CN111974024B - Supercritical extraction device for traditional chinese medicine based on high-energy microbubble technique - Google Patents

Abstract

The invention discloses a supercritical extraction device for traditional Chinese medicine based on a high-energy micro-bubble technology, which belongs to the field of supercritical extraction devices, wherein supercritical carbon dioxide is continuously injected into an extraction kettle body through a feed pipe, the supercritical carbon dioxide can form supercritical carbon dioxide bubbles when passing through the high-energy micro-bubble generation device and rises in feed liquid, the supercritical carbon dioxide bubbles are easily exploded along with the rising of the supercritical carbon dioxide bubbles, the supercritical carbon dioxide bubbles are easily exploded, part of the supercritical carbon dioxide bubbles without self-explosion are easily exploded under the action of external force extrusion stimulation after touching a foam-extinguishing net, and the instantaneous energy generated by explosion can uniformly mix the supercritical carbon dioxide with the feed liquid, so that the extraction efficiency of the supercritical carbon dioxide in the feed liquid is greatly improved.

Description

Supercritical extraction device for traditional chinese medicine based on high-energy microbubble technique

Technical Field

The invention relates to the field of supercritical extraction devices, in particular to a traditional Chinese medicine supercritical extraction device based on a high-energy micro-bubble technology.

Background

Supercritical is a supercritical fluid, which is a non-gaseous and non-liquid state between gas and liquid, which can only exist when its temperature and pressure exceed critical points. Supercritical fluids have a higher density, similar to liquids, and a viscosity closer to gases. The principle of supercritical CO2 fluid extraction (SFE) separation is therefore a very desirable extractant by utilizing the relationship between the dissolution capacity of the supercritical fluid and its density, i.e. by utilizing the influence of pressure and temperature on the dissolution capacity of the supercritical fluid. In the supercritical state, the supercritical fluid is contacted with the substance to be separated to selectively extract the components with polarity, boiling point and molecular weight in sequence. Of course, the extracts obtained corresponding to the pressure ranges 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 common gas by means of decompression and temperature rising, and the extracted substances are completely or basically separated out, so that the purpose of separation and purification is achieved, and the supercritical CO2 fluid extraction process is formed by combining the extraction and separation processes.

Because supercritical extraction has higher device cost and more severe production conditions, the supercritical extraction is commonly used for extracting high-value substances, and the effective target components in the traditional Chinese medicine exactly meet the requirements, so that the effective target components in the pre-traditional Chinese medicine, which are difficult to be purified by the traditional technology, are usually purified by supercritical extraction.

However, because the components of the traditional Chinese medicine are complex, flocculent or other impurities generated by interfering components are very easy to influence the extraction efficiency of the traditional Chinese medicine in the supercritical extraction process, and meanwhile, the impurities are easy to be mixed in the extraction liquid, so that the subsequent purification of the effective target components is influenced.

Disclosure of Invention

1. Technical problem to be solved

Aiming at the problems existing in the prior art, the invention aims to provide a supercritical extraction device for traditional Chinese medicine based on a high-energy micro-bubble technology, which can greatly reduce the influence of flocculent or other impurities generated in the supercritical extraction process of the traditional Chinese medicine on the supercritical extraction efficiency, and is not easy to influence the subsequent purification of effective target components.

2. Technical proposal

In order to solve the problems, the invention adopts the following technical scheme.

The utility model provides a supercritical fluid extraction device for traditional chinese medicine based on high energy microbubble technique, includes extraction cauldron main part, hold feed liquid and extract in the extraction cauldron main part, extraction cauldron main part upper end opening fixedly connected with and self assorted kettle cover, be connected with sealing washer between extraction cauldron main part and the kettle cover, and sealing washer and kettle cover fixed connection, the lower extreme fixedly connected with inlet pipe of extraction cauldron main part, the inlet pipe is close to the one end of extraction cauldron main part and runs through the inlet pipe and extend to in the extraction cauldron main part, the inlet pipe is located the one end fixedly connected with of extraction cauldron main part and self assorted high energy microbubble generating device, the one end of extraction cauldron main part is gone up to open a pair of spacing spout, the extraction cauldron main part sliding connection has the net frame with self assorted, the ear piece portion on round frame portion and the outer wall of fixed connection, and ear piece portion and spacing spout phase-match, realize directional sliding connection through spacing spout and ear piece portion between extraction main part and the net frame, the notch department fixed connection of spacing spout runs through and blocks up and prevents that the cross-like fibrous that can form a plurality of critical fibrous that can cross and influence each other and cut apart in a plurality of critical fibrous that can be difficult to realize in the extraction, the fibrous that can cut into a plurality of different pieces or the fibrous supercritical fluid is difficult to realize in the supercritical fluid extraction process.

Further, the density of the feed liquid and the density of the extraction liquid have obvious differences, the density of the feed liquid is slightly higher than that of the extraction liquid, technicians can adjust the density of the feed liquid by using inert inorganic salts only dissolved in the feed liquid, and the overall density of the net frame and the foam-extinguishing net is similar to that of the feed liquid, so that the net frame and the foam-extinguishing net can be suspended in the feed liquid and can only be at the bottom of the extraction liquid, after the extraction liquid and the feed liquid are layered, the net frame and the foam-extinguishing net are always in the feed liquid layer, the detonation work of supercritical carbon dioxide bubbles can be performed in the feed liquid layer as much as possible, and the utilization efficiency of supercritical carbon dioxide bubbles is increased.

Further, a limiting slide bar is fixedly connected between the side walls of the limiting slide groove, and penetrates through the screen frame, and the limiting slide bar has a limiting function, so that the screen frame is not easy to incline or roll over when sliding in the extraction kettle main body.

Further, be connected with the wear-resisting ring between frame and the spacing slide bar, wear-resisting ring and frame fixed connection, wear-resisting ring can reduce the wearing and tearing between frame and the spacing slide bar by a wide margin, makes the connection between frame and the spacing slide bar be difficult for appearing rocking.

Further, the foam-extinguishing net comprises a net body, the lower end of the net body is fixedly connected with a needle-breaking net, and a section of the needle-breaking net, which is far away from the net body, is a sharp end, so that carbon dioxide bubbles in a supercritical state can be conveniently punctured.

Further, the side wall of broken needle net is last fixedly connected with catches the barb, it has the elasticity cavity to catch the in-situ cutting of barb, catches the barb and can catch the flocculent impurity of suspension in the feed liquid, and the catching barb that has excavated the elasticity cavity can increase self elasticity by a wide margin, when not influencing broken needle net and catching the effect, can directly clear up broken needle net bending deformation with external force, conveniently follow-up to catching the barb and unify the clearance.

Further, elastic fiber includes the fibre main part, the excavation has the filling chamber in the fibre main part, and fills the chamber and keep away from the link of preventing blockking up curtain and spacing spout lateral wall, can increase by a wide margin and prevent blockking up the elasticity of curtain, be difficult for making under the effect of net frame prevent blockking up the curtain and take place hard fracture.

Further, the main rod is inserted into the filling cavity, both ends of the main rod are fixedly connected with the fiber main body, a plurality of filling particles are filled in the filling cavity, the main rod can increase the toughness of the fiber main body, and the filling particles can increase the strength of the fiber main body, so that the fiber main body is not easy to generate overlarge elastic deformation under the action of external force, and the fiber main body is not easy to be broken directly.

Further, the outside fixedly connected with a plurality of capillary fibers of trunk stick, the one end that trunk stick was kept away from to capillary fibers runs through filling granule and fibre main part in proper order and extends to the outside of fibre main part, and capillary fibers can strengthen the fibre main part, makes the fibre main part be difficult for taking place to crack or fracture because of excessive deformation, and the capillary fibers that runs through filling granule form fixed relation each other simultaneously, and when the fibre main part takes place to crack or fracture, capillary fibers very difficult follow trunk stick drops, and filling granule also is difficult for spilling from filling the intracavity, is difficult for influencing the extraction environment in the extraction cauldron main part, and also realizes connecting through the capillary fibers of intertwining between two adjacent anti-clogging curtains.

3. Advantageous effects

Compared with the prior art, the invention has the advantages that:

According to the scheme, the liquid level of the feed liquid in the extraction kettle main body is not low, the height of a screen frame and the height of a foam extinguishing net are low, the temperature and the air pressure in the extraction kettle main body are regulated to the critical condition of the carbon dioxide serving as an extractant, the supercritical carbon dioxide is continuously injected into the extraction kettle main body through a feed pipe, the supercritical carbon dioxide can form supercritical carbon dioxide bubbles when passing through a high-energy micro-bubble generating device, the supercritical carbon dioxide bubbles rise in the feed liquid, the pressure of the supercritical carbon dioxide bubbles is reduced along with rising of the supercritical carbon dioxide bubbles, the supercritical carbon dioxide bubbles are extremely easy to explode, part of the supercritical carbon dioxide bubbles without self-explosion are also extremely easy to explode under the action of external force extrusion stimulation after touching the foam extinguishing net, the instant energy generated by explosion can uniformly mix the supercritical carbon dioxide with the feed liquid, the extraction efficiency of the supercritical carbon dioxide can be greatly increased, the influence of flocculent or other impurities generated in the supercritical extraction process of the traditional Chinese medicine on the supercritical extraction efficiency can be greatly reduced, and the purification of the effective target components is not easily affected.

Drawings

FIG. 1 is an exploded view of the main structure of the extraction vessel of the present invention;

FIG. 2 is a schematic structural view of an extraction tank according to the present invention;

FIG. 3 is a front cross-sectional view of the extraction pot of the present invention;

FIG. 4 is a schematic diagram of the structure shown at A in FIG. 3;

FIG. 5 is a schematic view of the partial structure of the surface of the foam control net of the present invention;

FIG. 6 is a front cross-sectional view of an elastic fiber of the present invention;

Fig. 7 is a schematic diagram of the structure at B in fig. 6.

The reference numerals in the figures illustrate:

1 extraction kettle main body, 2 kettle cover, 3 sealing washer, 4 inlet pipe, 5 high energy microbubble generating device, 6 spacing spout, 7 net frame, 8 foam control net, 801 net body, 802 broken foam needle, 803 catching barb, 804 elastic cavity, 9 spacing slide bar, 10 wear ring, 11 anti-blocking curtain, 1101 fiber main body, 1102 filling cavity, 1103 trunk stick, 1104 filling particle, 1105 capillary fiber.

Detailed Description

The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, based on the embodiments of the present invention, and all other embodiments obtained by those skilled in the art without making any inventive effort are within the scope of the present invention.

In the description of the present invention, it should be noted that the positional or positional relationship indicated by the terms such as "upper", "lower", "inner", "outer", "top/bottom", etc. are based on the positional or positional relationship shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, 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, unless explicitly specified and limited otherwise, the terms "mounted," "configured to," "engaged with," "connected to," and the like are to be construed broadly, and include, for example, "connected to," whether fixedly connected to, detachably connected to, or integrally connected to, mechanically connected to, electrically connected to, directly connected to, indirectly connected to, and in communication with each other via an intermediate medium. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.

Example 1:

Referring to fig. 1-4, a supercritical extraction device for traditional Chinese medicine based on high-energy micro-bubble technology comprises an extraction kettle body 1, wherein the extraction kettle body 1 is internally provided with feed liquid and extract liquid for supercritical extraction, a kettle cover 2 matched with the extraction kettle body 1 is fixedly connected with an opening at the upper end of the extraction kettle body 1, a sealing gasket 3 is connected between the extraction kettle body 1 and the kettle cover 2, the sealing gasket 3 is fixedly connected with the kettle cover 2, the extraction kettle body 1 and the kettle cover 2 are fixedly connected and detached through a buckle, which is a technology known to a person skilled in the art, so that the detailed description and drawing in the specification are omitted, the lower end of the extraction kettle body 1 is fixedly connected with a feed pipe 4, one end of the feed pipe 4 close to the extraction kettle body 1 penetrates through the feed pipe 4 and extends into the extraction kettle body 1, one end fixedly connected with that inlet pipe 4 is located extraction cauldron main part 1 is located with self assorted high-energy microbubble generating device 5, the cutting has a pair of spacing spout 6 on the lateral wall of extraction cauldron main part 1, sliding connection has with self assorted carriage 7 in extraction cauldron main part 1, carriage 7 includes round frame portion and fixed connection's ear piece portion on round frame portion lateral wall, and ear piece portion and spacing spout 6 assorted, realize directional sliding connection through spacing spout 6 and ear piece portion between extraction cauldron main part 1 and carriage 7, the notch department fixedly connected with of spacing spout 6 prevents blockking up curtain 11, prevent blockking up curtain 11 and include a plurality of elastic fiber, cross winding is in the same place each other between a plurality of elastic fiber, form a plurality of compartments of cutting apart usefulness, the compartment has the effect of keeping apart, make impurity in the feed liquid be difficult for getting into spacing spout 6, be difficult for influencing the normal sliding of carriage 7.

In particular, the structure of temperature and air pressure detection control device, discharging system and the like are needed to be configured for normal operation of the extraction kettle body 1, meanwhile, a solenoid valve, a supply pump and other power structures which can control the opening or closing of the feed pipe 4 are needed to be installed in the feed pipe 4 so as to ensure that the extraction kettle body 1 can normally operate, and the specific structure and the matching mode with the extraction kettle body 1 in the application are all known techniques of the technical personnel in the field, so that the detailed description and drawing in the specification are not needed, when the extraction kettle body 1 normally operates, the kettle cover 2 is in a sealed state, the extraction kettle body 1 is filled with the liquid for extraction, the liquid level of the liquid in the extraction kettle body 1 is not lower than the height of the net frame 7 and the bubble-killing net 8, the temperature and the air pressure in the extraction kettle body 1 are adjusted to the critical condition of the carbon dioxide of the extractant, carbon dioxide in a supercritical state is continuously injected into the extraction kettle main body 1 through the feed pipe 4, carbon dioxide bubbles in the supercritical state can be formed when passing through the high-energy microbubble generating device 5 and rise in the feed liquid, along with the rising of the carbon dioxide bubbles in the supercritical state, the self-received hydraulic pressure is reduced, the carbon dioxide bubbles in the supercritical state are extremely easy to explode, part of the carbon dioxide bubbles in the supercritical state which do not explode automatically are also extremely easy to explode under the action of external force extrusion stimulation after touching the foam-extinguishing net 8, the instant energy generated by the explosion can uniformly mix the carbon dioxide in the supercritical state with the feed liquid, the extraction efficiency of the carbon dioxide in the supercritical state in the feed liquid is greatly increased, the influence of flocculent or other impurities generated in the supercritical extraction process of traditional Chinese medicines on the supercritical extraction efficiency can be greatly reduced, the subsequent purification of the effective target components is not easy to be influenced.

Referring to fig. 4, the density of the liquid and the density of the extract are obviously different, the density of the liquid is slightly higher than that of the extract, a technician can adjust the density of the liquid by using inert inorganic salt only dissolved in the liquid, the overall density of the net frame 7 and the foam-extinguishing net 8 is similar to that of the liquid, so that the net frame 7 and the foam-extinguishing net 8 can be suspended in the liquid and can only sink at the bottom of the extract, after the extract and the liquid are layered, the net frame 7 and the foam-extinguishing net 8 are always in the liquid layer, the detonation of supercritical carbon dioxide bubbles can be performed in the liquid layer as much as possible, the utilization efficiency of supercritical carbon dioxide bubbles is increased, a limit slide bar 9 is fixedly connected between the side walls of the limit slide groove 6, the limit slide bar 9 penetrates through the net frame 7, the limit slide bar 9 has a limit function, the net frame 7 is not easy to incline or roll over when the net frame 7 slides in the extraction kettle body 1, a wear-resistant ring 10 is connected between the net frame 7 and the limit slide bar 9, the wear-resistant ring 10 is fixedly connected with the net frame 7, the wear-resistant ring 10 can be greatly reduced, the wear-resistant ring 9 is easy to be connected between the net frame 7 and the limit slide bar 9, and the limit slide bar is not easy to shake.

Referring to fig. 5, the foam-killing net 8 includes a net body 801, a needle-breaking net 802 is fixedly connected to the lower end of the net body 801, a section of the needle-breaking net 802 away from the net body 801 is a sharp end, so that carbon dioxide bubbles in a supercritical state can be conveniently punctured, a capturing barb 803 is fixedly connected to the side wall of the needle-breaking net 802, an elastic cavity 804 is cut in the capturing barb 803, flocculent impurities suspended in feed liquid can be captured by the capturing barb 803, the elasticity of the capturing barb 803 cutting the elastic cavity 804 can be greatly increased, and when the capturing effect of the needle-breaking net 802 is not affected, the bending deformation of the needle-breaking net 802 can be directly cleaned by external force, so that the capturing barb 803 can be conveniently and uniformly cleaned.

Referring to fig. 6-7, the elastic fiber includes a fiber main body 1101, a filling cavity 1102 is cut in the fiber main body 1101, and the filling cavity 1102 is far away from the connecting end of the anti-blocking curtain 11 and the side wall of the limiting chute 6, so that the elasticity of the anti-blocking curtain 11 can be greatly increased, the anti-blocking curtain 11 is not easy to be hard broken under the action of the net frame 7, a main rod 1103 is inserted in the filling cavity 1102, both ends of the main rod 1103 are fixedly connected with the fiber main body 1101, a plurality of filling particles 1104 are filled in the filling cavity 1102, the main rod 1103 can increase the toughness of the fiber main body 1101, the filling particles 1104 can increase the strength of the fiber main body 1101, so that the fiber main body 1101 is not easy to generate excessive elastic deformation under the action of external force, the fiber main body 1101 is not easy to be directly broken, the outside fixedly connected with a plurality of capillary fibers 1105 of backbone stick 1103, the one end that the capillary fibers 1105 kept away from backbone stick 1103 runs through filling granule 1104 and fiber main part 1101 in proper order and extends to the outside of fiber main part 1101, capillary fibers 1105 can strengthen fiber main part 1101, make fiber main part 1101 be difficult for taking place to crack or fracture because of excessive deformation, the capillary fibers 1105 that runs through filling granule 1104 form fixed relation each other simultaneously, when fiber main part 1101 takes place to crack or fracture, capillary fibers 1105 very difficult follow backbone stick 1103 and drop, filling granule 1104 also is difficult for spilling from filling intracavity 1102, be difficult for influencing the extraction environment in the extraction cauldron main part 1, and connect through the capillary fibers 1105 of intertwining between two adjacent anti-clogging curtains 11.

According to the scheme, the liquid level of the feed liquid in the extraction kettle main body 1 is not low, the height of the screen frame 7 and the height of the foam extinguishing net 8 are low, the temperature and the air pressure in the extraction kettle main body 1 are regulated to the critical condition of the extractant carbon dioxide, the supercritical carbon dioxide is continuously injected into the extraction kettle main body 1 through the feeding pipe 4, the supercritical carbon dioxide can form supercritical carbon dioxide bubbles when passing through the high-energy micro-bubble generating device 5, the supercritical carbon dioxide bubbles rise in the feed liquid, the hydraulic pressure of the supercritical carbon dioxide bubbles is reduced along with the rising of the supercritical carbon dioxide bubbles, the supercritical carbon dioxide bubbles are extremely easy to explode, part of the supercritical carbon dioxide bubbles without self-explosion are also extremely easy to explode under the action of external force extrusion stimulation after touching the foam extinguishing net 8, the instantaneous energy generated by explosion can uniformly mix the supercritical carbon dioxide with the feed liquid, the extraction efficiency of the supercritical carbon dioxide can be greatly increased, the influence of flocculent or other impurities generated in the supercritical extraction process of the traditional Chinese medicine can be greatly reduced, and the purification of the following effective target components is not easily affected.

The above description is only of the preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, any person skilled in the art should be able to make equivalent substitutions or modifications according to the technical solution and the modified concept thereof within the scope of the present invention.

Claims (7)

1. A supercritical extraction device for Chinese medicine based on high-energy microbubble technology, comprising an extraction kettle body (1), wherein the extraction kettle body (1) contains feed liquid and extract liquid, the upper end opening of the extraction kettle body (1) is fixedly connected to a kettle cover (2) matching the extraction kettle body, a sealing gasket (3) is connected between the extraction kettle body (1) and the kettle cover (2), and the sealing gasket (3) is fixedly connected to the kettle cover (2), the lower end of the extraction kettle body (1) is fixedly connected to a feed pipe (4), one end of the feed pipe (4) close to the extraction kettle body (1) passes through the feed pipe (4) and extends into the extraction kettle body (1), characterized in that: one end of the feed pipe (4) located in the extraction kettle body (1) is fixedly connected to a high-energy microbubble generating device (5) matching the extraction kettle body, a pair of limiting sliding grooves (6) are cut on the side wall of the extraction kettle body (1), and a mesh frame (7) matching the extraction kettle body (1) is slidably connected inside the extraction kettle body (1), The net frame (7) comprises a circular frame portion and an ear block portion fixedly connected to the outer wall of the circular frame portion, and the ear block portion matches the limiting slide groove (6). The extraction kettle body (1) and the net frame (7) are directional slidingly connected through the limiting slide groove (6) and the ear block portion. The notch of the limiting slide groove (6) is fixedly connected with an anti-blocking curtain (11), and the anti-blocking curtain (11) comprises a plurality of elastic fibers, and the plurality of elastic fibers are cross-entangled with each other to form a plurality of partitioning compartments. The defoaming net (8) is installed inside the net frame (7). There is a significant difference in density between the feed liquid and the extraction liquid, and the density of the feed liquid is slightly higher than that of the extraction liquid. The overall density of the net frame (7) and the defoaming net (8) is close to that of the feed liquid. The defoaming net (8) comprises a net body (801), and a pin-breaking net (802) is fixedly connected to the lower end of the net body (801), and a section of the pin-breaking net (802) away from the net body (801) is a sharp end. 2. A supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology according to claim 1, characterized in that a limiting slide bar (9) is fixedly connected between the side walls of the limiting slide groove (6), and the limiting slide bar (9) passes through the mesh frame (7). 3. According to a supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology as described in claim 1, it is characterized in that: a wear-resistant ring (10) is connected between the mesh frame (7) and the limiting sliding rod (9), and the wear-resistant ring (10) is fixedly connected to the mesh frame (7). 4. A supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology according to claim 3, characterized in that: a capture barb (803) is fixedly connected to the side wall of the needle-breaking net (802), and an elastic cavity (804) is excavated inside the capture barb (803). 5. A supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology according to claim 4, characterized in that: the elastic fiber includes a fiber body (1101), a filling cavity (1102) is excavated in the fiber body (1101), and the filling cavity (1102) is far away from the connection end of the anti-blocking curtain (11) and the side wall of the limiting slide groove (6). 6. A supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology according to claim 5, characterized in that: a main rod (1103) is inserted into the filling cavity (1102), both ends of the main rod (1103) are fixedly connected to the fiber body (1101), and the filling cavity (1102) is filled with a plurality of filling particles (1104). 7. A supercritical extraction device for traditional Chinese medicine based on high-energy microbubble technology according to claim 6, characterized in that: a plurality of capillary fibers (1105) are fixedly connected to the outside of the main rod (1103), and the end of the capillary fiber (1105) away from the main rod (1103) sequentially penetrates the filling particles (1104) and the fiber body (1101) and extends to the outside of the fiber body (1101).