CN111558234B - Supercritical extraction separation kettle, extraction system and extraction method - Google Patents
Supercritical extraction separation kettle, extraction system and extraction method Download PDFInfo
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- CN111558234B CN111558234B CN202010534854.3A CN202010534854A CN111558234B CN 111558234 B CN111558234 B CN 111558234B CN 202010534854 A CN202010534854 A CN 202010534854A CN 111558234 B CN111558234 B CN 111558234B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/001—Filters in combination with devices for the removal of gas, air purge systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/005—Co-current extraction
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Abstract
本发明公开了一种超临界萃取分离釜及萃取系统和萃取方法。所述超临界萃取分离釜包括釜体、顶盖，以及釜体内由外向内依次套设的环形萃取层、环形多孔介质层、旋风分离器，这种环形层状结构一方面使得萃取剂以内旋的流动形式完成萃取，增大了萃取剂流动过程中同待萃取物之间的接触面积，大幅提高萃取产率；另一方面增加了萃取釜内部的空间利用率，避免了超临界萃取过程中常见的壁流问题；同时通过设计进气孔朝向以及设置弧形引流板，使得萃取分离釜内流场更加均匀、稳定。本发明的超临界萃取分离釜体具有萃取、降压与分离纯化三种功能，能够实现高品质、高效的生物活性成分萃取，以及萃取剂的循环重复利用。
The present invention discloses a supercritical extraction separation kettle, an extraction system and an extraction method. The supercritical extraction separation kettle comprises a kettle body, a top cover, and an annular extraction layer, an annular porous medium layer and a cyclone separator which are sequentially arranged from the outside to the inside of the kettle body. On the one hand, this annular layered structure enables the extractant to complete the extraction in the form of an inward-rotating flow, thereby increasing the contact area between the extractant and the object to be extracted during the flow process, and greatly improving the extraction yield; on the other hand, it increases the space utilization rate inside the extraction kettle, avoiding the common wall flow problem in the supercritical extraction process; at the same time, by designing the direction of the air inlet and setting an arc-shaped guide plate, the flow field inside the extraction separation kettle is made more uniform and stable. The supercritical extraction separation kettle body of the present invention has three functions of extraction, pressure reduction and separation and purification, and can achieve high-quality and efficient extraction of bioactive components, as well as the recycling and reuse of the extractant.
Description
Technical Field
The invention relates to the technical field of supercritical extraction, in particular to a supercritical extraction separation kettle, an extraction system comprising the supercritical extraction separation kettle and an extraction method for extracting biological active ingredients at low temperature by using the extraction system.
Background
When the pressure and temperature of the fluid exceed the values corresponding to the critical points, the fluid enters a supercritical state, and the acting force between fluid molecules is between that of the liquid and gas molecules, so that the fluid simultaneously shows high density similar to that of the liquid, good dissolution capacity and fluidity, low viscosity similar to that of the gas and good diffusivity, and can be used as an ideal extractant. At present, more than 90% of supercritical extraction processes are performed by using carbon dioxide, mainly because the critical pressure and temperature of the carbon dioxide are low, and the supercritical extraction process has the advantages of no toxicity, incombustibility, low cost, high purity, easy diffusion and low viscosity.
At present, a supercritical extraction device widely used in actual production is realized by constructing supercritical extraction circulation, wherein fluid sequentially passes through parts such as an extraction kettle, a separator, a filter and the like in the extraction process to finish relevant processes such as extraction, separation, self-purification and the like of an extract to be extracted, and finally the fluid enters the circulation to recover an initial state and then enters the extraction kettle again to perform the next extraction work. The supercritical extraction circulation device used at present mainly has the following problems that ① parts are more required in the extraction, separation and purification processes, the actual circulation occupied space is large, the ② traditional hollow belt type extraction kettle has the problems that the space utilization rate in the kettle is low, the wall flow is easy to form due to a direct-current structure, the flow stability is reduced, ③ parts are redundant, and the disassembly process is complex. It is these problems that exist, so that extraction efficiency in actual production is greatly limited.
Disclosure of Invention
In order to solve the problems of space, efficiency and the like in the current supercritical extraction, the invention provides a novel supercritical extraction separation kettle structure, and a set of supercritical carbon dioxide circulating extraction system is constructed based on the novel supercritical extraction separation kettle structure.
The invention provides a supercritical extraction separation kettle, which comprises a kettle body, a top cover, an annular extraction layer, an annular porous medium layer and a cyclone separator, wherein the top of the kettle body is in sealing connection with the top cover, an extractant outlet is arranged in the center of the top cover, an extraction product outlet is arranged in the center of the bottom of the kettle body, a plurality of supercritical fluid air inlets are formed in the middle of the side wall of the kettle body, the annular extraction layer, the annular porous medium layer and the cyclone separator are sequentially arranged in the kettle body from outside to inside, raw materials to be extracted are placed in the annular extraction layer and extracted by the supercritical fluid, mixed fluid after extraction is filtered by the annular porous medium layer and enters the cyclone separator, the cyclone separator is provided with a hollow center shaft, the top end of the center shaft is communicated with the extractant outlet, liquid extraction products with higher density flow out from the extraction product outlet at the bottom of the kettle body under the centrifugal action of the cyclone separator, and gaseous extractant with lower density enters the center shaft and is discharged from the extractant outlet at the top end.
Furthermore, the top cover and the kettle body are preferably made of carbon steel. In one embodiment of the invention, the inner diameter of the kettle body is 500mm, the wall thickness is 60mm, and the height of the kettle body is 500mm. The kettle body and the top cover are sealed through the rubber ring and are fastened and connected through the bolt and nut assembly, so that the kettle body is sealed. A plurality of (e.g. 4) supercritical fluid air inlet holes are symmetrically arranged at the center of the side wall of the kettle body, and the aperture of the supercritical fluid air inlet hole is 12mm, for example. The central axis of the cyclone separator is provided with a guide vane with an annular spiral structure, and preferably, the direction of an opening of the supercritical fluid air inlet is consistent with the spiral direction of the guide vane on the central axis of the cyclone separator. In one embodiment of the invention, the aperture of the extraction product outlet opening at the bottom of the kettle body is 20mm, and the aperture of the extraction agent discharge outlet arranged at the center of the top cover is 20mm.
Furthermore, the annular extraction layer is of a cylindrical double-layer structure, an annular cylindrical frame body is formed by an inner wall and an outer wall with holes, the rigid support function is achieved, the aperture of the holes is preferably 0.5-1 mm, metal filter screens are tightly attached to the inner sides of the inner wall and the outer wall, the material isolation function is achieved, the mesh number of the filter screens is preferably not less than 35 meshes, a plurality of arc-shaped drainage plates are arranged in an annular space with a certain width and surrounded by the metal filter screens, the drainage direction of the arc-shaped drainage plates is consistent with the direction of a supercritical fluid air inlet hole, and the arc-shaped drainage plates are used for increasing the flow path of supercritical fluid through raw material powder to be extracted so as to improve extraction efficiency.
The supercritical extraction separation kettle replaces the functions of a filter, a separator and a throttle valve in the traditional supercritical extraction circulation device through a single annular porous medium layer. In one embodiment of the invention, the thickness of the annular porous medium layer is 50mm, porous ceramics can be selected as medium materials, and the median pore diameter of the medium is required to be below 50 μm so as to realize the filtering and purifying effects of the porous medium layer on the mixed fluid after extraction. In addition, preferably, the open porosity of the annular porous medium layer is above 60%, and the specific surface area is above 2.7m 2/g, so that smooth circulation of the supercritical fluid is ensured, and the turbulent pressure reduction effect is realized through the complex structure in the porous medium, so that the mutual separation of the extracting agent and the extracted product is facilitated.
In the supercritical extraction separation kettle, the cyclone separator adopts a vertical cylinder structure, the central shaft of the cyclone separator is provided with guide vanes, the guide vanes preferably adopt a ring-shaped spiral structure from bottom to top, the height of the vanes is 20-40 mm, the distance between the vanes is 40-50 mm, the outer wall of the cyclone separator is preferably an annular metal frame with holes, the annular metal frame is tightly attached to the inner wall of the annular porous medium layer so as to prevent wall flow, a plurality of (e.g. 4) arc-shaped guide plates are connected in the outer wall of the cyclone separator, the opening direction of the arc-shaped guide plates is consistent with the spiral direction of the guide vanes in the central shaft of the cyclone separator, and the inner space of the equipment is fully utilized so as to reduce the load of cyclone parts. In actual production, the liquid extraction product with higher density is screwed onto the outer wall of the central shaft of the cyclone separator by utilizing the density difference between the extracting agent and the extraction product, flows downwards along the guide vane by gravity, is discharged through the extraction product outlet and stored in a related container, the gaseous extracting agent with lower density is continuously involved into the lower part of the cyclone separator, passes through the hollow central shaft from the lower part of the central shaft, and finally is discharged out of the extraction separation kettle from the extracting agent outlet above the top cover of the kettle body.
In the supercritical extraction separation kettle, preferably, arc-shaped drainage plates are arranged in the annular extraction layer and the cyclone separator, and supercritical fluid entering from the supercritical fluid inlet hole is sequentially guided by the arc-shaped drainage plates and the cyclone separator in the annular extraction layer and the cyclone separator, so that the smooth flow of the supercritical fluid in the extraction separation kettle is ensured.
In a second aspect of the invention, a set of supercritical carbon dioxide circulating extraction system is constructed by utilizing the supercritical extraction separation kettle, and a method for extracting plant or microorganism active substances at low temperature is provided.
The invention provides a supercritical carbon dioxide circulating extraction system which comprises a supply tank, a heater, an infusion pump, a precooler, a supercritical extraction separation kettle, a cooler and pipelines for connecting the supply tank with the precooler, wherein the supply tank is used for storing carbon dioxide liquid, the carbon dioxide liquid output from the supply tank is heated into supercritical carbon dioxide fluid through the heater, the supercritical carbon dioxide fluid enters the precooler for precooling under the action of the infusion pump and then enters the supercritical extraction separation kettle for extracting active ingredients from materials to be extracted in the kettle, an extraction product flows out from the bottom of the kettle body and is collected, the separated supercritical carbon dioxide fluid is discharged from the top of the kettle body and is cooled and liquefied through the cooler and then is circulated back into the supply tank.
Further, pressure sensors are arranged on the pipeline from the heater to the infusion pump, the pipeline from the precooler to the supercritical extraction separation kettle and the pipeline from the cooler to the supply tank, and are used for monitoring the pressure of fluid in each pipeline. A velocimeter is arranged on a pipeline from the infusion pump to the precooler so as to monitor the flow rate of the supercritical carbon dioxide fluid.
Furthermore, a throttle valve is arranged on the pipeline from the precooler to the supercritical extraction separation kettle to control the flow rate of supercritical carbon dioxide entering the supercritical extraction separation kettle, a throttle valve is also arranged on the pipeline connecting the extractant outlet of the supercritical extraction separation kettle and the cooler to control the flow rate of discharged supercritical carbon dioxide fluid, and a throttle valve is also arranged on the extraction product outflow pipeline at the bottom of the supercritical extraction separation kettle.
In the supercritical carbon dioxide circulating extraction system, carbon dioxide liquid stored in a supply tank is output to a heater, is heated to the temperature and the pressure (50 ℃ and 10-11 MPa) required by extraction by the heater to obtain supercritical carbon dioxide fluid, then enters a precooler for precooling under the action of an infusion pump, the supercritical carbon dioxide fluid at the outlet of the precooler is controlled to be 43.5-45.2 ℃ and 10.0-10.5 MPa, is sent into a supercritical extraction separation kettle for extracting active ingredients, an extraction product flows out from the bottom of the extraction separation kettle under the action of a cyclone separator in the extraction separation kettle, the separated supercritical carbon dioxide fluid is discharged from the top of the kettle, enters a cooler for cooling and liquefying to reach the required state (-20 ℃ and 2.16 MPa), and is stored back into the supply tank.
The working flow of extracting the active ingredients of the biological materials at low temperature by using the supercritical carbon dioxide circulating extraction system is as follows:
1) Placing pretreated animal and plant, microorganism or other biological material powder to be extracted into an annular extraction layer in the extraction separation kettle, and closing the top cover of the extraction separation kettle;
2) Starting a cooler, a heater and a precooler, starting an infusion pump, heating carbon dioxide liquid output from a supply tank to the temperature and the pressure (50 ℃ and 10-11 MPa) required by supercritical fluid through the heater, entering the precooler through the infusion pump to precool, controlling the supercritical carbon dioxide fluid to be in the required state (43.5-45.2 ℃ and 10.0-10.5 MPa), and continuously inputting the supercritical carbon dioxide fluid into an extraction separation kettle to extract;
3) Cooling and liquefying supercritical carbon dioxide fluid separated from a cyclone separator in an extraction separation kettle by a cooler to reach a required state (-20 ℃ and 2.16 MPa), and storing the supercritical carbon dioxide fluid back into a supply tank;
4) Continuously outputting carbon dioxide liquid from the supply tank, and repeating the steps 2) and 3) for extraction circulation until the required extraction product is obtained.
In the step 2), the carbon dioxide liquid is firstly heated to the temperature and the pressure (50 ℃ and 10-11 MPa) required by the supercritical fluid by a heater, and then pumped into a precooler by an infusion pump for precooling, so that the pressure surge at the inlet of an extraction separation kettle is avoided, and the supercritical fluid at the outlet of the precooler is controlled to be in a state of 43.5-45.2 ℃ and 10.0-10.5 MPa, so that higher extraction purity and extraction efficiency are obtained.
Preferably, in the step 2), a velocimeter is arranged at the outlet of the infusion pump, the power of the infusion pump is regulated, and the indication number of the velocimeter is controlled within the range of 2-4 m/s.
The invention has the advantages that:
1) Compared with the bottom-up extractant input mode in the traditional extraction kettle, the annular layered structure of the extraction separation kettle ensures that the extractant finishes extraction in an internal rotation flow mode, increases the contact area between the extractant and the to-be-extracted object in the flow process of the extractant, and greatly improves the extraction yield;
2) The annular layered structure design of the extraction separation kettle increases the space utilization rate inside the extraction kettle, avoids the common wall flow problem in the supercritical extraction process, and simultaneously ensures that the flow field in the extraction separation kettle is more uniform and stable by designing the orientation of the air inlet and arranging the arc-shaped drainage plate;
3) According to the invention, 3 functions of extraction, depressurization, separation and purification are realized through one extraction separation kettle body, and the functions can be realized only by setting up three parts respectively in the traditional circulation, so that the occupied space of equipment is saved compared with the traditional circulation, and the construction cost of the circulation is reduced;
4) The unique combination of supercritical carbon dioxide extraction temperature and pressure and the design of a special extraction separation kettle structure realize the extraction of the active ingredients of animals, plants and microorganisms with high quality and high efficiency;
5) The recycling of the carbon dioxide extractant is realized by constructing the extraction cycle, and the extraction capacity is greatly improved (the extraction efficiency is improved by about 35 percent);
Drawings
FIG. 1 is a schematic diagram of the supercritical carbon dioxide cycle extraction system according to an embodiment of the present invention;
FIG. 2 is a longitudinal sectional view (front view) of an extraction separation tank in an embodiment of the invention;
FIG. 3 is a cross-sectional view (top view) of an extraction separation tank in accordance with an embodiment of the invention;
In the figure, 1 is an extraction separation kettle, 2 is a first throttle valve, 3 is a second throttle valve, 4 is a cooler, 51 is a first pressure sensor, 52 is a second pressure sensor, 53 is a third pressure sensor, 6 is a supply tank, 7 is a heater, 8 is an infusion pump, 9 is a speedometer, 10 is a precooler, 11 is a third throttle valve, 1-1 is a top cover, 1-2 is a kettle body, 1-3 is an annular extraction layer, 1-4 is an annular porous medium layer, 1-5 is a cyclone separator, 1-6 is a bolt and nut assembly, 1-1-1 is an extractant outlet, 1-2-1 is a supercritical fluid inlet, 1-2-2 is an extraction product outlet, 1-3-1 is an annular cylindrical frame, 1-3-2 is an arc-shaped drainage plate, 1-3-3 is a metal filter screen, 1-5-1 is a cyclone separator outer wall, 1-5-2 is a cyclone separator arc-shaped drainage plate, 1-5-3 is a cyclone separator center shaft, and 1-5-4 is a flow guiding blade.
Detailed Description
The technical scheme of the invention is further described in detail through specific embodiments with reference to the accompanying drawings.
As shown in FIG. 1, the supercritical carbon dioxide circulating extraction system comprises an extraction separation kettle 1, a cooler 4, a supply tank 6, a heater 7, an infusion pump 8 and a precooler 10. The carbon dioxide liquid stored in the supply tank 6 is output to a heater 7, is heated to the temperature and the pressure (50 ℃ and 10-11 MPa) required by extraction by the heater 7 to obtain supercritical carbon dioxide fluid, the supercritical carbon dioxide fluid enters a precooler 10 for precooling under the action of an infusion pump 8, the supercritical carbon dioxide fluid at the outlet of the precooler 10 is controlled to be 43.5-45.2 ℃ and 10.0-10.5 MPa, the supercritical carbon dioxide fluid enters the extraction separation kettle 1 from the side surface of the extraction separation kettle 1 through a pipeline provided with a third throttle valve 11 to extract active components from materials in the kettle, the extraction product flows out from the bottom of the extraction separation kettle 1 under the action of a cyclone separator in the extraction separation kettle 1, a first throttle valve 2 is arranged on the outflow pipeline to control the flow speed, the separated supercritical carbon dioxide fluid is discharged from the top of the extraction separation kettle 1, is depressurized by a second throttle valve 3 and enters a cooler 4 to be cooled to reach the required state (-20 ℃ and 2.16 MPa) and then stored in the supply tank 6. A first pressure sensor 51 is arranged on the pipeline from the cooler 4 to the supply tank 6, a second pressure sensor 52 is arranged on the pipeline from the heater 7 to the infusion pump 8, and a third pressure sensor 53 is arranged on the pipeline from the precooler 10 to the extraction separation kettle 1, and is respectively used for monitoring the pressure of fluid in each pipeline. The power of the infusion pump 8 is monitored by a tachometer 9 provided on the line between the infusion pump 8 and the precooler 10.
The structure of the extraction separation kettle 1 in the extraction system is shown in figures 2 and 3, and comprises a top cover 1-1, a kettle body 1-2, an annular extraction layer 1-3, an annular porous medium layer 1-4 and a cyclone separator 1-5, wherein the annular extraction layer 1-3, the annular porous medium layer 1-4 and the cyclone separator 1-5 are sequentially sleeved in the kettle body 1-2 from outside to inside, the annular extraction layer 1-3 is formed by enclosing an annular cylindrical frame body 1-3-1 with holes on the inner wall and the outer wall and a metal filter screen 1-3-3 closely attached to the inner sides of the two wall surfaces into an annular space with a certain width, four arc-shaped drainage plates 1-3-2 are arranged in the annular space at equal intervals, an extractant outlet 1-1-1 is arranged in the center of the top cover 1-1, an extraction product outlet 1-2-2 is arranged at the bottom of the kettle body 1-2, a relevant vessel can be connected below the extraction product outlet 1-2-2 for collecting extraction products, four supercritical fluid inlet holes 1-2 are arranged on the side walls of the kettle body 1-2, and the four supercritical fluid 1-2 are respectively corresponding to the arc-shaped drainage plates 1-3 in the annular drainage plates 1-3-3.
The top cover 1-1 and the kettle body 1-2 are made of Q245R carbon steel, the inner diameter of the kettle body 1-2 is 500mm, the wall thickness is 60mm, and the height of the kettle body is 500mm. The kettle body 1-2 and the top cover 1-1 are sealed by a polyurethane rubber ring and are tightly connected by a bolt and nut component 1-6, so that the kettle body is sealed. 4 supercritical fluid air inlets 1-2-1 are formed in the middle of the side wall of the kettle body 1-2, the aperture of the supercritical fluid air inlets 1-2-1 is 12mm, the direction of the aperture is consistent with the internal rotation direction of a central shaft 1-5-3 of the cyclone separator (namely the spiral direction of a guide vane 1-5-4), and supercritical fluid entering from the supercritical fluid air inlets 1-2-1 is sequentially guided by arc-shaped guide plates 1-3-2 and 1-5-2 in the annular extraction layer 1-3 and the cyclone separator 1-5 so as to ensure smooth flow of the supercritical fluid in the extraction separation kettle. The aperture of the extraction product outlet 1-2-2 arranged at the bottom of the kettle body 1-2 is 20mm, and the aperture of the extraction agent outlet 1-1-1 arranged in the center of the top cover 1-1 is 20mm.
Unlike traditional cylindrical extraction frame, the present invention adopts annular extraction layered structure. The annular extraction layers 1-3 are of double-layer structure, and the inner layer width is 50mm (namely, the distance between the outer wall and the inner wall of the annular cylinder with holes in the radial direction). The metal filter screens 1-3-3 positioned on the inner sides of the inner wall surface and the outer wall surface of the annular cylindrical frame body 1-3-1 play a role in isolating materials, the mesh number of the filter screens is not less than 35 meshes, the annular cylinder with holes on the inner wall and the outer wall plays a role in rigid support, the aperture diameter of the holes is 0.5-1 mm, and the inlet flow direction of the arc-shaped flow guide plates 1-3-2 arranged in the annular extraction layer 1-3 is consistent with the direction of the supercritical fluid air inlet holes 1-2-1, so that the flow path of supercritical fluid passing through raw material powder to be extracted is increased, and the extraction efficiency is improved.
The present invention replaces the action of filters, separators and throttles in conventional supercritical extraction cycles by a single annular porous media layer 1-4. The thickness of the annular porous medium layer 1-4 is 50mm, porous ceramics can be selected as medium materials, and the median pore diameter of the medium is required to be below 50 mu m, so that the filtering and purifying effects of the porous medium layer on the extracted mixed fluid are realized. In addition, the open porosity of the annular porous medium layer 1-4 is required to be more than 60%, the specific surface area is required to be more than 2.7m 2/g, so that smooth circulation of supercritical fluid is ensured, the turbulent pressure reduction effect is realized through the complex structure in the porous medium, and the mutual separation of the extracting agent and the extracted product is facilitated.
The cyclone separator 1-5 adopts a vertical cylinder structure, the outer wall 1-5-1 of the cyclone separator is an annular metal frame with holes, the annular metal frame is clung to the inner wall of a porous medium layer 1-4 to prevent wall flow phenomenon, 4 equidistant arc-shaped flow guiding plates 1-5-2 are connected in the outer wall 1-5-1 of the cyclone separator, the opening direction of the arc-shaped flow guiding plates is consistent with the spiral direction of the upper flow guiding blades 1-5-4 of the central shaft 1-5-3 of the cyclone separator, the internal space of the device is fully utilized to reduce the load of cyclone parts, the flow guiding blades 1-5-4 adopt a circular spiral structure from bottom to top, the blade height is 20-40 mm, the blade spacing is 40-50 mm, the central shaft 1-5-3 of the cyclone separator is of a hollow structure, in actual production, liquid extraction products with higher density are screwed onto the outer wall of the central shaft 1-5-3 of the cyclone separator through centrifugal effect, flow downwards along the flow guiding blades 1-5-4 through gravity effect, the extraction product outlets 1-2-2 are discharged and stored in the relevant containers, the lower central shaft 1-1-3 is discharged from the upper part of the cyclone separator through the lower central shaft 1-1-3 of the cyclone separator, and the lower part of the cyclone separator is continuously discharged from the upper part of the central shaft 1-1-1-lower part of the cyclone separator is discharged from the upper part of the cyclone separator 1-1-lower part of the central shaft 1 is continuously below the hollow part.
The supercritical carbon dioxide circulating extraction system constructed by the extraction separation kettle is used for extracting the effective biological components in herbaceous plants at low temperature.
The following describes the extraction steps of herbal extracts, taking mugwort as an example:
1) Putting a proper amount of dry mugwort in a ball mill, grinding for 3 hours at a low speed under a cooling condition, controlling the temperature in the grinding process to be not more than 35 ℃, and grinding the ground mugwort to obtain mugwort powder with the particle size of 0.5-0.7 mm;
2) Placing the ground mugwort powder into an annular extraction layer 1-3 of an extraction separation kettle 1, closing a top cover 1-1 of the extraction separation kettle, screwing a sealing nut, and starting supercritical carbon dioxide extraction circulation;
3) Adjusting the power of an infusion pump 8, controlling the flow rate of an extracting agent in supercritical carbon dioxide extraction circulation to be 2-4 m/s, controlling the supercritical carbon dioxide state input into an extraction separation kettle 1 to be 43.5-45.2 ℃ and 10.0-10.5 MPa through a heater 7 and a precooler 10, and controlling the extraction time of mugwort powder to be 75-87 minutes (not more than 90 minutes);
4) And closing the infusion pump 8 after extraction is finished, closing the second throttle valve 3 and the third throttle valve 11, opening the first throttle valve 2, taking out the liquid in the collector at the bottom of the extraction separation kettle 1, standing for 10 minutes, and obtaining the required liquid oily mugwort extract after the vaporization and separation of the residual carbon dioxide are finished.
The present invention is not limited to the above-described preferred embodiments, and it will be understood by those skilled in the art that various changes, substitutions and alterations are possible in the form and construction illustrated and described herein without departing from the spirit and scope of the invention. Therefore, the invention should not be limited to the disclosure of the drawings and the embodiments, but the scope of the invention is defined by the claims.
Claims (7)
1. The supercritical extraction separation kettle is characterized by comprising a kettle body, a top cover, an annular extraction layer, an annular porous medium layer and a cyclone separator, wherein the top of the kettle body is in sealing connection with the top cover, an extractant outlet is arranged in the center of the top cover, an extraction product outlet is arranged in the center of the bottom of the kettle body, and a plurality of supercritical fluid air inlets are formed in the middle of the side wall of the kettle body; the cyclone separator is of a vertical cylinder structure, a guide vane of an annular spiral structure from bottom to top is arranged on the central shaft of the cyclone separator, an annular metal frame with holes is arranged on the outer wall of the cyclone separator, the annular cylinder frame is tightly attached to the annular porous medium layer, a plurality of arc-shaped guide plates are arranged on the inner sides of the inner wall and the outer wall of the annular cylinder frame, the metal filter screens are used for isolating materials, a plurality of arc-shaped guide plates are arranged in an annular space with a certain width and surrounded by the metal filter screens, the direction of the guide plates is consistent with the direction of a supercritical fluid air inlet, the cyclone separator is of a vertical cylinder structure, the direction of an opening of the supercritical fluid air inlet is consistent with the spiral direction of the guide vane on the central shaft of the cyclone separator, a plurality of arc-shaped guide plates are connected in the outer wall of the annular cylinder frame, the opening direction of the arc-shaped guide plates is consistent with the spiral direction of the guide vane, the raw materials to be extracted are placed in the annular extraction layer, the extracted supercritical fluid enters the cyclone separator after being filtered by the annular porous medium layer, the mixed fluid enters the cyclone separator, the central shaft is provided with a central shaft of the hollow separator, the hollow central shaft is communicated with the cyclone separator, the liquid extraction product with higher density flows out from an extraction product outlet at the bottom of the kettle body, and the gaseous extractant with lower density enters the center shaft and is discharged from an extractant outlet at the top end.
2. The supercritical extraction separation kettle according to claim 1, wherein four equidistant supercritical fluid air inlets are formed in the side wall of the kettle body, and correspondingly four equidistant arc-shaped drainage plates are arranged in the annular extraction layer.
3. The supercritical extraction separation kettle according to claim 1, wherein the aperture of the annular cylindrical frame body of the annular extraction layer is 0.5-1 mm, the number of the metal filtering meshes is not less than 35 meshes, the open porosity of the annular porous medium layer is above 60%, the specific surface area is above 2.7 m 2/g, and the median aperture is below 50 μm.
4. The supercritical extraction separation kettle according to claim 1, wherein the annular porous medium layer is porous ceramic.
5. A supercritical carbon dioxide circulating extraction system comprises a supply tank, a heater, an infusion pump, a precooler, a supercritical extraction separation kettle, a cooler and a pipeline for connecting the supercritical extraction separation kettle and the cooler, wherein the supercritical extraction separation kettle is as set forth in any one of claims 1-4, the supply tank is used for storing carbon dioxide liquid, the carbon dioxide liquid output from the supply tank is heated into supercritical carbon dioxide fluid through the heater, the supercritical carbon dioxide fluid enters the precooler for precooling under the action of the infusion pump, then enters the supercritical extraction separation kettle for extracting active ingredients from materials to be extracted in the kettle, an extraction product flows out from the bottom of the kettle body of the supercritical extraction separation kettle and is collected, the separated supercritical carbon dioxide fluid is discharged from the top of the kettle body and is cooled and liquefied through the cooler and then is circulated back into the supply tank.
6. The supercritical carbon dioxide circulating extraction system according to claim 5, wherein pressure sensors are respectively arranged on a pipeline from the heater to the infusion pump, a pipeline from the precooler to the supercritical extraction separation kettle and a pipeline from the cooler to the supply tank, a velocimeter is arranged on a pipeline from the infusion pump to the precooler, a throttle valve is respectively arranged on a pipeline from the precooler to the supercritical extraction separation kettle, a pipeline from the extraction agent outlet of the supercritical extraction separation kettle to the cooler and an extraction product outflow pipeline from the bottom of the supercritical extraction separation kettle.
7. A method for extracting active ingredients of biological materials at low temperature, which comprises the following steps of:
1) Placing the biological material powder to be extracted into an annular extraction layer in the supercritical extraction separation kettle, and closing a top cover of the supercritical extraction separation kettle;
2) Starting a cooler, a heater and a precooler, starting an infusion pump, heating carbon dioxide liquid output from a supply tank to the temperature and the pressure required by supercritical fluid through the heater, entering the precooler through the infusion pump to precool, controlling the supercritical carbon dioxide fluid to be in a required state, and continuously inputting the supercritical carbon dioxide fluid into a supercritical extraction separation kettle to extract biological material powder;
3) The supercritical carbon dioxide fluid separated from the cyclone separator in the supercritical extraction separation kettle is cooled and liquefied by a cooler and then stored back into a supply tank;
4) Continuously outputting carbon dioxide liquid from the supply tank, and repeating the steps 2) and 3) for extraction circulation until the required extraction product is obtained.
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| CN112430499A (en) * | 2020-11-20 | 2021-03-02 | 湖南和广生物科技有限公司 | Basket-free supercritical fluid extraction device capable of feeding and discharging rapidly |
| CN114717046A (en) * | 2022-04-11 | 2022-07-08 | 马丽芝 | Device and extraction process for cyclically extracting rapeseed oil by supercritical carbon dioxide |
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