odorifera T.chen trunk and root.Have promoting the circulation of QI to relieve pain, the effect of promoting blood circulation and hemostasis.Be used for the vexed pain in ambition, the twinge of the gastral cavity side of body, the external treatment traumatic injury is hemorrhage.Existing chemical medicine reason studies show that Lignum Dalbergiae Odoriferae can suppress thrombosis, and the composition that plays anticoagulation is the volatile oil part.
The method of extraction oil has steam distillation, solvent extraction etc. from Lignum Dalbergiae Odoriferae.Relatively poor with steam distillation gained Lignum Dalbergiae Odoriferae oil taste, fragrance is not strong, with natural Lignum Dalbergiae Odoriferae fragrance gap is arranged.With solvent extraction residual organic solvent in oil, can not preserve the natural sex of Lignum Dalbergiae Odoriferae oil, and subsequent treatment is cumbersome, so steam distillation and solvent extraction all are not ideal extracting process.
Supercritical fluid extraction is the novel extraction method of development in recent years, and the most frequently used supercritical solvent is a carbon dioxide, supercriticality (critical temperature T
c=31.06 ℃, critical pressure Pc=7.39MPa) the existing similar liquid character of the carbon dioxide under can keep gas performance again, utilize its liquid character that the big characteristics of substance dissolves degree are extracted, utilize gas property to be easy to diffusion and material separated with motion, thus reach to the extraction of different material with separate.And with the change of temperature and pressure, solvent density changes greatly, shows as changes in solubility accordingly, thereby can pass through controlled pressure, temperature realization extraction and separating process.
Carbon dioxide under the subcritical state is liquid, and the liquid state that is under the high saturation pressure can be used as solvent, when separating with solute liquid gas is steamed to get final product.Subcritical liquid carbon dioxide is powerful to the solubility property of material, and temperature is lower than supercritical, and resulting result and supercritical are close, just has difference aspect extract yield or the quality, can differ an order of magnitude sometimes.
To sum up, use super (Asia) critical fluids extraction temperature low, nontoxic, can prevent the thermal decomposition and the oxidation of labile element.
Bibliographical information supercritical carbon dioxide extraction Lignum Dalbergiae Odoriferae oil is arranged, but its author has used ethanol to do entrainer, need remove entrainer for obtaining pure Lignum Dalbergiae Odoriferae oil, subsequent treatment is cumbersome, and oily yield is 1.05%.The present invention directly adopts super (Asia) critical carbon dioxide as the solvent extraction Lignum Dalbergiae Odoriferae oil, and gained oil yield is 1.28%, and yield is higher than document, and does not need subsequent treatment, is a kind of better extracting process.
Summary of the invention
In order to solve the defective that exists in the prior art, the present invention proposes a kind of technology of not using the high extraction Lignum Dalbergiae Odoriferae oil of entrainer and yield, super by using (Asia) critical carbon dioxide fluid extraction technology is to extraction temperature, pressure, time and CO
2Flow velocity is optimized, and obtains good process conditions.
The present invention extracts the method for Lignum Dalbergiae Odoriferae oil, is to adopt super (Asia) critical carbon dioxide fluid extraction method, and its processing step comprises:
1, Lignum Dalbergiae Odoriferae heartwood grinding and processing was become the coarse powder of 35-80 mesh sieve;
2, above-mentioned coarse powder is inserted in the extraction kettle extract, control extraction temperature in the kettle is 20-55 ℃, and pressure is 20-40MPa;
3, control extraction-container temperature is 30-60 ℃, and pressure is in the scope of 6-12MPa;
4, the extraction time is 1-2h;
5, the carbon dioxide flow velocity is 20-40L/h, recycles in extraction process;
6, the Lignum Dalbergiae Odoriferae oil color that obtains from separating still under subcritical state or low temperature is reddish brown, limpid, have the natural fragrant and sweet flavor of Lignum Dalbergiae Odoriferae.The gained Lignum Dalbergiae Odoriferae oil contains small amount of precipitate under relatively-high temperature, and color is a brownish red.
The specific embodiment
Specific embodiment one
Get exsiccant Lignum Dalbergiae Odoriferae heartwood raw material, grinding and processing becomes 40 purpose coarse powder, take by weighing 280g and insert the extraction kettle of HA220-50-06 type supercritical extraction unit (production of Jiangsu Province Nantong Huaan Overcritical Extraction Co., Ltd.) 1L, extracting pressure is 25MPa, and temperature in the kettle is 40 ℃, the extraction-container temperature is 50 ℃, pressure is 8.2MPa, and carbon dioxide flow is 22L/h, recycles to extract in extraction process, the extraction time is 1 hour, obtains volatile oil of Lignum Dalbergiae Odoriferae 3.48g from separating still.
Specific embodiment two
Get exsiccant Lignum Dalbergiae Odoriferae heartwood raw material, grinding and processing becomes 40 purpose coarse powder, take by weighing 280g and insert the extraction kettle of HA220-50-06 type supercritical extraction unit (production of Jiangsu Province Nantong Huaan Overcritical Extraction Co., Ltd.) 1L, extracting pressure is 30MPa, and temperature in the kettle is 30 ℃, the extraction-container temperature is 50 ℃, pressure is 7MPa, and carbon dioxide flow is 22L/h, recycles to extract in extraction process, the extraction time is 1 hour, obtains volatile oil of Lignum Dalbergiae Odoriferae 3.60g from separating still.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103636821A (en) * | 2013-12-06 | 2014-03-19 | 凤台县新大食用油脂有限公司 | Rice bran oil capable of calming liver, clearing internal heat and regulating internal secretion |
| CN103636817A (en) * | 2013-12-06 | 2014-03-19 | 凤台县新大食用油脂有限公司 | Rice bran oil capable of protecting liver, improving eyesight and promoting digestion |
| CN107287035A (en) * | 2017-08-09 | 2017-10-24 | 中国热带农业科学院农产品加工研究所 | A kind of preparation method for dropping the essential oil that smells good |
| CN108634236A (en) * | 2018-05-16 | 2018-10-12 | 浙江海润达科技有限公司 | A kind of preparation method of ultralow fat activity squid-soybean mixing peptide oral liquid |
| CN111013190A (en) * | 2020-01-14 | 2020-04-17 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon leaves |
| CN111228851A (en) * | 2020-01-14 | 2020-06-05 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon bark |
| CN114774202A (en) * | 2022-06-22 | 2022-07-22 | 海南众志承生物科技有限公司 | Preparation method of Hainan Huanghua pear essential oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470255A (en) * | 2002-07-22 | 2004-01-28 | 王智民 | Preparation extracted from the root of red-rooted solvia and pseudo-ginseng and its compound preparation and medical use |
| CN101023983A (en) * | 2006-02-23 | 2007-08-29 | 山东绿叶天然药物研究开发有限公司 | Medicine composition and use |
| CN101085005A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力制药股份有限公司 | Traditional Chinese medicinal composition containing red sage root, ligusticum wallichii and dalbergia oil and its preparation |
| CN101190281A (en) * | 2006-11-27 | 2008-06-04 | 杭州尤美特科技有限公司 | Prune tree extract and preparation method and application thereof |
-
2010
- 2010-02-03 CN CN2010101048226A patent/CN102138960A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470255A (en) * | 2002-07-22 | 2004-01-28 | 王智民 | Preparation extracted from the root of red-rooted solvia and pseudo-ginseng and its compound preparation and medical use |
| CN101023983A (en) * | 2006-02-23 | 2007-08-29 | 山东绿叶天然药物研究开发有限公司 | Medicine composition and use |
| CN101085005A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力制药股份有限公司 | Traditional Chinese medicinal composition containing red sage root, ligusticum wallichii and dalbergia oil and its preparation |
| CN101190281A (en) * | 2006-11-27 | 2008-06-04 | 杭州尤美特科技有限公司 | Prune tree extract and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘海燕等: "降香挥发油研究进展", 《中草药》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103636821A (en) * | 2013-12-06 | 2014-03-19 | 凤台县新大食用油脂有限公司 | Rice bran oil capable of calming liver, clearing internal heat and regulating internal secretion |
| CN103636817A (en) * | 2013-12-06 | 2014-03-19 | 凤台县新大食用油脂有限公司 | Rice bran oil capable of protecting liver, improving eyesight and promoting digestion |
| CN103636817B (en) * | 2013-12-06 | 2015-12-02 | 凤台县新大食用油脂有限公司 | A kind of have the rice bran oil that liver-nourishing and eyesight-improving urgees to digest effect |
| CN103636821B (en) * | 2013-12-06 | 2015-12-02 | 凤台县新大食用油脂有限公司 | A kind of have flat liver and relieve inflammation or internal heat and regulate the rice bran oil of endocrine effect |
| CN107287035A (en) * | 2017-08-09 | 2017-10-24 | 中国热带农业科学院农产品加工研究所 | A kind of preparation method for dropping the essential oil that smells good |
| CN108634236A (en) * | 2018-05-16 | 2018-10-12 | 浙江海润达科技有限公司 | A kind of preparation method of ultralow fat activity squid-soybean mixing peptide oral liquid |
| CN108634236B (en) * | 2018-05-16 | 2021-07-30 | 浙江海润达科技有限公司 | Preparation method of ultra-low fat active squid-soybean mixed peptide oral liquid |
| CN111013190A (en) * | 2020-01-14 | 2020-04-17 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon leaves |
| CN111228851A (en) * | 2020-01-14 | 2020-06-05 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon bark |
| CN111228851B (en) * | 2020-01-14 | 2021-03-09 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon bark |
| CN114774202A (en) * | 2022-06-22 | 2022-07-22 | 海南众志承生物科技有限公司 | Preparation method of Hainan Huanghua pear essential oil |
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Application publication date: 20110803 |