CN101433562A - Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof - Google Patents
Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing ginkgo leaf extract powder by drying supercritical fluid and a device thereof. The method comprises the following steps: placing alcoholic solution of ginkgo leaf extract without impurity into a sealed dry chamber cylinder body, and then introducing carbon dioxide into the solution at a flow speed of 20 to 45 liters per hour, wherein temperature of the carbon dioxide is between 0 and 5 DEG C; controlling pressure of the dry chamber cylinder body at 10 to 30MPa and temperature of between 35 and 75 DEG C; and after the carbon dioxide becomes stable supercritical fluid, continuously displacing and drying the fluid for 4 to 8 hours to finally obtain light-yellow dry finished powder of the ginkgo leaf extract. The device comprises a carbon dioxide steel bottle, a gas-liquid separation container, a gas cooling unit, a transition container, a carbon dioxide transfer pump, a heater, the dry chamber cylinder body, a first-stage separation cylinder body, a second-stage separation cylinder body, valves and pipelines, and the components are mutually connected through the valves and the pipelines. The content of flavone in obtained power is more than 25 weight percent, the alcoholic solution in the extract can be reclaimed, and the carbon dioxide can also be recycled.
Description
Technical field
The present invention relates to a kind of drying means of Folium Ginkgo extract, particularly a kind of dry method for preparing ginkgo leaf extract powder of supercritical fluid of utilizing.
Background technology
Semen Ginkgo is a deciduous tree, and the height of tree reaches 40m.Its branch has the long and short two kind, and leaf clusters on brachyplast, alternate on long shoot.Blade is fan-shaped, long 4～8cm, and 2 shallow splitting in the middle of the wide 5～10cm, tip, the base portion wedge shape, vein is parallel, the fork-shaped difference.Compendium of Material Medica is put down in writing its leaf and is had very high medical value, and nature and flavor sweetness and bitterness and puckery is gone into lung, kidney two warps, has that relieving asthma and cough, leukorrhagia stopping are turbid, the effect of urine reducing.The composition of Folium Ginkgo comprises distinctive flavonoid, terpenes and the ginkgoic acid that can cause allergic reaction, and these ginkgetins-glucoside composition has powerful antioxidation and free radical ability.Studies show that Folium Ginkgo extract can be used for the treatment of memory and lose stomach pain, dysentery, hypertension, psychentonia and respiratory problems such as asthma, bronchitis and poor circulation and the anxiety that causes thereof.
Because Folium Ginkgo extract has very high medical value, so, domestic and international research personnel spent a large amount of research carried out the Folium Ginkgo extraction process with and the research of pharmacology, few people study the influence of dry effective ingredient to such extract.Traditional drying means has spray drying and freezing and grind etc., and still, spray drying is owing to adopted high temperature air, and a lot of biological activitys are destroyed in dry run, and causing thereafter, medical value reduces.Adopt lyophilization to pass through and grind, so the product cut size that comes out distribution is wide, granule is irregular, and the energy consumption height of dry run.In recent years, supercritical fluid has obtained extensive studies and application owing to have characteristic in fields such as reaction, hydrolysis, dryings.Because do not have the tension force on surface under super critical condition, there is not the change of the microstructure that causes because of the effect of capillary sheet surface tension in the material that is dried yet.Though the existing report of supercritical drying device, but, different with the supercritical drying device of the present invention's utilization, for example, application number be 200710064875.8 patent about supercritical drying device, relate generally to the sacrifice layer release tech field of the MEMS key manufacture in the microelectric technique, supercritical drying chamber, be used for the release of sacrifice layer, form by reaction under high pressure chamber and temperature-controlled chamber; The reaction under high pressure chamber is used to hold the silicon chip support, and carbon dioxide replacement and the exsiccant reative cell of gasification are provided.Application (patent) number: 00812047.1 patent has also been narrated the above-mentioned exsiccant supercritical drying drying system of wafer that similarly is used for.Application (patent) number: the supercritical drying device of 02295010.9 narration not have in the back of hothouse to add relevant two-stage decompression still, and system is wayward, and the carbon dioxide waste seriously.
Though introduced a kind of supercritical drying and prepared SO and application number is 200410016977.9 patent
4 2-/ TiO
2Method, it utilizes the mixed solution of sulphuric acid-alcohol-water slowly to splash into butyl titanate-alcoholic solution, obtains the TiO2 colloidal sol of homogeneous transparent; With resulting colloidal sol ageing, obtain wet gel again; Wet gel and ethanol in inert atmosphere, under the super critical condition, are placed 0.5～8h, cooling, roasting again then could obtain SO
4 2-/ TiO
2Dry finished product is not the supercritical drying on the just sincere justice.Application (patent) number: 200410155314.5 patent prepares the method for nano magnesia with supercritical drying, and last the needs equally adopts high-temperature roasting obtain dry finished product powder.
This shows, though supercritical drying device has report to be used to the drying of inorganic salt material, the preparation of special nano material, but do not see the utilization supercritical drying so far for Folium Ginkgo extract or the drying of similar extract and the report or the patent of associated process conditions thereof, and relevant supercritical device is also different with the supercritical drying Process configuration that the present invention uses.To sum up, utilize preparing ginkgo leaf extract powder using supercritical liquid desiccation that the technology report of present patent application is not arranged at present.
Summary of the invention
It is destroyed easily and supercritical drying is wayward, carbon dioxide waste important disadvantages to the present invention is directed to effective ingredient that the high temperature drying method exists, propose a kind of method and device thereof, have the advantage that method is simple, with low cost, do not destroy effective ingredient with preparing ginkgo leaf extract powder using supercritical liquid desiccation.
Technical scheme of the present invention is: a kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, the alcoholic solution of pure Folium Ginkgo extract is placed in the hothouse cylinder body of sealing, flow velocity with 20L/h-45L/h feeds carbon dioxide then, the temperature of carbon dioxide is 0 ℃～5 ℃, control hothouse cylinder pressure is 35 ℃～75 ℃ in 10-30MPa, temperature, after carbon dioxide becomes stable supercritical fluid, replace dry 4h-8h then continuously, finally obtain the dry finished product powder of flaxen Folium Ginkgo extract.Wherein the alcoholic solution of pure Folium Ginkgo extract is that alcoholic solution with Folium Ginkgo extract adopts 1000 purpose screen filtrations to remove impurity.Can directly use the alcoholic solution of pure Folium Ginkgo extract, also can be with the alcoholic solution elder generation process evaporation and concentration of Folium Ginkgo extract, the liquid that is concentrated to the solid content about 30%wt enters the hothouse drying again, and is faster like this.After the carbon dioxide in the hothouse becomes stable supercritical fluid, start firsts and seconds and separate cylinder body, the pressure that the control firsts and seconds separates cylinder body is that 3.5MPa-5.0MPa, temperature are 20 ℃～40 ℃.Ethanol in the alcoholic solution of Folium Ginkgo extract can recycling.Carbon dioxide after the use re-uses after separating in gas-liquid separator behind the ethanol and merging with the carbon dioxide that newly enters.
The described employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, comprise carbon dioxide steel cylinder, the gas-liquid separation container, the gas cooled unit, transition container, the carbon dioxide delivery pump, heater, the hothouse cylinder body, the flash trapping stage cylinder body, secondary separates cylinder body, valve and pipeline, each several part interconnects by valve and pipeline, carbon dioxide steel cylinder is connected with gas-liquid separator, gas-liquid separator is connected with the air-turbocooler group, the gas cooled unit is connected with transition container, transition container is connected with the carbon dioxide delivery pump, the carbon dioxide delivery pump is connected with heater, heater is connected with the hothouse cylinder body, the hothouse cylinder body is connected with the flash trapping stage cylinder body, and the flash trapping stage cylinder body separates cylinder body with secondary and is connected, and secondary separates the gentle liquid/gas separator of cylinder body and connects.Hothouse cylinder body, flash trapping stage cylinder body, secondary splitter cylinder be external to be equipped with the hot water jacket, links to each other with heater by pipeline.
When dry, open the drain tap of carbon dioxide steel cylinder earlier, starting the gas cooled unit cools off carbon dioxide, make carbon dioxide be cooled to 0 ℃～5 ℃, close the outlet valve of hothouse cylinder body, start the carbon dioxide delivery pump then, carbon dioxide is gently sent in the hothouse cylinder body, keep pressure at 10MPa-30MPa, start the heater heating simultaneously, by the hot water jacket hothouse cylinder body is separated the cylinder body heating with firsts and seconds, wherein the intravital holding temperature of hothouse cylinder is about 35 ℃-75 ℃, and the intravital temperature maintenance of splitter cylinder is about 20 ℃-40 ℃; When carbon dioxide become supercritical fluid and keep stablize 0.5h after, slowly open the valve valve behind the hothouse cylinder body separates cylinder body with two after, make the intravital pressure of splitter cylinder maintain 3.5MPa-5.0MPa, control the flow of carbon dioxide delivery pump simultaneously, be controlled at 20L/h-40L/h, keep continuous drying 4-8h, promptly finished whole dry run, after having closed relevant valve and having stopped delivery pump etc., can open the exhaust-valve on the hothouse cylinder body, lay down the top cover of cylinder body then, dried Folium Ginkgo extract is poured in the packaging bag, if the drying solid in packaging bag also has a small amount of fritter, can be broken with the have gentle hands pine.
Beneficial effect:
(1) the present invention has adopted supercritical carbon dioxide fluid to replace spirit solvent, reach the liquid dried purpose, eliminated the solvent in the high-temperature gas evaporating liquid of conventional drying, high-temperature gas is to the destructive shortcoming of effective ingredient, the problem that has existed the duct to subside in the microstructure of the dry products of energy consumption height, acquisition when also having avoided adopting lyophilization.
(2) ginkgo leaf extract powder that adopts supercritical drying of the present invention to obtain has kept original high activity composition, and for example, flavones content has reached more than the 25%wt.Exsiccant fineness of powder is even, narrow diameter distribution, and mean diameter is little, and does not have the duct collapse phenomenon that exists in the finished product of conventional drying.
(3) the present invention is in order further to improve separating carbon dioxide and spirit solvent, behind described hothouse cylinder body, be provided with two-stage and separate cylinder body, can multistage release, can fully separate the ethanol that supercritical carbon dioxide fluid carries out, thereby guaranteed the abundant separation of gas-liquid, residual alcohol content is less than 8%wt in the powder body.
(4) the present invention has adopted the technology that carbon dioxide recycles, carbon dioxide after the use separates in gas-liquid separator behind the ethanol and after the new carbon dioxide merging and re-uses, thereby reduced the consumption of carbon dioxide, isolated ethanol also can recycling.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is the particle size distribution figure of the Folium Ginkgo extract dried powder that obtains of the present invention
The specific embodiment
Below in conjunction with Fig. 1, Fig. 2, the present invention is elaborated:
A kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, the alcoholic solution of pure Folium Ginkgo extract is placed in the hothouse cylinder body of sealing, flow velocity with 20L/h-45L/h feeds carbon dioxide then, the temperature of carbon dioxide is 0 ℃～5 ℃, control hothouse cylinder pressure is 35 ℃～75 ℃ in 10-30MPa, temperature, after carbon dioxide becomes stable supercritical fluid, replace dry 4h-8h then continuously, finally obtain the dry finished product powder of flaxen Folium Ginkgo extract.After the carbon dioxide in the hothouse becomes stable supercritical fluid, start firsts and seconds and separate cylinder body, the pressure that the control firsts and seconds separates cylinder body is that 3.5MPa-5.0MPa, temperature are 20 ℃～40 ℃.Ethanol in the alcoholic solution of Folium Ginkgo extract can recycling.Carbon dioxide after the use re-uses after separating in gas-liquid separator behind the ethanol and merging with the carbon dioxide that newly enters.The recycling after entering gas-liquid separator separates behind the carbon dioxide replacement of ethanol in the alcoholic solution of Folium Ginkgo extract.The alcoholic solution of described pure Folium Ginkgo extract is that the alcoholic solution with Folium Ginkgo extract adopts 1000 purpose screen filtrations to remove impurity.Can directly use the alcoholic solution of pure Folium Ginkgo extract, also can be with the alcoholic solution elder generation process evaporation and concentration of Folium Ginkgo extract, the liquid that is concentrated to the solid content about 30%wt enters the hothouse drying again, and is faster like this.
The described employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, comprise carbon dioxide steel cylinder 1, gas-liquid separation container 2, gas cooled unit 3, transition container 4, carbon dioxide delivery pump 5, heater 6, hothouse cylinder body 7, flash trapping stage cylinder body 8, secondary separates cylinder body 9, valve and pipeline, each several part interconnects by valve and pipeline, carbon dioxide steel cylinder 1 is connected with gas-liquid separator 2, gas-liquid separator 2 is connected with air-turbocooler group 3, gas cooled unit 3 is connected with transition container 4, transition container 4 is connected with carbon dioxide delivery pump 5, carbon dioxide delivery pump 5 is connected with heater 6, heater 6 is connected with hothouse cylinder body 7, hothouse cylinder body 7 is connected with flash trapping stage cylinder body 8, flash trapping stage cylinder body 8 separates cylinder body 9 with secondary and is connected, and secondary separates cylinder body 9 and is connected with gas-liquid separator 2.Be equipped with the hot water jacket outside hothouse cylinder body 7, flash trapping stage cylinder body 8, the secondary separation cylinder body 9, link to each other with heater 6 by pipeline.
When dry, open the drain tap of carbon dioxide steel cylinder earlier, starting the gas cooled unit cools off carbon dioxide, make carbon dioxide be cooled to 0 ℃～5 ℃, close the outlet valve of hothouse cylinder body, start the carbon dioxide delivery pump then, carbon dioxide is gently sent in the hothouse cylinder body, keep pressure at 10MPa-30MPa, start the heater heating simultaneously, by the hot water jacket hothouse cylinder body is separated the cylinder body heating with firsts and seconds, wherein the intravital holding temperature of hothouse cylinder is about 35 ℃-75 ℃, and the intravital temperature maintenance of splitter cylinder is about 20 ℃-40 ℃; When carbon dioxide become supercritical fluid and keep stablize 0.5h after, slowly open the valve valve behind the hothouse cylinder body separates cylinder body with two after, make the intravital pressure of splitter cylinder maintain 3.5MPa-5.0MPa, control the flow of carbon dioxide delivery pump simultaneously, be controlled at 20L/h-40L/h, keep continuous drying 4-8h, promptly finished whole dry run, after having closed relevant valve and having stopped delivery pump etc., can open the exhaust-valve on the hothouse cylinder body, lay down the top cover of cylinder body then, dried Folium Ginkgo extract is poured in the packaging bag, if the drying solid in packaging bag also has a small amount of fritter, can be broken with the have gentle hands pine.
A kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation is to be realized by the supercritical drying device that a cover band carbon dioxide recycles.Raw material is the alcoholic solution of the Folium Ginkgo extract of 130g and spirituosity 90%wt.The pressure of supercritical carbon dioxide in hothouse cylinder body 7 need be controlled at 10MPa, by heater 6 dry kiln cylinder bodies 7 and flash trapping stage cylinder body 8, hot water among the hot water jacket of secondary separation cylinder body 9, temperature in the hothouse cylinder body 7 is controlled at 40 ℃, temperature in the flash trapping stage cylinder body 8 is controlled at 30 ℃, the temperature that secondary separates in the cylinder body 9 is controlled at 20 ℃, open valve and be cooled to 0 ℃-5 ℃ from the carbon dioxide of carbon dioxide steel cylinder 1 through freezing unit 3 afterwards, be transported to continuously in the hothouse cylinder body 7 by carbon dioxide delivery pump 5 through transition container 4 backs, valve behind the hothouse cylinder body 7 is in closed condition at this moment, after carbon dioxide becomes supercritical fluid and stable 0.5h, open hothouse cylinder body 7 and flash trapping stage cylinder body 8 again, secondary separates the valve behind the cylinder body 9, control valve, make the flow-control of the carbon dioxide carried by carbon dioxide delivery pump 5 at 35L/h, adjustment separates the valve opening behind the cylinder body, make that the pressure in the flash trapping stage cylinder body 8 is 4.7MPa, the pressure that secondary separates cylinder body 9 is 4.0MPa, move 4.5h continuously by above-mentioned state, whole dry run is finished.At this moment, can open the valve of hothouse cylinder base or open the dried powder that the gland on hothouse cylinder body top takes out.From secondary separate displacement that cylinder body 9 comes out the Folium Ginkgo extract alcoholic solution carbon dioxide of ethanol enter gas-liquid separator 2 and separate, the ethanol of separating from carbon dioxide can reclaim by the valve of gas-liquid separation inferior part of the cylinder block.Also have part ethanol can separate the valve recovery of cylinder body 9 bottoms with secondary in the dry run by flash trapping stage cylinder body 8.
The good fluidity of dried powder, the flavones content that detects in the powder body is 25.8%wt, remaining alcohol content is less than 8%wt.The particle size distribution of product as shown in Figure 2, the particle diameter of visible entire product is between 1 μ m-65 μ m, mean diameter is 28.4 μ m, narrower than the spray-dired distribution of particles (1 μ m-125 μ m) of routine, (70 μ m-80 μ m) is little for mean diameter.
A kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, the alcoholic solution of pure Folium Ginkgo extract is placed in the hothouse cylinder body of sealing, flow velocity with 20L/h feeds carbon dioxide then, the temperature of carbon dioxide is 0 ℃, control hothouse cylinder pressure is 60 ℃ in 13MPa, temperature, after carbon dioxide becomes stable supercritical fluid, replace dry 4h then continuously, finally obtain the dry finished product powder of flaxen Folium Ginkgo extract.After the carbon dioxide in the hothouse becomes stable supercritical fluid, start firsts and seconds and separate cylinder body, the pressure that the control firsts and seconds separates cylinder body is that 3.5MPa, temperature are 20 ℃.Ethanol in the alcoholic solution of Folium Ginkgo extract can recycling.Carbon dioxide after the use re-uses after separating in gas-liquid separator behind the ethanol and merging with the carbon dioxide that newly enters.The recycling after entering gas-liquid separator separates behind the carbon dioxide replacement of ethanol in the alcoholic solution of Folium Ginkgo extract.The alcoholic solution of described pure Folium Ginkgo extract is that the alcoholic solution with Folium Ginkgo extract adopts 1000 purpose screen filtrations to remove impurity.Can directly use the alcoholic solution of pure Folium Ginkgo extract, also can be with the alcoholic solution elder generation process evaporation and concentration of Folium Ginkgo extract, the liquid that is concentrated to the solid content about 30%wt enters the hothouse drying again, and is faster like this.
The described employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, comprise carbon dioxide steel cylinder 1, gas-liquid separation container 2, gas cooled unit 3, transition container 4, carbon dioxide delivery pump 5, heater 6, hothouse cylinder body 7, flash trapping stage cylinder body 8, secondary separates cylinder body 9, valve and pipeline, each several part interconnects by valve and pipeline, carbon dioxide steel cylinder 1 is connected with gas-liquid separator 2, gas-liquid separator 2 is connected with air-turbocooler group 3, gas cooled unit 3 is connected with transition container 4, transition container 4 is connected with carbon dioxide delivery pump 5, carbon dioxide delivery pump 5 is connected with heater 6, heater 6 is connected with hothouse cylinder body 7, hothouse cylinder body 7 is connected with flash trapping stage cylinder body 8, flash trapping stage cylinder body 8 separates cylinder body 9 with secondary and is connected, and secondary separates cylinder body 9 and is connected with gas-liquid separator 2.Be equipped with the hot water jacket outside hothouse cylinder body 7, flash trapping stage cylinder body 8, the secondary separation cylinder body 9, link to each other with heater 6 by pipeline.
When dry, open the drain tap of carbon dioxide steel cylinder earlier, starting the gas cooled unit cools off carbon dioxide, make carbon dioxide be cooled to 0 ℃, close the outlet valve of hothouse cylinder body, start the carbon dioxide delivery pump then, carbon dioxide is gently sent in the hothouse cylinder body, keep pressure at 13MPa, start the heater heating simultaneously, by the hot water jacket hothouse cylinder body is separated the cylinder body heating with firsts and seconds, wherein the intravital holding temperature of hothouse cylinder is about 60 ℃, and the intravital temperature maintenance of firsts and seconds splitter cylinder is at 20 ℃～30 ℃; When carbon dioxide become supercritical fluid and keep stablize 0.5h after, slowly open the valve valve behind the hothouse cylinder body separates cylinder body with two after, make the intravital pressure of splitter cylinder maintain 3.5MPa, control the flow of carbon dioxide delivery pump simultaneously, be controlled at 20L/h, keep continuous drying 6h, promptly finished whole dry run, after having closed relevant valve and having stopped delivery pump etc., can open the exhaust-valve on the hothouse cylinder body, lay down the top cover of cylinder body then, dried Folium Ginkgo extract is poured in the packaging bag, if the drying solid in packaging bag also has a small amount of fritter, can be broken with the have gentle hands pine.
Embodiment 3
A kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, the alcoholic solution of pure Folium Ginkgo extract is placed in the hothouse cylinder body of sealing, flow velocity with 45L/h feeds carbon dioxide then, the temperature of carbon dioxide is 5 ℃, control hothouse cylinder pressure is 75 ℃ in 30MPa, temperature, after carbon dioxide becomes stable supercritical fluid, replace dry 8h then continuously, finally obtain the dry finished product powder of flaxen Folium Ginkgo extract.After the carbon dioxide in the hothouse becomes stable supercritical fluid, start firsts and seconds and separate cylinder body, the pressure that the control firsts and seconds separates cylinder body is that 5.0MPa, temperature are 40 ℃.Ethanol in the alcoholic solution of Folium Ginkgo extract can recycling.Carbon dioxide after the use re-uses after separating in gas-liquid separator behind the ethanol and merging with the carbon dioxide that newly enters.The recycling after entering gas-liquid separator separates behind the carbon dioxide replacement of ethanol in the alcoholic solution of Folium Ginkgo extract.The alcoholic solution of described pure Folium Ginkgo extract is that the alcoholic solution with Folium Ginkgo extract adopts 1000 purpose screen filtrations to remove impurity.Can directly use the alcoholic solution of pure Folium Ginkgo extract, also can be with the alcoholic solution elder generation process evaporation and concentration of Folium Ginkgo extract, the liquid that is concentrated to the solid content about 30%wt enters the hothouse drying again, and is faster like this.
The described employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, comprise carbon dioxide steel cylinder 1, gas-liquid separation container 2, gas cooled unit 3, transition container 4, carbon dioxide delivery pump 5, heater 6, hothouse cylinder body 7, flash trapping stage cylinder body 8, secondary separates cylinder body 9, valve and pipeline, each several part interconnects by valve and pipeline, carbon dioxide steel cylinder 1 is connected with gas-liquid separator 2, gas-liquid separator 2 is connected with air-turbocooler group 3, gas cooled unit 3 is connected with transition container 4, transition container 4 is connected with carbon dioxide delivery pump 5, carbon dioxide delivery pump 5 is connected with heater 6, heater 6 is connected with hothouse cylinder body 7, hothouse cylinder body 7 is connected with flash trapping stage cylinder body 8, flash trapping stage cylinder body 8 separates cylinder body 9 with secondary and is connected, and secondary separates cylinder body 9 and is connected with gas-liquid separator 2.Be equipped with the hot water jacket outside hothouse cylinder body 7, flash trapping stage cylinder body 8, the secondary separation cylinder body 9, link to each other with heater 6 by pipeline.
When dry, open the drain tap of carbon dioxide steel cylinder earlier, starting the gas cooled unit cools off carbon dioxide, make carbon dioxide be cooled to 5 ℃, close the outlet valve of hothouse cylinder body, start the carbon dioxide delivery pump then, carbon dioxide is gently sent in the hothouse cylinder body, keep pressure at 30MPa, start the heater heating simultaneously, by the hot water jacket hothouse cylinder body is separated the cylinder body heating with firsts and seconds, wherein the intravital holding temperature of hothouse cylinder is about 75 ℃, and the intravital temperature maintenance of splitter cylinder is about 40 ℃; When carbon dioxide become supercritical fluid and keep stablize 0.5h after, slowly open the valve valve behind the hothouse cylinder body separates cylinder body with two after, make the intravital pressure of splitter cylinder maintain 5.0MPa, control the flow of carbon dioxide delivery pump simultaneously, be controlled at 40L/h, keep continuous drying 8h, promptly finished whole dry run, after having closed relevant valve and having stopped delivery pump etc., can open the exhaust-valve on the hothouse cylinder body, lay down the top cover of cylinder body then, dried Folium Ginkgo extract is poured in the packaging bag, if the drying solid in packaging bag also has a small amount of fritter, can be broken with the have gentle hands pine.
Claims (6)
1, a kind of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation, it is characterized in that: the alcoholic solution of pure Folium Ginkgo extract is placed in the hothouse cylinder body of sealing, flow velocity with 20L/h-45L/h feeds carbon dioxide then, the temperature of carbon dioxide is 0 ℃～5 ℃, control hothouse cylinder pressure is 35 ℃～75 ℃ in 10-30MPa, temperature, after carbon dioxide becomes stable supercritical fluid, replace dry 4h-8h then continuously, finally obtain the dry finished product powder of flaxen Folium Ginkgo extract.
2, the method with preparing ginkgo leaf extract powder using supercritical liquid desiccation according to claim 1, it is characterized in that after the carbon dioxide in the hothouse becomes stable supercritical fluid, start firsts and seconds and separate cylinder body, the pressure that the control firsts and seconds separates cylinder body is that 3.5MPa-5.0MPa, temperature are 20 ℃～40 ℃.
3, the method with preparing ginkgo leaf extract powder using supercritical liquid desiccation according to claim 1, it is characterized in that the alcoholic solution of described pure Folium Ginkgo extract is that the alcoholic solution with Folium Ginkgo extract adopts 1000 purpose screen filtrations to remove impurity.
4, the method with preparing ginkgo leaf extract powder using supercritical liquid desiccation according to claim 1 is characterized in that, the carbon dioxide separation after the described use is fallen behind the ethanol and to be re-used the ethanol recycling after merging with the carbon dioxide that newly enters.
5, a kind of employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation as claimed in claim 1, it is characterized in that, comprise carbon dioxide steel cylinder (1), gas-liquid separation container (2), gas cooled unit (3), transition container (4), carbon dioxide delivery pump (5), heater (6), hothouse cylinder body (7), flash trapping stage cylinder body (8), secondary separates cylinder body (9), valve and pipeline, each several part interconnects by valve and pipeline, carbon dioxide steel cylinder (1) is connected with gas-liquid separator (2), gas-liquid separator (2) is connected with air-turbocooler group (3), gas cooled unit (3) is connected with transition container (4), transition container (4) is connected with carbon dioxide delivery pump (5), carbon dioxide delivery pump (5) is connected with heater (6), heater (6) is connected with hothouse cylinder body (7), hothouse cylinder body (7) is connected with flash trapping stage cylinder body (8), flash trapping stage cylinder body (8) separates cylinder body (9) with secondary and is connected, and secondary separates cylinder body (9) and is connected with gas-liquid separator (2).
6, the employed device of method with preparing ginkgo leaf extract powder using supercritical liquid desiccation as claimed in claim 5, it is characterized in that, be equipped with the hot water jacket outside hothouse cylinder body (7), flash trapping stage cylinder body (8), the secondary separation cylinder body (9), link to each other with heater (6) by pipeline.
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| CN107441763A (en) * | 2017-09-25 | 2017-12-08 | 太和县三九药业有限公司 | Saussurea involucrata means of supercritical extraction device |
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Family Cites Families (3)
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| US6508259B1 (en) * | 1999-08-05 | 2003-01-21 | S.C. Fluids, Inc. | Inverted pressure vessel with horizontal through loading |
| CN2589914Y (en) * | 2002-12-30 | 2003-12-03 | 石油大学(北京) | Supercritical carbon dioxide drying equipment |
| CN101275806A (en) * | 2007-03-28 | 2008-10-01 | 中国科学院微电子研究所 | Carbon dioxide supercritical drying device |
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|---|---|---|---|---|
| CN102491326A (en) * | 2011-11-30 | 2012-06-13 | 航天特种材料及工艺技术研究所 | Device for drying supercritical fluid and method for preparing aerogel material |
| CN102491326B (en) * | 2011-11-30 | 2014-06-25 | 航天特种材料及工艺技术研究所 | Device for drying supercritical fluid and method for preparing aerogel material |
| CN104482728A (en) * | 2014-10-28 | 2015-04-01 | 浙江工业大学 | Supercritical CO2Method and device for drying valsartan |
| CN106546067A (en) * | 2015-09-18 | 2017-03-29 | 海南椰国食品有限公司 | Bacterial cellulose gel film replaces low temperature integrated dry drying system |
| CN107441763A (en) * | 2017-09-25 | 2017-12-08 | 太和县三九药业有限公司 | Saussurea involucrata means of supercritical extraction device |
| CN108295501A (en) * | 2018-04-04 | 2018-07-20 | 南通市华安超临界萃取有限公司 | A kind of overcritical nanometer drying preparation facilities |
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|---|---|
| CN101433562B (en) | 2011-09-07 |
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Assignee: Wuxi Aobo Purification & Desiccant Air Conditioner Co., Ltd. Assignor: Institute of Chemical Industry of Forest Products, Chinese Academy of Forestry Contract record no.: 2012320010105 Denomination of invention: Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof Granted publication date: 20110907 License type: Exclusive License Open date: 20090520 Record date: 20120528 |
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