A supercritical extraction device and method for ultrafine powder

Abstract

The present invention discloses a supercritical extraction device and method for ultrafine powder, which relates to the field of extraction technology, including: an extraction tank; a supply assembly for supplying supercritical carbon dioxide and conveying it to the extraction tank through a first tube body; a second tube body, one end of which is connected to the extraction tank, and the other end of which is sequentially connected in series with a first separation bin, a fourth tube body, a second separation bin, a sixth tube body, and a collection tank; the extraction tank includes: a tank body, the bottom of which has a waste pipe; a suction plate, which is arranged in the tank body and close to the feed end of the second tube body; a bypass pipe, one end of which is connected to the suction plate, and the other end is connected to the feed end of a pump body, and the discharge end of the pump body is connected to the bottom of the tank body. By timely pumping away the raised material particles, the extraction process is ensured to proceed smoothly.

Description

Technical Field

[0001] The invention relates to the technical field of extraction, in particular to a supercritical extraction device and method for ultrafine powder. Background Art

[0002] Supercritical extraction is currently a common physical extraction process and an advanced separation technology. Its core lies in using the characteristics of supercritical fluid to separate substances. However, the existing supercritical extraction technology requires that the particle size of the material be less than 100 mesh, otherwise the material will become compacted during the extraction, and the carbon dioxide fluid will carry the material out of the material basket and into the carbon dioxide pipeline, causing blockage in the carbon dioxide pipeline. In addition, the current equipment only separates the material in the material basket once in the state of carbon dioxide fluid, and the production efficiency is relatively low. Therefore, there is a need for a device that changes the route of the carbon dioxide fluid to increase production efficiency and prevents the carbon dioxide fluid from carrying out materials.

[0003] Therefore, it is necessary to provide a supercritical extraction device and method for ultrafine powder to solve the above problems. Summary of the invention

[0004] In order to solve the above problems, the present invention provides the following technical solution: a supercritical extraction device for ultrafine powder, comprising:

[0005] An extraction tank, in which the powder material to be extracted is preset;

[0006] A supply component, used for supplying supercritical carbon dioxide and transporting it to the extraction tank through the first tube;

[0007] A bulk material component, used for carrying out bulk material anti-caking treatment on the powder material body in the extraction tank;

[0008] A second tube body, one end of which is connected to the extraction tank, and the other end of which is connected in series with the first separation chamber, the fourth tube body, the second separation chamber, the sixth tube body, and the collection tank;

[0009] Wherein, the first separation chamber is further connected to the gas collecting tank by a third tube body, and the gas collecting tank is further connected to the second separation chamber by a fifth tube body;

[0010] A visual sensor is disposed in the extraction tank and close to a feed end of the second tube;

[0011] Wherein, the extraction tank comprises:

[0012] A tank body having a waste discharge pipe at the bottom and a feed inlet at the top;

[0013] A suction plate, which is arranged in the tank body and close to the feeding end of the second tube body;

[0014] A bypass pipe has one end connected to the suction plate and the other end connected to the feed end of the pump body, and the discharge end of the pump body is connected to the bottom of the tank body.

[0015] Furthermore, preferably, the extraction tank is also provided with a plurality of flow equalizing disks spaced apart along the axial direction of the extraction tank.

[0016] Further, preferably, the suction plate has a chamber for communicating with the bypass pipe, a plurality of through pipes penetrate through the middle of the chamber, and side holes communicating with the chamber are formed on the sides of the through pipes.

[0017] Further, preferably, the bulk material assembly comprises:

[0018] A rotating shaft, which is rotatably disposed in the extraction tank and driven by an external motor;

[0019] A plurality of attachment rods spaced apart along the axial direction of the rotating shaft and fixed on the rotating shaft;

[0020] A mesh plate is fixed on the attachment rod.

[0021] Furthermore, preferably, a plurality of bulk material tube groups are fixed on the attachment rod, and the bulk material tube groups include a straight tube and curved tubes fixed at both ends of the straight tube, wherein when the bulk material tube group rotates with the rotating shaft, the position of the powder material body located above the straight tube and the powder material body located below the straight tube can be adjusted through the two curved tubes.

[0022] Further, preferably, the straight tube comprises a tube body, both ends of which are fixed with flow guide tubes, an inner tube is connected between the two flow guide tubes, and an opening of the flow guide tube at one end close to the inner tube is smaller than an opening at the other end.

[0023] Further, preferably, a micro-actuator is provided between the inner tube and the tube body.

[0024] Further, as a preference, the inner tube is also provided with a plurality of bulk material nets spaced apart along the axial direction of the inner tube, and a draw rope is connected between two adjacent bulk material nets, and the draw rope is elastic.

[0025] A supercritical extraction method for ultrafine powders comprises the following steps:

[0026] S1. Ultrafinely grind the material to be extracted to ensure that the fineness reaches 100 mesh-2000 mesh;

[0027] S2. The supercritical carbon dioxide is delivered to the extraction tank through the supply assembly;

[0028] S3. Start the bulk material assembly and perform bulk anti-caking treatment on the powder material in the extraction tank to ensure that the powder material is evenly dispersed;

[0029] S4. Adjust the pressure in the extraction tank to 25Mpa-30Mpa, control the temperature at 30℃-70℃, selectively add 95% ethanol as an entrainer, the ratio of entrainer to powder material is 1.5:1, and set the extraction time to 1 hour-5 hours;

[0030] S5. Use a visual sensor to monitor the state of the powder material in the extraction tank. When it is detected that the particles are lifted, start the pump to suck to prevent the carbon dioxide fluid from carrying out the material from the second tube;

[0031] S6. After the extraction is completed, the fluid containing the extract is sequentially sent to the first separation chamber and the second separation chamber through the second tube body for separation, wherein the separation temperature of the first separation chamber is 50°C and the separation temperature of the second separation chamber is 30°C;

[0032] S7. The extract enters the collection tank through the sixth tube body for collection.

[0033] Compared with the prior art, the present invention provides a supercritical extraction device and method for ultrafine powder, which has the following beneficial effects:

[0034] The supercritical fluid extraction technology of the present invention utilizes that the fluid in the supercritical state has a strong penetrating power similar to that of gas and a large density and solubility similar to that of liquid, which enables it to more effectively penetrate into the interior of the powder body, thereby quickly and efficiently extracting the effective ingredients.

[0035] The present invention ensures the smooth progress of the extraction process by timely extracting the lifted material particles, thereby improving the extraction efficiency, and can also prevent the material particles from being carried out of the extraction tank by the fluid, avoiding impurities from mixing into the extract, and ensuring the purity and quality of the extract.

[0036] The present invention changes the moving route of the supercritical carbon dioxide fluid by arranging components such as a bulk material assembly, a flow equalizing plate, and a suction plate, thereby achieving deep utilization of the supercritical carbon dioxide and deep extraction of the powder material body. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 It is a schematic diagram of the main structure of a supercritical extraction device for ultrafine powder;

[0038] Figure 2 It is a schematic diagram of the three-dimensional structure of a supercritical extraction device for ultrafine powders;

[0039] Figure 3 for Figure 1 Schematic diagram of the half-section structure;

[0040] Figure 4 for Figure 3 A schematic diagram of the enlarged structure at point A;

[0041] Figure 5 It is a schematic diagram of the structure of a straight tube in a supercritical extraction device for ultrafine powders;

[0042] In the figure: 1, supply assembly; 2, first tube body; 3, extraction tank; 4, bulk material assembly; 5, second tube body; 6, first separation chamber; 7, third tube body; 8, fourth tube body; 9, second separation chamber; 10, fifth tube body; 11, gas collecting tank; 12, sixth tube body; 13, collecting tank; 101, gas storage tank; 102, heater; 103, pressurizer; 104, reflux pipe; 31, tank body; 32, waste pipe; 33, bypass pipe; 34, suction plate; 35, flow equalizing plate; 341, chamber; 342, through pipe; 343, side hole; 41, mesh plate; 42, attachment rod; 43, bent pipe; 44, straight pipe; 441, tube body; 442, inner tube; 443, micro mover; 444, guide tube; 445, bulk material net; 446, pull rope. DETAILED DESCRIPTION

[0043] The terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned description of the drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequential order. It should be understood that the terms used in this way can be interchangeable under appropriate circumstances, which is merely a way of distinguishing the objects of the same attributes when describing them in the embodiments of the present application. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, so that the process, method, system, product or equipment comprising a series of units need not be limited to those units, but may include other units that are not clearly listed or inherent to these processes, methods, products or equipment.

[0044] Please refer to Figure 1-Figure 5 In an embodiment of the present invention, a supercritical extraction device for ultrafine powder is provided, comprising:

[0045] An extraction tank 3, in which the powder material to be extracted is preset;

[0046] The supply assembly 1 is used to supply supercritical carbon dioxide and transport it to the extraction tank 3 through the first tube body 2; the supply assembly 1 includes a gas storage tank 101, a heater 102, and a pressurizer 103 connected in series, the output end of the pressurizer 103 is connected to the first tube body 2, and a reflux pipe 104 is also provided between the first tube body 2 and the heater 102, which will not be repeated here;

[0047] The bulk material component 4 is used for carrying out bulk material anti-caking treatment on the powder material body in the extraction tank 3;

[0048] A second tube body 5, one end of which is connected to the extraction tank 3, and the other end of which is connected in series with the first separation chamber 6, the fourth tube body 8, the second separation chamber 9, the sixth tube body 12, and the collection tank 13;

[0049] The first separation chamber 6 is further connected to the gas collecting tank 11 by a third tube body 7, and the gas collecting tank 11 is further connected to the second separation chamber 9 by a fifth tube body 10;

[0050] A visual sensor, which is disposed in the extraction tank 3 and close to the feeding end of the second tube 5;

[0051] Wherein, the extraction tank 3 comprises:

[0052] The tank body 31 has a waste discharge pipe 32 at the bottom and a feed inlet at the top;

[0053] A suction plate 34, which is disposed in the tank body 31 and close to the feeding end of the second tube body 5;

[0054] The bypass pipe 33 has one end connected to the suction plate 34 and the other end connected to the feed end of the pump body. The discharge end of the pump body is connected to the bottom of the tank body 31 .

[0055] The implementation includes the following steps:

[0056] S1. Ultrafinely grind the material to be extracted to ensure that the fineness reaches 100 mesh-2000 mesh;

[0057] S2. The supercritical carbon dioxide is delivered to the extraction tank 3 through the supply assembly 1;

[0058] S3. Start the bulk material assembly 4, and perform bulk anti-caking treatment on the powder material in the extraction tank 3 to ensure that the powder material is evenly dispersed;

[0059] S4. Adjust the pressure in the extraction tank 3 to 25Mpa-30Mpa, control the temperature at 30℃-70℃ (the extraction tank 3 has its own temperature and pressure adjustment function), selectively add 95% ethanol as an entrainer, the ratio of entrainer to powder material is 1.5:1, and set the extraction time to 1 hour-5 hours;

[0060] S5. Using a visual sensor to monitor the state of the powder material in the extraction tank 3, when the particles are detected to be raised, the pump is started to suck to prevent the carbon dioxide fluid from the second tube 5 to bring out the material;

[0061] S6. After the extraction is completed, the fluid containing the extract is sequentially sent to the first separation chamber 6 and the second separation chamber 9 through the second tube body 5 for separation, wherein the separation temperature of the first separation chamber 6 is 50°C and the separation temperature of the second separation chamber 9 is 30°C;

[0062] S7. The extract enters the collection tank 13 through the sixth tube 12 for collection.

[0063] The bulk material component 4 is used to prevent the powder from agglomerating, ensuring that the powder is evenly dispersed during the extraction process, avoiding agglomeration, thereby improving the extraction efficiency and uniformity. The application of the visual sensor enables real-time monitoring of the state of the powder in the extraction tank 3. Once particles are found to be lifted, the pump is immediately started for suction, effectively preventing the powder from being carried out by the carbon dioxide fluid, thereby ensuring the stability of the extraction process and the recovery rate of the product.

[0064] In addition, in this embodiment, the first separation chamber 6 and the second separation chamber 9 are used for multi-stage separation, and the temperature of each separation chamber (the first separation chamber 6 and the second separation chamber 9) is adjustable, which helps to more thoroughly separate the extract and the solvent (carbon dioxide), thereby improving the purity and recovery rate of the product. At the same time, multi-stage separation also reduces the complexity and cost of subsequent processing.

[0065] Furthermore, the extraction tank 3 is also provided with a plurality of flow equalizing disks 35 spaced apart along the axial direction of the extraction tank 3 .

[0066] The suction plate 34 has a chamber 341 for communicating with the bypass pipe 33 . A plurality of through pipes 342 penetrate through the middle of the chamber 341 . Side holes 343 communicating with the chamber 341 are formed on the sides of the through pipes 342 .

[0067] In this embodiment, the chamber 341 is the core part of the suction plate 34 and is connected to the bypass pipe 33. When the visual sensor detects that particles in the extraction tank 3 are lifted up, the pump body connected to the chamber 341 is started to pump out the fluid in the upper part of the chamber 341 through the bypass pipe 33. In this way, the material particles can be effectively prevented from being taken out of the extraction tank by the supercritical fluid, thereby ensuring the stability of the extraction process and the purity of the extract.

[0068] More specifically, the through pipe 342 penetrates the middle of the chamber 341, so that the fluid in the extraction tank 3 can evenly and effectively pass through the through pipe 342 into the second tube body 5. At the same time, since the side hole 343 is located on the side of the through pipe 342, it is convenient for the fluid to enter the chamber 341 from the side hole 343 under the suction of the pump body, and then enter the bypass pipe 33.

[0069] In this embodiment, the bulk material assembly 4 includes:

[0070] A rotating shaft, which is rotatably disposed in the extraction tank 3 and driven by an external motor;

[0071] A plurality of attachment rods 42 spaced apart along the axial direction of the rotating shaft and fixed to the rotating shaft;

[0072] The mesh plate 41 is fixed on the attachment rod 42 .

[0073] In addition, a plurality of bulk material tube groups are fixed on the attachment rod 42, and the bulk material tube groups include a straight tube 44 and curved tubes 43 fixed at both ends of the straight tube 44, wherein when the bulk material tube group rotates with the rotating shaft, the positions of the powder material bodies located above the straight tube 44 and the powder material bodies located below the straight tube 44 can be adjusted through the two curved tubes 43.

[0074] The active rotation of the bulk material assembly is achieved by the rotating shaft driven by an external motor. Compared with passive or static dispersion, this active dispersion method can more effectively promote the movement and distribution of the powder material in the extraction tank 3, reducing the problems of local accumulation and uneven concentration.

[0075] The attachment rods 42 are spaced apart along the axial direction of the rotating shaft and fixed with a mesh disk 41 . This structure increases the contact area with the powder material body and helps to disperse the powder into the entire extraction tank 3 more quickly.

[0076] During implementation, during the rotation of the bulk material assembly 4 (rotation speed is 10-20 rpm), the powder material can be more evenly distributed in the extraction tank through the screening effect of the mesh disk 41 and the stirring effect of the bulk material tube group. This is very important for improving extraction efficiency and ensuring product quality.

[0077] Among them, the setting of the bend pipe 43 makes the powder material mixed more fully in the vertical direction and reduces the occurrence of stratification. Specifically, when the shaft drives the attachment rod 42 and the mesh disk 41 to rotate, the existence of the bend pipe 43 helps to "capture" the powder material. The "capture" here can be understood as the specific shape and position of the bend pipe 43 during the rotation process, which enables them to intercept and guide the flow of the powder material. Specifically, the design of the bend pipe 43 enables it to change the movement trajectory of the powder material, guiding them from the top or bottom of the straight pipe 44 to different positions, thereby achieving more uniform mixing and dispersion.

[0078] In order to further prevent the powder material from forming nodules, the straight tube 44 includes a tube body 441, and flow guide tubes 444 are fixed at both ends of the tube body. An inner tube 442 is connected between the two flow guide tubes 444, and the opening of the flow guide tube 444 at one end close to the inner tube 442 is smaller than the opening at the other end.

[0079] In addition, a micro-actuator 443 is disposed between the inner tube 442 and the tube body 441 .

[0080] The inner tube 442 is further provided with a plurality of bulk material nets 445 spaced apart along the axial direction of the inner tube 442 , and a pull rope 446 is connected between two adjacent bulk material nets 445 , and the pull rope 446 is elastic.

[0081] The guide tube 444 is fixed at both ends of the inner part of the straight tube 44, and the opening of the guide tube 444 at one end close to the inner tube 442 is smaller than the opening at the other end, which helps to generate a certain pressure difference and flow rate change when the powder body passes through the straight tube 44. It helps to push the powder body to the central area of ​​the straight tube 44 and reduce accumulation near the tube wall.

[0082] The micro mover 443 enables the inner tube 442 to generate a small vibration or displacement. This vibration helps to break the static friction between the powder bodies. The micro mover 443 can adjust the vibration frequency and amplitude as needed to adapt to the characteristics and process requirements of different powder bodies.

[0083] In addition, the bulk material net 445 not only increases the contact area between the powder material body and the inner wall of the inner tube 442, but also helps to disperse the powder material body. When the powder material body passes through the bulk material net 445, it will be subject to a certain resistance and dispersion effect, thereby reducing the formation of nodules. The elastic design of the pull rope 446 allows the bulk material nets 445 to maintain a certain distance between each other, and has a certain buffering effect when subjected to external force, which helps to prevent the bulk material net 445 from being damaged by the impact of the powder material body.

[0084] Based on this, this embodiment also provides a supercritical extraction method for ultrafine powder, comprising the following steps:

[0085] S1. Ultrafinely grind the material to be extracted to ensure that the fineness reaches 100 mesh-2000 mesh;

[0086] S2. The supercritical carbon dioxide is delivered to the extraction tank 3 through the supply assembly 1;

[0087] S3. Start the bulk material assembly 4, and perform bulk anti-caking treatment on the powder material in the extraction tank 3 to ensure that the powder material is evenly dispersed, thereby improving the extraction efficiency and uniformity;

[0088] S4. Adjust the pressure in the extraction tank 3 to 25Mpa-30Mpa, control the temperature at 30 ℃-70 ℃, selectively add 95% ethanol as an entrainer, the entrainer to powder material ratio is 1.5:1, set the extraction time to 1 hour -5 hours;

[0089] S5. The state of the powder material in the extraction tank 3 is monitored by a visual sensor. When the particles are detected to be lifted, the pump is started to suck to prevent the carbon dioxide fluid from being taken out of the second tube 5, thereby ensuring the stability of the extraction process and the recovery rate of the product;

[0090] S6. After the extraction is completed, the fluid containing the extract is sequentially sent to the first separation chamber 6 and the second separation chamber 9 through the second tube body 5 for separation, wherein the separation temperature of the first separation chamber 6 is 50°C and the separation temperature of the second separation chamber 9 is 30°C;

[0091] S7. The extract enters the collection tank 13 through the sixth tube 12 for collection.

[0092] What is described above is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A supercritical extraction device for ultrafine powders, characterized in that: include: An extraction tank (3) having a powder material to be extracted pre-placed therein; A supply component (1) is used to supply supercritical carbon dioxide and transport it to the extraction tank (3) through the first tube (2); A bulk material component (4) is used to perform bulk material anti-caking treatment on the powder material body in the extraction tank (3); A second tube body (5), one end of which is in communication with the extraction tank (3), and the other end of which is sequentially connected in series with the first separation chamber (6), the fourth tube body (8), the second separation chamber (9), the sixth tube body (12), and the collection tank (13); The first separation chamber (6) is further connected to the gas collecting tank (11) by means of a third tube (7), and the gas collecting tank (11) is further connected to the second separation chamber (9) by means of a fifth tube (10); A visual sensor is arranged in the extraction tank (3) and close to the feed end of the second tube body (5); wherein the extraction tank (3) comprises: a tank body (31) having a waste discharge pipe (32) at the bottom and a feed inlet at the top; a suction plate (34) disposed in the tank body (31) and close to the feed end of the second tube body (5); a bypass pipe (33) having one end connected to the suction plate (34) and the other end connected to the feed end of the pump body, and a discharge end of the pump body connected to the bottom of the tank body (31); The bulk material assembly (4) comprises: A rotating shaft, which is rotatably disposed in the extraction tank (3) and driven by an external motor; A plurality of attachment rods (42) spaced apart along the axial direction of the rotating shaft and fixed on the rotating shaft; A mesh plate (41) fixed to the attachment rod (42); A plurality of bulk material tube groups are fixed on the attachment rod (42), the bulk material tube groups comprising a straight tube (44) and bent tubes (43) fixed at both ends of the straight tube (44), wherein when the bulk material tube group rotates with the rotating shaft, the positions of the powder material bodies located above the straight tube (44) and the powder material bodies located below the straight tube (44) can be adjusted through the two bent tubes (43); The straight tube (44) comprises a tube body (441), both ends of which are fixed with flow guide tubes (444), an inner tube (442) is connected between the two flow guide tubes (444), and an opening of one end of the flow guide tube (444) close to the inner tube (442) is smaller than an opening at the other end.

2. A supercritical extraction device for ultrafine powder according to claim 1, characterized in that: The extraction tank (3) is also provided with a plurality of flow equalizing disks (35) distributed at intervals along the axial direction of the extraction tank (3).

3. The supercritical extraction device for ultrafine powder according to claim 1, characterized in that: The suction plate (34) has a chamber (341) for communicating with the bypass pipe (33); a plurality of through pipes (342) penetrate through the middle of the chamber (341); and side holes (343) communicating with the chamber (341) are provided on the sides of the through pipes (342).

4. The supercritical extraction device for ultrafine powder according to claim 1, characterized in that: A micro-actuator (443) is provided between the inner tube (442) and the tube body (441).

5. The supercritical extraction device for ultrafine powder according to claim 1, characterized in that: The inner tube (442) is further provided with a plurality of bulk material nets (445) spaced apart along the axial direction of the inner tube (442), and a drawstring (446) is connected between two adjacent bulk material nets (445), and the drawstring (446) is elastic.

6. A supercritical extraction method for ultrafine powders, characterized in that: The extraction is performed using a supercritical extraction device for ultrafine powders as described in any one of claims 1 to 5, and comprises the following steps: S1. Ultrafinely grind the material to be extracted to ensure that the fineness reaches 100 mesh-2000 mesh; S2. The supercritical carbon dioxide is delivered to the extraction tank (3) through the supply assembly (1); S3. Start the bulk material assembly (4) and perform bulk anti-caking treatment on the powder material in the extraction tank (3) to ensure that the powder material is evenly dispersed; S4. Adjust the pressure in the extraction tank (3) to 25Mpa-30Mpa, control the temperature at 30°C-70°C, selectively add 95% ethanol as an entrainer, the ratio of entrainer to powder material is 1.5:1, and set the extraction time to 1 hour-5 hours; S5. Using a visual sensor to monitor the state of the powder material in the extraction tank (3), when the particles are detected to be lifted, the pump is started to suck to prevent the carbon dioxide fluid from the second tube (5) from carrying out the material; S6. After the extraction is completed, the fluid containing the extract is sequentially sent to the first separation chamber (6) and the second separation chamber (9) through the second tube body (5) for separation, wherein the separation temperature of the first separation chamber (6) is 50° C., and the separation temperature of the second separation chamber (9) is 30° C.; S7. The extract enters the collection tank (13) through the sixth tube (12) for collection.

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