CN112386944B - Supercritical fluid high-efficiency extraction separation device for pharmacy - Google Patents
Supercritical fluid high-efficiency extraction separation device for pharmacy Download PDFInfo
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- CN112386944B CN112386944B CN202011147208.8A CN202011147208A CN112386944B CN 112386944 B CN112386944 B CN 112386944B CN 202011147208 A CN202011147208 A CN 202011147208A CN 112386944 B CN112386944 B CN 112386944B
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- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
Abstract
The invention discloses a supercritical fluid high-efficiency extraction separation device for pharmacy, which belongs to the field of supercritical fluid extraction, and is characterized in that crushed extract is filled into a contraction extrusion bag in advance to expand the contraction extrusion bag, the contraction extrusion bag is shrunk by utilizing the increase of pressure in the extraction process, a feed channel is sealed by utilizing an elastic connecting piece through a blocking ball, so that the contraction extrusion bag extrudes the extract from a magnetic sealing sheet, the contact area of the extract and CO2 is increased, the extraction efficiency is improved, the flow rate of CO2 is reduced by utilizing a blocking ball with a bent channel, the residence time of CO2 is prolonged, the contact time of the extract and CO2 is increased, the extraction efficiency is further improved, compared with the prior art, the contact time and the contact area of the extract and the CO2 are improved, and the extraction efficiency is greatly improved.
Description
Technical Field
The invention relates to the field of supercritical fluid extraction, in particular to a supercritical fluid high-efficiency extraction separation device for pharmacy.
Background
Supercritical fluid extraction is a novel extraction separation technology. It uses supercritical fluid, i.e. fluid in thermodynamic state with temperature higher than critical temperature and pressure higher than critical pressure, as extractant. Extracting specific components from liquid or solid to achieve the separation purpose. The supercritical fluid extraction is characterized in that; the extractant is gas at normal pressure and room temperature, and is easy to separate from raffinate phase and extraction component after extraction; operating at a lower degree of fullness, particularly suitable for the separation of natural substances; the pressure, temperature and entrainer can be adjusted to adjust the solvency of the supercritical fluid and the extracted component can be introduced into the desired product by gradually changing the density and temperature and pressure.
The characteristics of supercritical extraction determine that the application range is very wide. For example, in the pharmaceutical industry, it can be used for extracting effective components from Chinese herbal medicines, refining heat-sensitive biological medicines, and separating lipid mixtures. CO2 is safe, nontoxic and cheap liquid, supercritical CO2 has the diffusion coefficient similar to gas and the dissolving power of liquid, the surface tension is zero, the supercritical CO2 can quickly permeate into solid substances to extract essence of the solid substances, the supercritical CO2 has the characteristics of high efficiency, difficult oxidation, pure nature, no chemical pollution and the like, and the change of the flow of CO2 has two effects on the supercritical extraction. Too large a flow of CO2 increases the CO2 flow rate in the extractor, shortens the CO2 residence time, reduces the contact time with the extracted matter, and is not favorable for improving the extraction rate. On the other hand, the flow of CO2 is increased, so that the mass transfer driving force in the extraction process can be increased, the mass transfer coefficient is correspondingly increased, the mass transfer rate is accelerated, and the extraction capacity of the SFE is improved.
In order to improve the extraction efficiency, the contact time and the contact area between the CO2 and the extracted matter are mostly increased by arranging a contact plate in the conventional supercritical fluid extractor, but the problem is solved from the aspect of CO2, the particle size of the extracted matter is an important factor influencing the extraction efficiency, and a device for improving the extraction efficiency from the aspects of both CO2 and the extracted matter is not provided at present.
Disclosure of Invention
1. Technical problem to be solved
In view of the problems in the prior art, the invention aims to provide a supercritical fluid high-efficiency extraction and separation device for pharmacy, which fills a shrunk and extruded bag with crushed extract in advance, the material is expanded, the contracted extrusion bag is contracted by utilizing the increase of pressure in the extraction process, the feed channel is sealed by utilizing the elastic connecting piece to lead the ball plug to be closed, thereby the extracted matter is extruded and sprayed out of the magnetic sealing sheet by the contraction extrusion bag, the contact area of the extracted matter and CO2 is increased, the extraction efficiency is improved, and the flow rate of CO2 is reduced by a blocking ball with a bent channel, so that the residence time of CO2 is prolonged, the contact time of the extracted matter and CO2 is increased, the extraction efficiency is further improved, compared with the prior art, the method improves the contact time and the contact area of CO2 and the extracted substance, and greatly improves the extraction efficiency.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A supercritical fluid high-efficiency extraction separation device for pharmacy comprises an extractor body, wherein the upper end and the lower end of the extractor body are respectively provided with a feed inlet and a discharge outlet, a feed pipe is inserted into the upper part of the extractor body, the lower end of the feed pipe is communicated with a contraction extrusion bag, an extract can be mixed with CO2 to be filled when being filled into the contraction extrusion bag, so that the CO2 can ensure that the contraction extrusion bag expands and can also be used as a raw material to be supplemented into supercritical CO2, the inner wall of the upper end of the feed pipe is fixedly connected with an installation block, the installation block is internally provided with a feed channel, a cylindrical channel and a discharge channel from top to bottom in sequence, the inner wall of the lower end of the installation block is fixedly connected with a support rod, a blocking ball is arranged above the support rod, an elastic connecting piece is fixedly connected between the blocking ball and the support rod, and the side wall of the feed pipe below the installation block is provided with a plurality of openings, and the inner wall of each opening is fixedly connected with two magnetic closed sheets which are symmetrically arranged, a plurality of blocking plates are fixedly connected between the outer side wall of the feeding pipe and the inner wall of the extractor body and positioned on two sides of the opening, a plurality of holes are formed in each blocking plate, and a plurality of blocking balls are embedded in each blocking plate. The method comprises the steps of filling crushed extracted substances into a contraction extrusion bag in advance to expand the contraction extrusion bag, reducing the contraction extrusion bag by utilizing the increase of pressure in the extraction process, sealing a feeding channel by utilizing an elastic connecting piece to enable a blocking ball to extrude the extracted substances out of a magnetic sealing sheet, so that the contact area of the extracted substances and CO2 is increased, the extraction efficiency is improved, and the flow rate of CO2 is reduced by utilizing the blocking ball with a bent channel, so that the residence time of CO2 is prolonged, the contact time of the extracted substances and CO2 is increased, the extraction efficiency is further improved, compared with the prior art, the contact time and the contact area of the CO2 and the extracted substances are improved, and the extraction efficiency is greatly improved.
Further, the shrinkage squeezing bag comprises an outer bag and an inner bag, the outer bag and the inner bag have elasticity and can be shrunk and changed, elastic fillers are filled between the outer bag and the inner bag, the elastic fillers are soft elastic materials, the elastic fillers increase the elasticity of the shrinkage squeezing bag, the shrinkage squeezing bag expands when the powdery extracted materials are filled, and when the powdery extracted materials are pressurized in the extraction process, the pressure enables the shrinkage squeezing bag to shrink, so that the extracted materials are sprayed out.
Furthermore, the elastic connecting piece comprises a supporting body, the supporting body is in a vertical state in a free state, two elastic rods are embedded in the supporting body, the supporting body is made of rubber materials, when the extracted matter is filled into the contraction extrusion bag, the blocking ball is pushed open, the elastic connecting piece is bent at the moment, and after the filling of the extracted matter is stopped, the elastic force of the elastic rods enables the supporting body to be stretched straight, so that the cylindrical channel is blocked by the blocking ball.
Furthermore, the magnetic sealing sheet comprises a silica gel sheet, magnet blocks are embedded in the free ends of the silica gel sheet, the magnets of the two opposite magnet blocks are opposite in magnetism, the two magnet blocks are adsorbed together in a free state, the extracted matter can be prevented from directly entering the extractor body in the filling process, and when the contraction extrusion bag starts to contract, the extracted matter pushes the two silica gel sheets open under the extrusion effect, so that the extracted matter is ejected from the position.
Furthermore, the blocking ball comprises a ball body, a plurality of flow channels are formed in the ball body, so that the flow rate of CO2 is reduced, the residence time is prolonged, the CO2 is fully contacted with the extract, and a plurality of adhesion rods are fixedly connected to the outer wall of the ball body.
Furthermore, the plurality of flow channels are all in an S-shaped bent shape, and openings at the upper end and the lower end of each flow channel are respectively positioned at the upper side and the lower side of the retardation plate.
Furthermore, the adhesion rod comprises a main rod body, the side wall of the main rod body is fixedly connected with an auxiliary rod body, the outer surface of the auxiliary rod body is composed of uniformly distributed capillary tubes, the capillary tubes have an adsorption effect and can adsorb an extracted substance sprayed from the contraction extrusion bag, and the CO2 passing through the blocking ball can be conveniently and fully contacted with the capillary tubes.
Furthermore, the radius of the blocking ball is larger than the inner diameter of the cylindrical passage, the blocking ball blocks the cylindrical passage in a natural state, and the blocking ball is opened when being filled with the extracted substance, is similar to a structure of a one-way valve and plays a role in preventing backflow.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme fills the crushed extracted substances into the contraction extrusion bag in advance to expand the contraction extrusion bag, the contraction extrusion bag is shrunk by utilizing the increase of pressure in the extraction process, the feed channel is sealed by utilizing the blocking ball by utilizing the elastic connecting piece, so that the contraction extrusion bag extrudes the extracted substances out of the magnetic closing sheet to increase the contact area of the extracted substances and CO2 and improve the extraction efficiency, and the flow rate of CO2 is reduced by utilizing the blocking ball with the bent channel, so that the residence time of CO2 is prolonged, the contact time of the extracted substances and CO2 is increased, the extraction efficiency is further improved, compared with the prior art, the contact time and the contact area of the extracted substances and the CO2 are improved, and the extraction efficiency is greatly improved.
(2) The contraction extrusion bag comprises an outer bag and an inner bag, the outer bag and the inner bag have elasticity and can be contracted, elastic fillers are filled between the outer bag and the inner bag, the elastic fillers are made of soft elastic materials, the elastic fillers increase the elasticity of the contraction extrusion bag, the contraction extrusion bag expands when being filled with powdery extracted substances, and when the pressure is applied in the extraction process, the pressure enables the contraction extrusion bag to shrink, so that the extracted substances are sprayed out.
(3) The elastic connecting piece comprises a supporting body, the supporting body is in a vertical state in a free state, two elastic rods are embedded in the supporting body, the supporting body is made of rubber materials, when the extracted matter is filled into the shrinkage squeezing bag, the blocking ball is pushed open, the elastic connecting piece is bent at the moment, and after the filling of the extracted matter is stopped, the elastic force of the elastic rods enables the supporting body to be stretched straight, so that the cylindrical channel is blocked by the blocking ball.
(4) The magnetic sealing sheet comprises a silica gel sheet, magnet blocks are embedded in the free ends of the silica gel sheet, the two opposite magnet blocks are opposite in magnetism, the two magnet blocks are adsorbed together in a free state, the extracted matter can be prevented from directly entering the extractor body in the filling process, and when the shrinkage extrusion bag begins to shrink, the extracted matter pushes the two silica gel sheets open under the extrusion effect, so that the extracted matter is ejected from the place.
(5) The retarding ball comprises a ball body, a plurality of flow channels are formed in the ball body, so that the flow rate of CO2 is reduced, the detention time is prolonged, the ball body is fully contacted with an extracted substance, and a plurality of sticking rods are fixedly connected to the outer wall of the ball body.
(6) The plurality of flow channels are all in S-shaped bent shapes, and openings at the upper end and the lower end of each flow channel are respectively positioned at the upper side and the lower side of the retardation plate.
(7) The adhesion rod comprises a main rod body, the side wall of the main rod body is fixedly connected with an auxiliary rod body, the outer surface of the auxiliary rod body is composed of uniformly distributed capillaries, the capillaries have an adsorption effect and can adsorb an extracted substance sprayed from a contraction extrusion bag, and CO2 passing through the blocking ball can be conveniently and fully contacted with the capillaries.
(8) The radius of the blocking ball is larger than the inner diameter of the cylindrical passage, the blocking ball blocks the cylindrical passage in a natural state, and the blocking ball is opened when being filled with the extracted substance, is similar to a structure of a one-way valve and plays a role in preventing backflow.
Drawings
FIG. 1 is a schematic view of the inflated state of a deflated bladder of the present invention;
FIG. 2 is a schematic view of a deflated bladder of the present invention in a deflated state;
FIG. 3 is a schematic cross-sectional view of the mounting block of the present invention;
FIG. 4 is a schematic cross-sectional view of the elastic connecting member of the present invention;
FIG. 5 is a schematic view of the closed state of the magnetic closure of the present invention;
FIG. 6 is a schematic view of the magnetic closure of the present invention in an open state;
FIG. 7 is a schematic cross-sectional view of a blocker plate according to the present invention;
fig. 8 is a schematic view of the structure at a in fig. 7.
The reference numbers in the figures illustrate:
1 extractor body, 2 feed inlets, 3 discharge outlets, 4 feeding pipes, 5 shrinkage extrusion bags, 501 outer bags, 502 inner bags, 503 elastic fillers, 6 mounting blocks, 601 feeding channels, 602 cylindrical channels, 603 discharge channels, 7 support rods, 8 blocking balls, 9 elastic connectors, 901 supports, 902 elastic rods, 10 magnetic closing sheets, 1001 silica gel sheets, 1002 magnet blocks, 11 blocking plates, 1101 holes, 12 blocking balls, 1201 spheres, 1202 flow channels, 1203 adhesion rods and 1204 capillary tubes.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and 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 a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection 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 explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1-8, a supercritical fluid high-efficiency extraction separation device for pharmacy comprises an extractor body 1, referring to fig. 1-2, the upper end and the lower end of the extractor body 1 are respectively provided with a feed inlet 2 and a discharge outlet 3, the upper part of the extractor body 1 is inserted with a feed pipe 4, the lower end of the feed pipe 4 is communicated with a shrinkage extrusion bag 5, and the extract can be mixed with CO2 to be filled when being filled into the shrinkage extrusion bag 5, so that CO2 can enable the shrinkage extrusion bag 5 to expand and can also be used as a raw material to be supplemented into supercritical CO2, the shrinkage extrusion bag 5 comprises an outer bag 501 and an inner bag 502, the outer bag 501 and the inner bag 502 have elasticity and shrinkage change, an elastic filler 503 is filled between the outer bag 501 and the inner bag 502, the elastic filler 503 is made of a soft elastic material, the elastic filler 503 increases the elasticity of the shrinkage extrusion bag 5, the shrinkage extrusion bag 5 expands when being filled with powdered extract, when the pressure is applied in the extraction process, the pressure makes the shrinkage squeezing bag 5 shrink, so that the extracted matter is sprayed out;
referring to fig. 3-4, an installation block 6 is fixedly connected to an inner wall of an upper end of a feeding pipe 4, a feeding channel 601, a cylindrical channel 602 and a discharging channel 603 are sequentially formed in the installation block 6 from top to bottom, a support rod 7 is fixedly connected to an inner wall of a lower end of the installation block 6, a ball 8 is arranged above the support rod 7, the radius of the ball 8 is larger than the inner diameter of the cylindrical channel 602, the ball 8 blocks the cylindrical channel 602 in a natural state, the ball 8 is opened when being filled with an extracted substance, the ball is similar to a one-way valve structure and plays a role of preventing backflow, an elastic connecting piece 9 is fixedly connected between the ball 8 and the support rod 7, the elastic connecting piece 9 comprises a support body 901, the support body 901 is in a vertical state when in a free state, two elastic rods are embedded in the support body 901, the support body 902 is made of rubber material, when the extracted substance is filled into a shrinkage squeezing bag 5, the blocking ball 8 is pushed open, the elastic connecting piece 9 is bent at the moment, and after the filling of the extracted substance is stopped, the elastic force of the elastic rod 902 enables the support body 901 to be straightened, so that the cylindrical channel 602 is blocked by the blocking ball 8, and the side wall of the feeding pipe 4 positioned below the mounting block 6 is provided with a plurality of openings;
referring to fig. 5-6, the inner wall of each opening is fixedly connected with two symmetrically arranged magnetic closing sheets 10, each magnetic closing sheet 10 comprises a silicon sheet 1001, a magnet block 1002 is embedded in the free end of each silicon sheet 1001, the two opposite magnet blocks 1002 are opposite in magnetism, the two magnet blocks 1002 are mutually adsorbed together in a free state, the extracted matter can be prevented from directly entering the extractor body 1 in the filling process, and when the compression bag 5 is contracted, the extracted matter pushes the two silicon sheets 1001 open under the compression effect, so that the extracted matter is ejected from the extraction device body 1;
referring to fig. 7-8, a plurality of retardation plates 11 are fixedly connected between the outer side wall of the feeding pipe 4 and the inner wall of the extractor body 1, the retardation plates 11 are located at two sides of the opening, each retardation plate 11 is provided with a plurality of holes 1101, a plurality of retardation balls 12 are embedded on the retardation plates 11, each retardation ball 12 comprises a ball 1201, a plurality of flow channels 1202 are formed inside the ball 1201, the plurality of flow channels 1202 are all in an S-shaped curved shape, the openings at the upper end and the lower end of each flow channel 1202 are respectively located at the upper side and the lower side of the retardation plate 11, so as to reduce the flow rate of CO2 and prolong the residence time, the ball 1201 is fully contacted with the extract, the outer wall of the ball 1201 is fixedly connected with a plurality of adhesion rods 1203, the adhesion rod 1203 comprises a main rod, the side wall of the main rod is fixedly connected with an auxiliary rod, the outer surface of the auxiliary rod is composed of uniformly distributed capillaries 1204, the capillaries have an adsorption function, and can suck the extract sprayed from the shrinkage squeeze bag 5, it is convenient to have the CO2 passing through the blocker ball 12 in full contact therewith.
Before the device is used, the extracted substance is ground into powder, then the powder is mixed with CO2 gas and is filled into a feeding pipe 4, the extracted substance and CO2 gas push open a blocking ball 8, so that the extracted substance enters a shrinkage and extrusion bag 5 through a mounting block 6, the shrinkage and extrusion bag 5 is expanded under the pressure, after the filling of the extracted substance is stopped, the elastic force of an elastic rod 902 enables a support body 901 to be straightened, so that the blocking ball 8 blocks a cylindrical channel 602, then an extraction flow is started, the shrinkage and extrusion bag 5 starts to shrink in the process of pressurizing an extractor body 1, the extracted substance and CO2 gas push open two silica gel sheets 1001 under the extrusion action, so that the silica gel sheets are sprayed into the extractor body 1 from the position, the blocking ball 12 reduces the flow rate of CO2 and prolongs the residence time, and the extracted substance is in full contact with the extracted substance, so that the extraction efficiency is improved.
The method comprises the steps of filling crushed extracted substances into a contraction extrusion bag in advance to expand the contraction extrusion bag, reducing the contraction extrusion bag by utilizing the increase of pressure in the extraction process, sealing a feeding channel by utilizing an elastic connecting piece to enable a blocking ball to extrude the extracted substances out of a magnetic sealing sheet, so that the contact area of the extracted substances and CO2 is increased, the extraction efficiency is improved, and the flow rate of CO2 is reduced by utilizing the blocking ball with a bent channel, so that the residence time of CO2 is prolonged, the contact time of the extracted substances and CO2 is increased, the extraction efficiency is further improved, compared with the prior art, the contact time and the contact area of the CO2 and the extracted substances are improved, and the extraction efficiency is greatly improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the equivalent replacement or change according to the technical solution and the modified concept of the present invention should be covered by the scope of the present invention.
Claims (6)
1. The utility model provides a high-efficient extraction and separation device of supercritical fluid for pharmacy, includes extractor body (1), feed inlet (2) and discharge gate (3), its characterized in that have been seted up respectively to the upper and lower both ends of extractor body (1): a feeding pipe (4) is inserted into the upper part of the extractor body (1), the lower end of the feeding pipe (4) is communicated with a shrinkage extrusion bag (5), the inner wall of the upper end of the feeding pipe (4) is fixedly connected with an installation block (6), a feeding channel (601), a cylindrical channel (602) and a discharging channel (603) are sequentially arranged in the installation block (6) from top to bottom, the inner wall of the lower end of the installation block (6) is fixedly connected with a support rod (7), a blocking ball (8) is arranged above the support rod (7), an elastic connecting piece (9) is fixedly connected between the blocking ball (8) and the support rod (7), the side wall of the feeding pipe (4) positioned below the installation block (6) is provided with a plurality of openings, the inner wall of each opening is fixedly connected with two magnetic sealing sheets (10) which are symmetrically arranged, and a plurality of blocking plates (11) are fixedly connected between the outer side wall of the feeding pipe (4) and the inner wall of the extractor body (1), the retarding plates (11) are positioned on two sides of the opening, a plurality of holes (1101) are formed in each retarding plate (11), and a plurality of retarding balls (12) are inlaid in each retarding plate (11);
the magnetic sealing piece (10) comprises a silica gel piece (1001), a magnet block (1002) is embedded in the free end of the silica gel piece (1001), and the two opposite magnet blocks (1002) are opposite in magnetism;
the radius of the blocking ball (8) is larger than the inner diameter of the cylindrical channel (602).
2. The supercritical fluid high-efficiency extraction separation apparatus for pharmaceutical use according to claim 1, wherein: the contraction and extrusion bag (5) comprises an outer bag (501) and an inner bag (502), an elastic filler (503) is filled between the outer bag (501) and the inner bag (502), and the elastic filler (503) is made of a soft elastic material.
3. The supercritical fluid high-efficiency extraction separation apparatus for pharmaceutical use according to claim 1, wherein: the elastic connecting piece (9) comprises a supporting body (901), two elastic rods (902) are embedded in the supporting body (901), and the supporting body (901) is made of rubber materials.
4. The supercritical fluid high-efficiency extraction separation apparatus for pharmaceutical use according to claim 1, wherein: the blocking ball (12) comprises a ball body (1201), a plurality of flow channels (1202) are formed in the ball body (1201), and a plurality of adhesion rods (1203) are fixedly connected to the outer wall of the ball body (1201).
5. The supercritical fluid high-efficiency extraction separation apparatus for pharmaceutical use according to claim 4, wherein: the plurality of flow channels (1202) are S-shaped and bent, and openings at the upper end and the lower end of each flow channel (1202) are respectively positioned at the upper side and the lower side of the retarding plate (11).
6. The supercritical fluid high-efficiency extraction separation apparatus for pharmaceutical use according to claim 4, wherein: the sticking rod (1203) comprises a main rod body, the side wall of the main rod body is fixedly connected with an auxiliary rod body, and the outer surface of the auxiliary rod body is composed of capillary tubes (1204) which are uniformly distributed.
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