CN101019908A - Supercritical extraction process of water extracted and alcohol deposited safflower residue - Google Patents
Supercritical extraction process of water extracted and alcohol deposited safflower residue Download PDFInfo
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- CN101019908A CN101019908A CN 200710061611 CN200710061611A CN101019908A CN 101019908 A CN101019908 A CN 101019908A CN 200710061611 CN200710061611 CN 200710061611 CN 200710061611 A CN200710061611 A CN 200710061611A CN 101019908 A CN101019908 A CN 101019908A
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Abstract
The supercritical extraction process of water extracted and alcohol deposited safflower residue includes low temperature drying the safflower residue at 60 deg.c; the first supercritical CO2 extracting at 8-12 MPa and 35-60 deg.c, the first separation at 8-10 MPa and 0-12 deg.c to obtain vegetable wax and the second separation at 1-6 MPa and 20-45 deg.c to obtain volatile safflower oil; the second extracting at 22-32 MPa and 35-60 deg.c, and separation at 2-6 MPa and 20-40 deg.c to obtain macromolecular non-polar matter. The present invention utilizes the non-polar matter in safflower effectively, realizes the initial separation of different kinds of matter and raises the comprehensive economic value of safflower processing.
Description
Technical field
The invention belongs to and use supercritical C0
2The method of contained volatile oil and macromole apolar substance in the safflower extracting water extract-alcohol precipitation medicinal residues.
Background technology
Flos Carthami is the tubular flower of Compositae-year this plant of SHENGCAO Flos Carthami (Carthamus tinctorius L.), establishing in large scale is arranged, aboundresources on Xinjiang of China Sichuan and other places.Studies show that Flos Carthami preparation such as Flos Carthami injection or oral liquid can be used to treat diseases such as metremia, cardiovascular, thrombosis, also make pain relieving, antiinflammatory, obtain a large amount of application clinically.
In producing Flos Carthami injection or oral liquid process, mainly adopt aqueous extraction-alcohol precipitation technology, produce a large amount of medicinal residues.On the one hand, medicinal residues are generally moist material, very easily addle, its flavor is strange, and is even more serious in summer, so medicinal residues should in time transport production plant area, pollute otherwise easily cause producing medicine and plant environment, even, also can pollute environment if transport mishandlingly; On the other hand, also there is a certain amount of active component in Chinese crude drug such as Flos Carthami usually through the medicinal residues after extracting, decocting.There are some researches show and contain chemical constituents such as amounts of protein, aminoacid, inorganic elements in the medicinal residues, and, also contain some effective ingredients, have value of exploiting and utilizing according to the difference of production technology.Supercritical carbon dioxide has very strong solvability, can easily regulate solubility property by changing operating parameter, is particularly suitable for the extraction of apolar substance, is to utilize one of water extract-alcohol precipitation medicinal residues effective way.Utilize supercritical carbon dioxide to the water extracted and alcohol deposited safflower residue grading extraction, can realize the efficient utilization of resource.The domestic patent that medicinal residues are utilized has at present: CN1793318A is the production method of the culture medium of edible fungus of raw material with the Chinese medicine slag.Shang Weiyou uses supercritical extraction technique further efficiently to utilize the method for water extract-alcohol precipitation medicinal residues Chinese medicine effective ingredient.
Summary of the invention
The objective of the invention is at above-mentioned deficiency, the method that a kind of technological process is simple, fully utilize effective ingredient in the water extracted and alcohol deposited safflower residue is provided.
As follows to method of the present invention:
(1). the water extracted and alcohol deposited safflower residue powder particle diameter is 0.15mm-1mm, cold drying below 60 ℃;
(2). with water extracted and alcohol deposited safflower residue with supercritical carbon dioxide as extractant, is 8-12MPa at pressure, temperature is to carry out the supercritical extraction first time under 35-60 ℃ the condition;
(3). extract carries out two-stage decompression separation for the first time, and flash trapping stage pressure is 8-10MPa, and temperature is 0-12 ℃, separates to obtain vegetable wax; The secondary separating pressure is 1-6MPa, and temperature is 20-45 ℃, obtains Flos Carthami volatile oil;
(4). boost to 22-32Mpa behind the supercritical extraction for the first time, temperature is under 35-60 ℃ the condition raffinate to be carried out the extraction second time, extract is 2-6MPa at separating pressure for the second time, and temperature is to carry out the second time under the 20-40 ℃ of condition to separate, and obtains the macromole apolar substance.
Advantage of the present invention:
1. utilize supercritical carbon dioxide extraction to obtain Flos Carthami volatile oil;
2. effectively utilized the apolar substance in the Flos Carthami;
3. realized the initial gross separation of heterogeneity material;
4. the mixed economy that has increased Chinese medicine processing is worth.
Description of drawings
Fig. 1 is a process chart of the present invention.
As shown in the figure, carbon dioxide enters carbon dioxide condensing tank 2 from gas tank 1 and is condensed into liquid, Inject the extraction that installs in advance the water extracted and alcohol deposited safflower residue of pulverizing drying from the bottom by high-pressure pump 3 Get tank 5, by water bath with thermostatic control 4 control extraction temperature, counterbalance valve 6 controlled pressures, under low pressure Water extracted and alcohol deposited safflower residue after processing is carried out the extraction first time, fallen step by step by counterbalance valve control Press, the CO 2 fluid that carries Flos Carthami volatile oil is sent to knockout drum 7,8 carries out the A second-order separation, supercritical carbon dioxide density reduces, and solute separates step by step with extractant, Obtain respectively wax component and Flos Carthami volatile oil. Controlled pressure is under high pressure to the safflower water extracting alcohol Heavy dregs of a decoction raffinate thing carries out the extraction second time, carries out separating the second time at knockout drum 9 and is divided greatly Sub-apolar substance. Extraction finishes that carbon dioxide enters tail gas tank 10 in the extractor 5, through gas Pump 11 is got back to the extraction systemic circulation and is used.
The specific embodiment
Embodiment 1: get water extracted and alcohol deposited safflower residue 100 grams, be crushed to 0.15mm-1mm, cold drying below 60 ℃ is placed in the extractor 5 and sealing.Open gas tank 1, carbon dioxide arrives extractors 5 through drainer 2, high-pressure pump 3, carries out extracting first time under 8MPa, 60 ℃.Extract enters flash trapping stage jar 7, carries out flash trapping stage and obtain the Flos Carthami vegetable wax under 8MPa, 12 ℃.Carbon dioxide continues to enter secondary knockout drum 8, and 6MPa, 45 ℃ of secondarys are isolated Flos Carthami volatile oil.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 2 hours, obtain Flos Carthami volatile oil 1.7 grams, vegetable wax 0.06g from knockout drum.Rising pressure is to 25mpa, carries out the water extracted and alcohol deposited safflower residue raffinate is extracted for the second time under 35 ℃ of temperature.Extract enters knockout drum 7 and carries out the separation second time, knockout drum pressure 2MPa, 20 ℃ of temperature.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 6 hours, obtain Flos Carthami apolar substance 4.2 grams from knockout drum 7.
Embodiment 2: get water extracted and alcohol deposited safflower residue 100 grams, be crushed to 0.15mm-1mm, cold drying below 60 ℃ is placed in the extractor 5 and sealing.Open gas tank 1, carbon dioxide arrives extractors 5 through drainer 2, high-pressure pump 3, carries out extracting first time under 10MPa, 45 ℃.Extract enters flash trapping stage jar 7, carries out flash trapping stage and obtain the Flos Carthami vegetable wax under 9MPa, 8 ℃.Carbon dioxide continues to enter secondary knockout drum 8, and 1MPa, 20 ℃ of secondarys are isolated Flos Carthami volatile oil.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 6 hours, obtain Flos Carthami volatile oil 2.4 grams, vegetable wax 0.08g from knockout drum.Rising pressure is to 28mpa, under 45 ℃ of temperature the water extracted and alcohol deposited safflower residue raffinate carried out the extraction second time.Extract enters knockout drum 7 and carries out the separation second time, knockout drum pressure 4MPa, 30 ℃ of temperature.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 6 hours, obtain Flos Carthami apolar substance 3.6 grams from knockout drum 7.
Embodiment 3: get water extracted and alcohol deposited safflower residue 100 grams, be crushed to 0.15mm-1mm, cold drying below 60 ℃ is placed in the extractor 5 and sealing.Open gas tank 1, carbon dioxide arrives extractors 5 through drainer 2, high-pressure pump 3, carries out extracting first time under 12MPa, 35 ℃.Extract enters flash trapping stage jar 7, carries out flash trapping stage and obtain the Flos Carthami vegetable wax under 10MPa, 12 ℃.Carbon dioxide continues to enter secondary knockout drum 8, and 4MPa, 30 ℃ of secondarys are isolated Flos Carthami volatile oil.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 6 hours, obtain Flos Carthami volatile oil 3.5 grams, vegetable wax 0.08g from knockout drum.Rising pressure is to 32mpa, under 60 ℃ of temperature the water extracted and alcohol deposited safflower residue raffinate carried out the extraction second time.Extract enters knockout drum 7 and carries out the separation second time, knockout drum pressure 6MPa, 40 ℃ of temperature.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 6 hours, obtain Flos Carthami apolar substance 4.5 grams from knockout drum 7.
Embodiment 4: get water extracted and alcohol deposited safflower residue 100 grams, be crushed to 0.15mm-1mm, 60 ℃ of following cold drying are placed in the extractor 5 and sealing.Open gas tank 1, carbon dioxide arrives extractors 5 through drainer 2, high-pressure pump 3, carries out extracting first time under 9MPa, 35 ℃.Extract enters flash trapping stage jar 7, carries out flash trapping stage and obtain the Flos Carthami vegetable wax under 10MPa, 12 ℃.Carbon dioxide continues to enter secondary knockout drum 8, and 4MPa, 30 ℃ of secondarys are isolated Flos Carthami volatile oil.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 7 hours, obtain Flos Carthami volatile oil 3.2 grams, vegetable wax 0.08g from knockout drum.Rising pressure is to 22mpa, under 40 ℃ of temperature the water extracted and alcohol deposited safflower residue raffinate carried out the extraction second time.Extract enters knockout drum 7 and carries out the separation second time, knockout drum pressure 6MPa, 40 ℃ of temperature.Separate the clean CO 2 fluid in back through in device, recycling after the condenser condenses.Behind the dynamic operation 5 hours, obtain Flos Carthami apolar substance 4.3 grams from knockout drum 7.
Claims (1)
1, a kind of method of supercritical safflower extracting water extract-alcohol precipitation medicinal residues is characterized in that comprising the steps:
(1). the water extracted and alcohol deposited safflower residue powder particle diameter is 0.15mm-1mm, cold drying below 60 ℃;
(2). with water extracted and alcohol deposited safflower residue with supercritical carbon dioxide as extractant, is 8-12MPa at pressure, temperature is to carry out the supercritical extraction first time under 35-60 ℃ the condition;
(3). extract carries out two-stage decompression separation for the first time, and flash trapping stage pressure is 8-10MPa, and temperature is 0-12 ℃, separates to obtain vegetable wax; The secondary separating pressure is 1-6MPa, and temperature is 20-45 ℃, obtains Flos Carthami volatile oil;
(4). boost to 22-32Mpa behind the supercritical extraction for the first time, temperature is under 35-60 ℃ the condition raffinate to be carried out the extraction second time, extract is 2-6MPa at separating pressure for the second time, and temperature is to carry out the second time under the 20-40 ℃ of condition to separate, and obtains the macromole apolar substance.
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| CN 200710061611 CN101019908A (en) | 2007-03-20 | 2007-03-20 | Supercritical extraction process of water extracted and alcohol deposited safflower residue |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007570A (en) * | 2012-12-10 | 2013-04-03 | 刘东波 | Integrated method for dehydrating traditional Chinese medicine materials, extracting essential oil and preparing essential oil |
| CN103421599A (en) * | 2013-07-31 | 2013-12-04 | 安徽省霍山县聚一科技有限公司 | Camellia oil preparation system and operation method thereof |
| CN105998112A (en) * | 2016-06-27 | 2016-10-12 | 四川省中医药科学院 | Method for preparing vegetable drug volatile oil from waste decoction dregs |
-
2007
- 2007-03-20 CN CN 200710061611 patent/CN101019908A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007570A (en) * | 2012-12-10 | 2013-04-03 | 刘东波 | Integrated method for dehydrating traditional Chinese medicine materials, extracting essential oil and preparing essential oil |
| CN103007570B (en) * | 2012-12-10 | 2016-03-02 | 刘东波 | A kind of method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil |
| CN103421599A (en) * | 2013-07-31 | 2013-12-04 | 安徽省霍山县聚一科技有限公司 | Camellia oil preparation system and operation method thereof |
| CN105998112A (en) * | 2016-06-27 | 2016-10-12 | 四川省中医药科学院 | Method for preparing vegetable drug volatile oil from waste decoction dregs |
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Open date: 20070822 |