CN110743192A - Adsorption separation regulation and control type supercritical fluid extraction equipment - Google Patents
Adsorption separation regulation and control type supercritical fluid extraction equipment Download PDFInfo
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Abstract
The invention discloses an adsorption separation regulation and control type supercritical fluid extraction device, which belongs to the field of pharmaceutical equipment, can extract effective substances from Chinese herbal medicines by utilizing the supercritical characteristic of carbon dioxide, has mild extraction regulation, no pollution, strong extraction capacity, high extraction rate, short extraction time and short production period, when the extracted effective substances enter the separation step, a novel regulation and control type adsorption component is introduced to actively adsorb the effective substances which are not completely released in the carbon dioxide to complete interception, so that the recovery rate of the effective substances is improved, meanwhile, the adsorption component can be adjusted by detecting the content of effective substances in the carbon dioxide with the assistance of the sampling detection technology in the prior art, make carbon dioxide can be fast through realizing recycling under the prerequisite that satisfies the absorption and hold back, show and improve holistic extraction efficiency and quality, and the absorption subassembly makes things convenient for the desorption to retrieve the effective substance and continues reuse.
Description
Technical Field
The invention relates to the field of pharmaceutical equipment, in particular to adsorption separation regulation type supercritical fluid extraction equipment.
Background
Supercritical fluid is a supercritical fluid, which is a non-gaseous and non-liquid state between gas and liquid, and can exist only when the temperature and pressure of the substance exceed critical points, the density of the supercritical fluid is higher and similar to that of liquid, and the viscosity of the supercritical fluid is closer to that of gas, so the supercritical fluid is an ideal extracting agent.
The solvent strength of the supercritical fluid depends on the temperature and pressure of extraction. By utilizing the characteristics, different components in a sample can be extracted sequentially according to the solubility in the fluid by only changing the pressure and the temperature of the extractant fluid, substances with weak polarity are extracted first under low pressure, and substances with larger polarity and large molecular weight and basic properties are extracted along with the increase of the pressure, so that the supercritical extraction is carried out under the program pressure to obtain different extracted components, and the separation effect can be realized. The temperature change is reflected in two factors which affect the density of the extractant and the vapor pressure of the solute, in a low temperature region (still above a critical temperature), the temperature is increased to reduce the fluid density, but the vapor pressure of the solute is not increased much, so that the temperature rise during the dissolving capacity of the extractant can make the solute be separated out from the fluid extractant, when the temperature is further increased to a high temperature region, although the density of the extractant is further reduced, the vapor pressure of the solute is increased, the volatility is increased, and the extraction rate is not reduced but increased.
The principle of supercritical CO2 fluid extraction (SFE) separation process is based on the relationship between the dissolving capacity of supercritical fluid and its density, i.e., the effect of pressure and temperature on the dissolving capacity of supercritical fluid. In the supercritical state, the supercritical fluid is contacted with the substance to be separated, so that the components with polarity, boiling point and molecular weight are selectively extracted in turn. Of course, the extracts obtained corresponding to each pressure range cannot be single, but the conditions can be controlled to obtain the mixed components with the optimal proportion, then the supercritical fluid is changed into the common gas by the methods of pressure reduction and temperature rise, and the extracted substances are completely or basically separated out, so that the separation and purification purposes are achieved, and therefore, the supercritical CO2 fluid extraction process is formed by combining the extraction and separation processes.
Although the existing supercritical CO2 fluid extraction has the advantages of pure natural green pollution-free extraction, strong extraction capacity, high extraction rate, short extraction time, short production period and the like, after actual extraction, when separation is carried out in a separation tank by changing the temperature and pressure, the phenomenon of incomplete separation exists, namely, carbon dioxide is still mixed with some effective substances which are extracted for a certain time when being released, separated and recycled, so that the extraction rate is difficult to exert to the maximum, the waste of the effective substances is caused, and meanwhile, the subsequent extraction efficiency is influenced after the effective substances enter circulation.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide an adsorption separation regulation type supercritical fluid extraction device which can extract effective substances from Chinese herbal medicines by utilizing the supercritical characteristic of carbon dioxide, has mild extraction regulation without pollution, strong extraction capability, high extraction rate, quick extraction time and short production period, introduces a novel regulation type adsorption component when the extracted effective substances enter a separation step, actively adsorbs and intercepts the effective substances which are not completely released in the carbon dioxide, improves the recovery rate of the effective substances, can be assisted with the sampling detection technology in the prior art, regulates the adsorption component by detecting the content of the effective substances in the carbon dioxide, ensures that the carbon dioxide can be quickly recycled on the premise of meeting the adsorption interception, and obviously improves the whole extraction efficiency and quality, and the adsorption component is convenient to desorb and recover effective substances and continuously recycle.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
An adsorption separation regulation type supercritical fluid extraction device comprises a storage tank and a control box, wherein a first three-way pipe is fixedly connected with an inlet end of the storage tank, a first communicating pipe is fixedly connected with the right end of the first three-way pipe, a condensing tank is fixedly connected with the first communicating pipe, a second communicating pipe is fixedly connected with the condensing tank, a pressurizing tank is fixedly connected with the second communicating pipe, a third communicating pipe is fixedly connected with the pressurizing tank, a heating tank is fixedly connected with the third communicating pipe, an extraction kettle is fixedly connected with the heating tank, a fourth communicating pipe is fixedly connected with an outlet end of the extraction kettle, a liquid pump is fixedly connected with the fourth communicating pipe, a separation tank is fixedly connected with an output end of the liquid pump, a second three-way pipe is fixedly connected with an outlet end of the separation tank, an adsorption vat is fixedly connected with an upper end of the second three-way pipe, and a third three-way, a return pipe is fixedly connected between the third three-way pipe and the second three-way pipe, a fifth communicating pipe is fixedly connected to the left end of the third three-way pipe, a liquefaction tank is fixedly connected to the fifth communicating pipe, a sixth communicating pipe is fixedly connected to the outlet end of the liquefaction tank, a compressor is fixedly connected to the sixth communicating pipe, and a circulation pipe is fixedly connected between the output end of the compressor and the upper end of the first three-way pipe.
Furthermore, the inner end of the adsorption vat is filled with an adsorption component, the adsorption component comprises a mosquito-repellent incense type fixing pipe and a plurality of gap adjusting air bags, the gap adjusting air bags are uniformly distributed along the mosquito-repellent incense type fixing pipe and are connected with each other, the mosquito-repellent incense type fixing pipe is fixedly connected with the inner end of the adsorption vat, a central magnetic suction block is arranged between every two adjacent gap adjusting air bags, an elastic main wire is fixedly connected between the central magnetic suction block and the gap adjusting air bags, electromagnets are installed at the inner end of the central magnetic suction block and are connected with a control box in series and electrically connected with each other, a plurality of adsorption branch wires which are distributed densely are bonded on the outer surface of the elastic main wire, one ends of the adsorption branch wires, far away from the elastic main wire, are fixedly connected with floating balls, the adsorption branch wires play a role in adsorbing effective substances in carbon dioxide to complete interception, the extraction rate is improved, realize the initiative and draw close and laminate on the elasticity owner silk, no longer the active absorption active material, carbon dioxide can be fast through not blockking, the elasticity owner silk plays the plastic effect to the clearance gasbag on the one hand, on the other hand can provide the absorption and divide the certain extension space of silk to be used for forming the absorption net of spatial mode, improves the adsorption effect, the elastic deformation effect of its self can satisfy the inflation and the shrink of adjusting the clearance gasbag, is used for adjusting the velocity of flow of carbon dioxide in adsorption component.
Further, adsorb and divide the silk to include the adsorbed layer, the adsorbed layer inner is equipped with the inner core, the inner core includes stretch yarn and flexible silk, and fixed connection between stretch yarn and the flexible silk, the adsorbed layer plays the effect of adsorbing effective substance, and the stretch yarn plays the effect of providing the elasticity, is used for unfolding naturally under no magnetic force state, resets into initial space adsorption net form, and the flexible silk has flexible changeable characteristic, can swing deformation under the impact of carbon dioxide, increase and the area of carbon dioxide contact, realize dynamic initiative absorption.
Furthermore, the elastic wires are made of elastic metal materials, the flexible wires are made of silicon rubber materials, the length ratio of the elastic wires to the flexible wires is 1:5-10, the adsorption layers cover the outer surfaces of the elastic wires and the flexible wires, and the elastic supporting effect of the elastic wires can be achieved only under the appropriate length ratio.
Furthermore, the adsorption layer is made of activated carbon fiber material, the fiber diameter is 5-20 μm, the specific surface area is about 1000-1500m2/g on average, the average pore diameter is 1.0-4.0nm, the activated carbon fiber has larger adsorption capacity and faster adsorption dynamic performance than granular activated carbon, has high adsorption efficiency on organic matters, anions and cations in liquid phase and gas phase, has high adsorption and desorption speeds, can be recycled, is acid-resistant, alkali-resistant, high temperature-resistant, strong in adaptability, good in conductivity and chemical stability, and is an ideal environment-friendly material.
Further, the floating ball includes and foam ball and magnetic block, the cavity has been absorbed in the division of magnetic block inner end, and the magnetic block fills in absorbing the cavity, the magnetic block is ferromagnetic metal material, and the foam ball plays the effect of protection magnetic block, avoids the impact wear who produces when passive absorption is drawn close together, and the texture is light simultaneously, and the quality under the equal volume is very little, and buoyancy is great, also can realize the swing under the micro-flow impact of carbon dioxide.
Furthermore, the length of the stretched adsorption divided filament is not less than the maximum length of the elastic main filament, so that the floating ball is prevented from being pulled to damage the adsorption divided filament after being adsorbed by the electromagnet under the maximum length of the elastic main filament, and the adsorption service life of the adsorption divided filament is prolonged.
Further, transfer clearance gasbag upper end and be provided with the inflation inlet, the inflation inlet adopts the rubber material, the fixed intraductal chisel of mosquito-repellent incense type has gas flow channel, and gas flow channel and inflation inlet are linked together, adsorb urn outer end and install the pump, and the output of pump with adsorb the urn and be connected and be linked together with gas flow channel, the fixed pipe of mosquito-repellent incense type can realize the effect of fixed clearance gasbag on the one hand, on the other hand directly with transfer the function that the clearance gasbag intercommunication realized filling gassing.
Further, an extraction medium is stored in the storage tank, the extraction medium is carbon dioxide, and the critical point condition of the carbon dioxide is 31.2 ℃ and 7.39 MPa.
Further, the equal fixedly connected with sampling tube of entrance point and the exit end of absorption urn, install the detector on the sampling tube, the sampling tube plays the effect of real-time sample, and the detector then carries out the content detection of active material to the carbon dioxide of sample.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme can realize the supercritical characteristic of utilizing carbon dioxide, extract effective substances from Chinese herbal medicines, the extraction is adjusted to be mild and pollution-free, the extraction capacity is strong, the extraction rate is high, the extraction time is short, the production period is short, when the extracted effective substances enter the separation step, a novel regulation and control type adsorption component is introduced, the effective substances which are not completely released in the carbon dioxide are actively adsorbed, the interception is completed, the recovery rate of the effective substances is improved, meanwhile, the sampling detection technology in the prior art can be supplemented, the adsorption component is adjusted through the detection of the content of the effective substances in the carbon dioxide, the carbon dioxide can be rapidly recycled through the realization on the premise of meeting the adsorption interception, the integral extraction efficiency and quality are obviously improved, and the adsorption component is convenient to desorb and recover the effective substances and continue to be repeatedly utilized.
(2) The inner end of the adsorption vat is filled with an adsorption component, the adsorption component comprises a mosquito-repellent incense type fixing pipe and a plurality of gap-adjusting air bags, the gap-adjusting air bags are uniformly distributed along the mosquito-repellent incense type fixing pipe and are connected with each other, the mosquito-repellent incense type fixing pipe is fixedly connected with the inner end of the adsorption vat, a central magnetic suction block is arranged between every two adjacent gap-adjusting air bags, an elastic main thread is fixedly connected between the central magnetic suction block and the gap-adjusting air bags, electromagnets are installed at the inner ends of the central magnetic suction blocks, the electromagnets are connected in series with each other and are electrically connected with a control box, a plurality of adsorption branch threads which are distributed densely are bonded on the outer surface of the elastic main thread, a floating ball is fixedly connected at one end of the adsorption branch threads, which is far away from the elastic main thread, the adsorption branch threads play a role in adsorbing effective substances in carbon dioxide to complete interception, no longer initiatively adsorb the active material, carbon dioxide can be passed through fast and not blockked, and elasticity owner silk plays the plastic effect to the clearance gasbag on the one hand, and on the other hand can provide and adsorb that the certain extension space of branch silk is used for forming the absorption net of spatial expression, improves the adsorption effect, and the expansion and the shrink of adjusting the clearance gasbag can be satisfied in its self elastic deformation effect, are used for adjusting the velocity of flow of carbon dioxide in adsorption component.
(3) The adsorption separation wire comprises an adsorption layer, the inner end of the adsorption layer is provided with an inner core, the inner core comprises an elastic wire and a flexible wire, the elastic wire and the flexible wire are fixedly connected, the adsorption layer plays a role in adsorbing effective substances, the elastic wire plays a role in providing elasticity and is used for being naturally unfolded in a non-magnetic force state and being reset to be in an initial space adsorption net shape, the flexible wire has flexible and variable characteristics, the flexible wire can swing and deform under the impact of carbon dioxide, the contact area between the flexible wire and the carbon dioxide is increased, and dynamic active adsorption is realized.
(4) The elastic wire is made of elastic metal materials, the flexible wire is made of silicon rubber materials, the length ratio of the elastic wire to the flexible wire is 1:5-10, the adsorption layer covers the outer surfaces of the elastic wire and the flexible wire, and the elastic supporting effect of the elastic wire can be realized only under the proper length ratio.
(5) The adsorption layer is made of activated carbon fiber material, the fiber diameter is 5-20 μm, the specific surface area is about 1000-1500m2/g on average, the average pore diameter is 1.0-4.0nm, the activated carbon fiber has larger adsorption capacity and faster adsorption kinetics performance than granular activated carbon, has high adsorption efficiency on organic matters, anions and cations in liquid phase and gas phase, has fast adsorption and desorption speeds, can be recycled, is acid-resistant, alkali-resistant, high-temperature-resistant, strong in adaptability, good in conductivity and chemical stability, and is an ideal environment-friendly material.
(6) The floating ball includes and foam ball and magnetic block, and the chisel has the absorption cavity in the magnetic block, and the magnetic block fills in adsorbing the cavity, and the magnetic block is ferromagnetic metal material, and the foam ball plays the effect of protection magnetic block, avoids the impact wear who produces when passive absorption is drawn close together, and the texture is light simultaneously, and the quality under the equal volume is very little, and buoyancy is great, also can realize the swing under the micro-flow impact of carbon dioxide.
(7) The length of the adsorption divided filament after being stretched is not less than the maximum length of the elastic main filament, so that the floating ball is prevented from being pulled to damage the adsorption divided filament after being adsorbed by the electromagnet under the maximum length of the elastic main filament, and the adsorption service life of the adsorption divided filament is prolonged.
(8) The gap adjusting air bag is characterized in that an inflation inlet is formed in the upper end of the gap adjusting air bag and made of rubber, a gas flow passage is formed in the mosquito-repellent incense type fixing pipe in a chiseled mode and communicated with the inflation inlet, an inflation pump is installed at the outer end of the adsorption urn, the output end of the inflation pump is connected with the adsorption urn and communicated with the gas flow passage, the mosquito-repellent incense type fixing pipe can achieve the effect of fixing the gap adjusting air bag on one hand, and the other hand can achieve the functions of inflation and deflation by being directly communicated with the gap adjusting air bag.
(9) The storage tank is stored with an extraction medium which is carbon dioxide, and the critical point condition of the carbon dioxide is 31.2 ℃ and 7.39 MPa.
(10) The equal fixedly connected with sampling tube of entrance point and the exit end of adsorbing the urn installs the detector on the sampling tube, and the sampling tube plays the effect of real-time sample, and the detector then carries out the content detection of active material to the carbon dioxide of sample.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of the adsorption assembly of the present invention;
FIG. 3 is a schematic structural view of a magnetic core block according to the present invention;
FIG. 4 is a cross-sectional view taken along line A-A of FIG. 3;
FIG. 5 is a schematic view of the suction assembly of the present invention in a retracted state;
FIG. 6 is a schematic structural view of an adsorption yarn separating part according to the present invention;
FIG. 7 is a schematic view of the adsorption state of the adsorption element according to the present invention;
FIG. 8 is a schematic view showing the supercritical state of carbon dioxide according to the present invention.
The reference numbers in the figures illustrate:
1 holding vessel, 2 first three-way pipe, 3 first communicating pipe, 4 condensing tanks, 5 second communicating pipe, 6 pressurizing tank, 7 third communicating pipe, 8 heating tank, 9 extraction kettle, 10 fourth communicating pipe, 11 liquid pump, 12 circulating pipe, 13 separating tank, 14 control box, 15 second three-way pipe, 16 adsorption vat, 17 return pipe, 18 sampling pipe, 19 detector, 20 third three-way pipe, 21 fifth communicating pipe, 22 liquefaction tank, 23 sixth communicating pipe, 24 compressor, 25 mosquito-repellent incense type fixed pipe, 26 gap-adjusting air bag, 27 elastic main wire, 28 central magnetic suction block, 29 adsorption branch wire, 291 adsorption layer, 292 elastic wire, 293 flexible wire, 30 floating ball, 301 foam ball, 302 magnetic block.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise specifically stated or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are used in a broad sense, and for example, "connected" may be a fixed connection, a detachable connection, an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection through an intermediate medium, and a communication between two elements.
Example 1:
referring to fig. 1, an adsorption separation regulation type supercritical fluid extraction apparatus comprises a storage tank 1 and a control box 14, wherein a first three-way pipe 2 is fixedly connected to an inlet end of the storage tank 1, a first communicating pipe 3 is fixedly connected to a right end of the first three-way pipe 2, a condensing tank 4 is fixedly connected to the first communicating pipe 3, a second communicating pipe 5 is fixedly connected to the condensing tank 4, a pressure tank 6 is fixedly connected to the second communicating pipe 5, a third communicating pipe 7 is fixedly connected to the pressure tank 6, a heating tank 8 is fixedly connected to the third communicating pipe 7, an extraction kettle 9 is fixedly connected to the heating tank 8, a fourth communicating pipe 10 is fixedly connected to an outlet end of the extraction kettle 9, an extraction pump 11 is fixedly connected to the fourth communicating pipe 10, a separation tank 13 is fixedly connected to an output end of the extraction pump 11, a second three-way pipe 15 is fixedly connected to an outlet end of the separation tank 13, an, adsorb 16 upper ends fixedly connected with third three-way pipe 20 of urn, fixedly connected with back flow pipe 17 between third three-way pipe 20 and the second three- way pipe 15, 20 left ends fixedly connected with fifth communicating pipe 21 of third three-way pipe, 21 fixedly connected with liquefaction jar 22 of fifth communicating pipe, the exit end fixedly connected with sixth communicating pipe 23 of liquefaction jar 22, sixth communicating pipe 23 fixedly connected with compressor 24, fixedly connected with circulating pipe 12 between the output of compressor 24 and the first three-way pipe 2 upper end, the equal fixedly connected with sampling tube 18 of entrance point and the exit end of absorption urn 16, install detector 19 on the sampling tube 18, sampling tube 18 plays the effect of real-time sample, detector 19 then carries out the content detection of active material to the carbon dioxide of sample.
Referring to fig. 8, the storage tank 1 stores an extraction medium, the extraction medium is carbon dioxide, the critical point condition of the carbon dioxide is 31.2 ℃ and 7.39MPa, the solubility of the solute in the solvent is generally proportional to the density of the solvent, the supercritical carbon dioxide fluid has an extraction capacity equivalent to that of the liquid solvent, and the supercritical carbon dioxide fluid has low viscosity and high permeability of gas, so the mass transfer capacity in the extraction process is much greater than that of the liquid solvent.
The mass transfer mechanism is that supercritical fluid enters the microporous surface of a natural product through external diffusion and internal diffusion, extracted components and the supercritical fluid are subjected to solvation and are dissolved, and the dissolved extracted components enter a supercritical fluid main body through internal diffusion and external diffusion, so that the extraction of effective substances on the Chinese herbal medicines is realized.
Referring to fig. 2-4, the inner end of the adsorption vat 16 is filled with an adsorption component, the adsorption component comprises a mosquito-repellent incense type fixing tube 25 and a plurality of gap-adjusting air bags 26, the gap-adjusting air bags 26 are uniformly distributed along the mosquito-repellent incense type fixing tube 25 and are connected with each other, the mosquito-repellent incense type fixing tube 25 is fixedly connected with the inner end of the adsorption vat 16, a central magnetic suction block 28 is arranged between every four adjacent gap-adjusting air bags 26, an elastic main filament 27 is fixedly connected between the central magnetic suction block 28 and the gap-adjusting air bags 26, electromagnets are installed at the inner end of the central magnetic suction block 28 and are electrically connected with the control box 14 in series, a plurality of adsorption branch filaments 29 which are densely distributed are adhered on the outer surface of the elastic main filament 27, a floating ball 30 is fixedly connected at one end of the adsorption branch filament 29 far away from the elastic main filament 27, the adsorption branch filament 29 plays a role of adsorbing effective substances in carbon dioxide to complete interception, the, realize on the initiative is drawn close and the laminating elasticity owner silk 27, no longer the active absorption active material, carbon dioxide can be passed through fast and is not blockked, elasticity owner silk 27 plays the plastic effect to clearance gasbag 26 on the one hand, on the other hand can provide the absorption and divide silk 29 certain extension space to be used for forming the adsorption net of spatial type, improve the adsorption effect, the expansion and the shrink of clearance gasbag 26 can be adjusted in its own elastic deformation effect, be used for adjusting the velocity of flow of carbon dioxide in the adsorption component, the length of absorption after dividing silk 29 extension is not less than the maximum length of elasticity owner silk 27, avoid under the maximum length of elasticity owner silk 27, floating ball 30 "pulls" the absorption after receiving the absorption of electro-magnet divides silk 29, the absorption life-span of extension absorption branch silk 29.
The upper end of the gap adjusting air bag 26 is provided with an inflation inlet which is made of rubber, a gas flow passage is drilled in the mosquito-repellent incense type fixing tube 25 and is communicated with the inflation inlet, an inflation pump is installed at the outer end of the adsorption urn 16, the output end of the inflation pump is connected with the adsorption urn 16 and is communicated with the gas flow passage, the mosquito-repellent incense type fixing tube 25 can realize the function of fixing the gap adjusting air bag 26 on one hand, and on the other hand, the gap adjusting air bag 26 is directly communicated with the mosquito-repellent incense type fixing tube to realize the functions of inflation and deflation.
Referring to fig. 6, the adsorption separation filament 29 includes an adsorption layer 291, an inner core is disposed at an inner end of the adsorption layer 291, the inner core includes an elastic filament 292 and a flexible filament 293, the elastic filament 292 and the flexible filament 293 are fixedly connected, the adsorption layer 291 plays a role of adsorbing effective substances, the elastic filament 292 plays a role of providing elastic force, is used for naturally unfolding in a non-magnetic state and restoring to an initial space adsorption net shape, the flexible filament 293 has a flexible and changeable characteristic, can swing and deform under the impact of carbon dioxide to increase the contact area with the carbon dioxide, so as to achieve dynamic active adsorption, the elastic filament 292 is an elastic metal material, the flexible filament 293 is a silicon rubber material, the length ratio of the elastic filament 292 to the flexible filament 293 is 1:5-10, the adsorption layer 291 covers the outer surfaces of the elastic filament 292 and the flexible filament 293, and the elastic filament 292 can achieve an elastic supporting effect only under a proper length ratio, the adsorption layer 291 is made of activated carbon fiber material, the fiber diameter is 5-20 μm, the specific surface area is about 1000-1500m2/g on average, the average pore diameter is 1.0-4.0nm, the activated carbon fiber has larger adsorption capacity and faster adsorption dynamic performance than granular activated carbon, has high adsorption efficiency on organic matters, anions and cations in liquid phase and gas phase, has fast adsorption and desorption speed, can be recycled, is acid-resistant, alkali-resistant, high-temperature-resistant, strong in adaptability, good in conductivity and chemical stability, is an ideal environment-friendly material, the floating ball 30 comprises a foam ball 301 and a magnetic block 302, an adsorption cavity is opened at the inner end of the magnetic block 302, the magnetic block 302 is filled in the adsorption cavity, the magnetic block 302 is made of ferromagnetic metal material, the foam ball 301 plays a role in protecting the magnetic block 302, and avoids impact abrasion generated when passive adsorption is closed, meanwhile, the carbon dioxide micro-flow device is light in texture, small in mass under the same volume, large in buoyancy and capable of swinging under the micro-flow impact of carbon dioxide.
During extraction, carbon dioxide in a storage tank 1 enters a condensing tank 4 through a first communicating pipe 3 to be condensed and converted into a vapor state, then the carbon dioxide is heated and pressurized to 31.2 ℃ and 7.39MPa through a pressurizing tank 6 and a heating tank 8 in sequence to be in a supercritical fluid state, an extract to be extracted is added into an extraction kettle 9, the supercritical carbon dioxide fluid is used for extracting effective substances, and after extraction, the carbon dioxide enters a separation tank 13 to be separated under the action of an extraction pump 11, but the separation effect is difficult to achieve the best, so that sampling detection is carried out through a sampling pipe 18 and a detector 19 before entering an adsorption vat 16, if the carbon dioxide is not separated completely, namely the content of the effective substances is mixed, an adsorption component in the adsorption vat 16 starts to operate for adsorption, please refer to fig. 7, when the carbon dioxide passes through gaps between gap adjusting airbags 26, the adsorption devillicate 29 is encountered and impacted, in the swing process of the adsorption devillicate 29, the adsorption layer 291 actively adsorbs effective substances in carbon dioxide, the expansion degree of the gap adjusting air bag 26 is controlled according to the detected content, when the content is higher, the separation is poorer, the gap adjusting air bag 26 should expand more, the gap between the gap adjusting air bag 26 is smaller, the carbon dioxide passing speed is slowed down, in a narrow space, on one hand, the contact adsorption time with the adsorption devillicate 29 is more sufficient, on the other hand, a space adsorption net formed between the adsorption devillicate 29 is tighter, the adsorption effect is better, when the content is lower, the gap adjusting air bag 26 can properly deflate to reduce the volume, the carbon dioxide passing speed is accelerated, the adsorption effect is weakened to a certain extent opposite to the above, when the content is detected to be zero, please refer to figure 5, the gap adjusting air bag 26 is completely deflated and contracted, the gap is released to the maximum, and the electromagnet adsorption floating ball 30, drag absorption branch silk 29 and straighten to paste and cover on elasticity main silk 27, the space adsorption net disintegrates, also disappear along with it with absorption to blocking of carbon dioxide, the speed that carbon dioxide passed through this moment is the biggest, can directly be used for subsequent circulation to use, improve whole extraction efficiency, it is worth noting that still there is the active material in the sample detection of transfer crack gasbag 26 exit end carbon dioxide, then open the solenoid valve on the back flow pipe 17 and close the solenoid valve on the fifth communicating pipe 21, make the carbon dioxide backward flow reenter the absorption jar 16 adsorb to no active material once more, carbon dioxide gets into liquefaction in the liquefaction jar 22 after the absorption and liquefies into liquid, and get into holding vessel 1 after compressing by compressor 24 and store and be used for the extraction circulation.
The invention can extract effective substances from Chinese herbal medicines by utilizing the supercritical characteristic of carbon dioxide, has mild extraction regulation, no pollution, strong extraction capacity, high extraction rate, short extraction time and short production period, introduces a novel regulation and control type adsorption component when the extracted effective substances enter the separation step, actively adsorbs the incompletely released effective substances in the carbon dioxide to complete interception, improves the recovery rate of the effective substances, can be assisted with the sampling detection technology in the prior art, regulates the adsorption component by detecting the content of the effective substances in the carbon dioxide, ensures that the carbon dioxide can be rapidly recycled on the premise of meeting the adsorption interception, obviously improves the integral extraction efficiency and quality, and facilitates the desorption and recovery of the effective substances by the adsorption component and continues to be recycled.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (10)
1. The utility model provides an adsorption separation regulation and control formula supercritical fluid extraction equipment, includes holding vessel (1) and control box (14), its characterized in that: the device is characterized in that a first three-way pipe (2) is fixedly connected with an inlet end of the storage tank (1), a first communicating pipe (3) is fixedly connected with the right end of the first three-way pipe (2), a condensing tank (4) is fixedly connected with the first communicating pipe (3), the condensing tank (4) is fixedly connected with a second communicating pipe (5), a pressurizing tank (6) is fixedly connected with the second communicating pipe (5), a third communicating pipe (7) is fixedly connected with the pressurizing tank (6), a heating tank (8) is fixedly connected with the third communicating pipe (7), an extraction kettle (9) is fixedly connected with the heating tank (8), a fourth communicating pipe (10) is fixedly connected with an outlet end of the extraction kettle (9), a liquid pump (11) is fixedly connected with the fourth communicating pipe (10), a separation tank (13) is fixedly connected with an output end of the liquid pump (11), and a second three-way pipe (15) is fixedly connected with an outlet end of, the utility model discloses a liquefaction system, including first three-way pipe (15), second three-way pipe (15) upper end fixedly connected with adsorbs vat (16), adsorb vat (16) upper end fixedly connected with third three-way pipe (20), fixedly connected with back flow (17) between third three-way pipe (20) and second three-way pipe (15), third three-way pipe (20) left end fixedly connected with fifth communicating pipe (21), fifth communicating pipe (21) fixedly connected with liquefaction jar (22), the exit end fixedly connected with sixth communicating pipe (23) of liquefaction jar (22), sixth communicating pipe (23) fixedly connected with compressor (24), fixedly connected with circulating pipe (12) between the output of compressor (24) and first three-way pipe (2) upper end.
2. The apparatus of claim 1, wherein the supercritical fluid extraction apparatus comprises: the inner end of the adsorption vat (16) is filled with an adsorption component which comprises a mosquito-repellent incense type fixed tube (25) and a plurality of gap-adjusting air bags (26), and the gap-adjusting air bags (26) are evenly distributed along the mosquito-repellent incense type fixed pipe (25) and are mutually connected, the mosquito-repellent incense type fixed pipe (25) is fixedly connected with the inner end of the adsorption urn (16), a central magnetic suction block (28) is arranged between every four adjacent gap-adjusting air bags (26), an elastic main wire (27) is fixedly connected between the central magnetic suction block (28) and the gap adjusting air bag (26), an electromagnet is arranged at the inner end of the central magnetic suction block (28), the electromagnets are connected in series and electrically connected with the control box (14), a plurality of adsorption branch wires (29) which are densely distributed are adhered on the outer surface of the elastic main wire (27), one end of the adsorption dividing wire (29) far away from the elastic main wire (27) is fixedly connected with a floating ball (30).
3. The apparatus of claim 2, wherein the supercritical fluid extraction apparatus comprises: adsorb and divide silk (29) including adsorbed layer (291), adsorbed layer (291) inner is equipped with the inner core, the inner core includes stretch yarn (292) and flexible silk (293), and fixed connection between stretch yarn (292) and the flexible silk (293).
4. The supercritical fluid extraction apparatus according to claim 3, wherein: the elastic wire (292) is made of elastic metal materials, the flexible wire (293) is made of silicon rubber materials, the length ratio of the elastic wire (292) to the flexible wire (293) is 1:5-10, and the adsorption layer (291) covers the outer surfaces of the elastic wire (292) and the flexible wire (293).
5. The supercritical fluid extraction apparatus according to claim 3, wherein: the adsorption layer (291) is made of activated carbon fiber material, the fiber diameter is 5-20 μm, the specific surface area is about 1000-1500m2/g on average, and the average pore diameter is 1.0-4.0 nm.
6. The apparatus of claim 2, wherein the supercritical fluid extraction apparatus comprises: the floating ball (30) comprises a foam ball (301) and a magnetic block (302), an adsorption cavity is formed in the inner end of the magnetic block (302), the magnetic block (302) is filled in the adsorption cavity, and the magnetic block (302) is made of a ferromagnetic metal material.
7. The apparatus of claim 2, wherein the supercritical fluid extraction apparatus comprises: the length of the adsorption dividing wire (29) after being stretched is not less than the maximum length of the elastic main wire (27).
8. The apparatus of claim 1, wherein the supercritical fluid extraction apparatus comprises: transfer clearance gasbag (26) upper end and be provided with the inflation inlet, the inflation inlet adopts the rubber material, it has gas flow channel to open in the fixed pipe of mosquito-repellent incense type (25), and gas flow channel is linked together with the inflation inlet, the inflator pump is installed to absorption urn (16) outer end, and the output of inflator pump with adsorb urn (16) and be connected with gas flow channel and be linked together.
9. The apparatus of claim 1, wherein the supercritical fluid extraction apparatus comprises: an extraction medium is stored in the storage tank (1), the extraction medium is carbon dioxide, and the critical point condition of the carbon dioxide is 31.2 ℃ and 7.39 MPa.
10. The apparatus of claim 1, wherein the supercritical fluid extraction apparatus comprises: the inlet end and the outlet end of the adsorption vat (16) are both fixedly connected with a sampling tube (18), and a detector (19) is arranged on the sampling tube (18).
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