Supercritical extraction separation equipment

Abstract

The invention provides supercritical extraction and separation equipment applied to the field of supercritical equipment, through the arrangement of a pressure reduction pipe bundle, when a supercritical fluid is changed into a gas state through temperature rise and pressure reduction, the pressure of gas overflow can be effectively dispersed, on one hand, gas concentrated on one pipeline in the prior art is dispersed into a plurality of pressure expansion pipes, and on the other hand, the pressure of the gas is reduced; on the other hand, under the action of the gas pressure, the multiple pressure expansion pipes gradually expand and abut against one another, the ventilation capacity of the pipeline in unit time can be increased, gas emission is accelerated, the multiple expanded pressure expansion pipes can also conduct mutual extrusion action, and then part of outward pressure of gas is offset; and the pipeline is further protected and is not easy to damage.

Description

Technical Field

[0001] The present application relates to the field of supercritical equipment, and in particular to a supercritical extraction separation equipment. Background Art

[0002] In the supercritical state, supercritical carbon dioxide is brought into contact with the substance to be separated, so that it can selectively extract components of different polarity, boiling point and molecular weight in sequence. Of course, the extract obtained corresponding to each pressure range cannot be single, but the conditions can be controlled to obtain the best proportion of mixed components, and then the supercritical fluid is turned into ordinary gas by means of decompression and heating, and the extracted substance is completely or basically precipitated, thereby achieving the purpose of separation and purification. Therefore, the supercritical fluid carbon dioxide extraction process is a combination of extraction and separation.

[0003] Due to the high efficiency and high purity of supercritical extraction, this method is used for the separation and purification of many substances. However, after supercritical extraction, the process of supercritical carbon dioxide converting from liquid to gas will cause the gas pipeline to be rapidly subjected to huge pressure shock in a short period of time, which will not only easily cause the pipe mouth to loosen and fall off, but also have a great impact on the service life of the pipe itself, and easily affect the stability and efficiency of the entire extraction process. Summary of the invention

[0004] The purpose of the present application is to reduce the pressure on the pipeline when the supercritical fluid is converted into gas, and to protect the pipeline from being damaged. Compared with the prior art, a supercritical extraction and separation device is provided, including an extraction tank, a separation tank and a recovery tank, a fluid pipe is connected between the extraction tank and the separation tank, a gas pipe is connected between the extraction tank and the recovery tank, a pressure reduction component is connected between the separation tank and the recovery tank, the pressure reduction component includes two transfer ball tubes fixedly connected to the ends of the separation tank and the recovery tank respectively, and a pressure reduction tube bundle connected between the two transfer ball tubes, the outer cover of the pressure reduction tube bundle is provided with a protective tube cover, the transfer ball tube includes two hemispherical shells threadedly connected to each other and a connecting pipe connected to the end of one of the hemispherical shells, and the end of the pressure reduction tube bundle is connected to the other hemispherical shell.

[0005] By setting up the pressure-reducing tube bundle, when the supercritical fluid is changed into gaseous state by increasing temperature and reducing pressure, the pressure of gas overflow can be effectively dispersed. On the one hand, the gas concentrated on one pipeline in the prior art is dispersed into multiple compression and expansion tubes, thereby greatly reducing the gas pressure on a single compression and expansion tube. On the other hand, under the action of gas pressure, multiple compression and expansion tubes gradually expand and conflict with each other, thereby increasing the ventilation volume of the pipeline per unit time and accelerating the discharge of gas. The expanded multiple compression and expansion tubes can also squeeze each other, thereby offsetting part of the outward pressure of the gas, further protecting the pipeline so that it is not easily damaged.

[0006] Furthermore, the gas pressure in the extraction tank is 7.39 MPa and the temperature is 31.2-50°C.

[0007] Furthermore, the pressure-reducing tube bundle includes an embedded hemispherical layer matching the inner wall of the hemispherical shell, a plurality of through-hole tubes fixedly connected to the ends of the embedded hemispherical layer, and a plurality of expansion tubes fixedly connected between two opposite through-hole tubes on the two hemispherical shells. A plurality of tube holes are drilled on the hemispherical shell, and the plurality of through-hole tubes respectively penetrate the plurality of tube holes. The through-hole tubes are hard structures, so that the pipelines penetrating the tube holes have high stability and are not easy to expand under the action of gas pressure, thereby effectively protecting the pipelines from generating large interaction forces with the inner walls and edges of the tube holes, so that the pressure-reducing tube bundle is not easy to be damaged. The embedded hemispherical layer and the expansion tube are both elastic sealing structures, and the edge of the embedded hemispherical layer is fixedly connected to the inner wall of the hemispherical shell. The embedded hemispherical layer fits the inner wall of the hemispherical shell as a whole and is hemispherical. At the same time, the edge of the embedded hemispherical layer and the hemispherical shell can be sealed by fixing, so that the contact area at the connection between the mouth of the pressure-reducing tube bundle and the transition ball tube is large, thereby greatly improving the connection stability and reducing the possibility of the end of the pressure-reducing tube bundle and the transition ball tube falling off.

[0008] Furthermore, the protective pipe cover is a symmetrical cylindrical structure with small ends and a large middle, and is made of a hard transparent material. The protective pipe cover can restrain and limit the multiple compression and expansion tubes, making it difficult for the multiple compression and expansion tubes to over-expand, thereby protecting them from damage due to excessive expansion.

[0009] Optionally, a pressure relief pipe is fixedly connected between the two transfer ball tubes. The pressure relief pipe is located in the middle of the multiple expansion tubes, and the two ends of the pressure relief pipe are respectively connected to the two transfer ball tubes. The pressure relief pipe is used for pressure relief. When the pressure is too high, causing the multiple expansion tubes to be squeezed and contacted with the pressure relief pipe, they can be controlled to release part of the gas outward, thereby achieving the effect of pressure relief, thereby effectively protecting the step-down tube bundle, reducing the impact of gas pressure on its service life, and effectively ensuring the stability of the entire extraction and separation process.

[0010] Furthermore, the outer diameters of the multiple expansion tubes are smaller than the outer diameter of the pressure relief tube, and the multiple expansion tubes are not in compression contact with the pressure relief tube, so that the multiple expansion tubes will not contact the pressure relief tube during initial expansion, thereby giving the expansion tubes a certain expansion space, which is convenient for accelerating the exhaust speed.

[0011] Furthermore, the pressure relief pipe includes a fixed pipe, a limiting pipe fixedly connected to the middle of the fixed pipe, and a pressure relief movable pipe sleeved on the outside of one side end of the fixed pipe. The pressure relief movable pipe and the fixed pipe are sealed with each other, and the inner walls of the pressure relief movable pipe and the limiting pipe are fixedly connected with brackets. An electric push rod is installed between the two brackets. The extended end of the electric push rod is connected to the bracket on the pressure relief movable pipe. A plurality of evenly distributed pressure relief holes are drilled at the outer end of the fixed pipe located in the pressure relief movable pipe. When the pressure is too high, the electric push rod extends, so that the pressure relief movable pipe gradually moves away from the limiting pipe, exposing the pressure relief holes. At this time, the gaseous carbon dioxide can be directly discharged to the outside, which can achieve a certain pressure relief effect and effectively alleviate the gas pressure on the step-down tube bundle.

[0012] It is worth noting that the pressure relief holes on the fixed pipe are concentrated on one side close to the limiting pipe, and the length of the fixed pipe in the pressure relief movable pipe without pressure relief holes is not less than half of the overall length of the fixed pipe in the pressure relief movable pipe.

[0013] Furthermore, a plurality of pressure sensors distributed in an array are installed at the outer end of the limit tube, a hemispherical cover is arranged outside the pressure sensor, the hemispherical cover is fixedly connected to the limit tube, a control chip is installed inside the limit tube, the pressure sensor and the electric push rod are both connected to the control chip signal, when the plurality of expansion tubes expand, they will gradually approach the pressure relief tube and be squeezed into contact with the pressure relief tube, at this time, the hemispherical cover is gradually squeezed and deformed by the expansion tube until the force data is displayed on the pressure sensor, when the plurality of pressure sensors are all subjected to force and reach the predetermined threshold value, it indicates that the plurality of expansion tubes have expanded, at this time, after the control chip monitors the signal, it determines that the gas pressure is too high, and controls the electric push rod to extend for pressure relief.

[0014] Furthermore, the hemispherical cover is an elastic hemispherical structure, and a bellows is connected to the middle of the pressure relief movable pipe. The length of the bellows is not less than 1 / 3 of the length of the pressure relief movable pipe, so that the compressible distance of the pressure relief movable pipe is not too long, effectively ensuring that it is not easy to be directly separated from the fixed pipe. At the same time, the compressible distance is not too short, which is convenient for fully exposing multiple pressure relief holes for pressure relief.

[0015] Compared with the prior art, the advantages of this application are:

[0016] By setting up the pressure-reducing tube bundle, when the supercritical fluid is changed into gaseous state by increasing temperature and reducing pressure, the pressure of gas overflow can be effectively dispersed. On the one hand, the gas concentrated on one pipeline in the prior art is dispersed into multiple compression and expansion tubes, thereby greatly reducing the gas pressure on a single compression and expansion tube. On the other hand, under the action of gas pressure, multiple compression and expansion tubes gradually expand and conflict with each other, thereby increasing the ventilation volume of the pipeline per unit time and accelerating the discharge of gas. The expanded multiple compression and expansion tubes can also squeeze each other, thereby offsetting part of the outward pressure of the gas, further protecting the pipeline so that it is not easily damaged. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1It is the main structural diagram of this application;

[0018] Figure 2 This is a schematic diagram of the application for setting a protective pipe cover for the outer cover of the step-down pipe bundle;

[0019] Figure 3 This is a schematic diagram of the front side of the step-down tube bundle of this application;

[0020] Figure 4 This is a front view of the balloon tube of this application;

[0021] Figure 5 A schematic diagram of a cross section of a hemispherical shell of the present application;

[0022] Figure 6 This is a diagram showing the change in the cross section of the reduced-pressure tube bundle under the action of gaseous carbon dioxide in Example 1 of the present application;

[0023] Figure 7 This is a schematic diagram of the cross section of the pressure relief pipe in this application;

[0024] Figure 8 A schematic diagram of the cross section of the limiting pipe for this application;

[0025] Fig. 9 This is a diagram showing the change in the cross-section of the reduced-pressure tube bundle under the action of gaseous carbon dioxide in Example 2 of the present application.

[0026] Description of the numbers in the figure:

[0027] 1 extraction tank, 2 separation tank, 3 recovery tank, 41 fluid tube, 42 gas tube, 5 transfer ball tube, 51 hemispherical shell, 52 connecting tube, 6 pressure reducing tube bundle, 61 embedded hemispherical layer, 62 through-hole tube, 63 expansion tube, 7 protective tube cover, 8 tube hole, 9 pressure relief tube, 91 fixed tube, 92 pressure relief dynamic tube, 93 limit tube, 10 electric push rod, 11 hemispherical cover, 12 pressure sensor, 13 bracket. DETAILED DESCRIPTION

[0028] The embodiments will be combined with the drawings in the specification to clearly and completely describe the technical solution of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without making any creative work shall fall within the scope of protection of the present application.

[0029] The first implementation method:

[0030] The present invention provides a supercritical extraction separation device, please refer to Figure 1 , including an extraction tank 1, a separation tank 2 and a recovery tank 3, a fluid pipe 41 is connected between the extraction tank 1 and the separation tank 2, a gas pipe 42 is connected between the extraction tank 1 and the recovery tank 3, a pressure reducing component is connected between the separation tank 2 and the recovery tank 3, the gas pressure in the extraction tank 1 is 7.39MPa, and the temperature is 31.2-50℃.

[0031] See also Figure 2-3 The decompression assembly includes two transfer spherical tubes 5 respectively fixedly connected to the ends of the separation tank 2 and the recovery tank 3, and a decompression tube bundle 6 connected between the two transfer spherical tubes 5. The outer cover of the decompression tube bundle 6 is provided with a protective tube cover 7. Please refer to Figure 4 The transfer ball tube 5 includes two hemispherical shells 51 threadedly connected to each other and a connecting tube 52 connected to the end of one of the hemispherical shells 51 , and the end of the step-down tube bundle 6 is connected to the other hemispherical shell 51 .

[0032] See also Figure 3 and Figure 5 The pressure-reducing tube bundle 6 includes an embedded hemispherical layer 61 matched with the inner wall of the hemispherical shell 51, a plurality of through-hole tubes 62 fixedly connected to the end of the embedded hemispherical layer 61, and a plurality of expansion tubes 63 fixedly connected between two opposite through-hole tubes 62 on the two hemispherical shells 51. A plurality of tube holes 8 are drilled on the hemispherical shell 51, and a plurality of through-hole tubes 62 respectively penetrate the plurality of tube holes 8. The through-hole tubes 62 are hard structures, so that the pipeline passing through the tube hole 8 has high stability and is not easy to expand under the action of gas pressure, thereby effectively protecting the pipeline from being easily tangled with the inner wall and edge of the tube hole 8. A larger interaction force is generated, so that the step-down tube bundle 6 is not easily damaged. The embedded hemispherical layer 61 and the pressure expansion tube 63 are both elastic sealing structures, and the edge of the embedded hemispherical layer 61 is fixedly connected to the inner wall of the hemispherical shell 51. The embedded hemispherical layer 61 fits the inner wall of the hemispherical shell 51 as a whole and is hemispherical. At the same time, the edge of the embedded hemispherical layer 61 and the hemispherical shell 51 can be sealed by fixing, so that the contact area of ​​the connection between the mouth of the step-down tube bundle 6 and the transfer ball tube 5 is larger, thereby greatly improving the connection stability and reducing the possibility of the end of the step-down tube bundle 6 and the transfer ball tube 5 falling off.

[0033] The protective tube cover 7 is a symmetrical cylindrical structure with small ends and a large middle, and is made of a hard transparent material. The protective tube cover 7 can restrain and limit the multiple compression tubes 63, making it difficult for the multiple compression tubes 63 to over-expand, thereby protecting them from damage due to excessive expansion.

[0034] By setting up the pressure-reducing tube bundle, when the supercritical fluid is changed into gas by increasing temperature and reducing pressure, the pressure of gas overflow can be effectively dispersed. On the one hand, the gas concentrated on one pipeline in the prior art is dispersed into multiple expansion tubes 63, thereby greatly reducing the gas pressure on a single expansion tube 63. On the other hand, under the action of gas pressure, multiple expansion tubes 63 gradually expand and conflict with each other, thereby increasing the ventilation volume of the pipeline per unit time and accelerating the discharge of gas. The expanded multiple expansion tubes 63 can also squeeze each other, thereby offsetting part of the outward pressure of the gas, further protecting the pipeline and making it less likely to be damaged.

[0035] The second implementation method:

[0036] Please refer to Fig. 9 A pressure relief pipe 9 is also fixedly connected between the two transfer ball tubes 5. The pressure relief pipe 9 is located in the middle of the multiple expansion tubes 63, and the two ends of the pressure relief pipe 9 are respectively connected to the two transfer ball tubes 5. The pressure relief pipe 9 is used for pressure relief. When the pressure is too large, causing the multiple expansion tubes 63 to be squeezed and contacted with the pressure relief pipe 9, they can be controlled to release part of the gas outward, thereby achieving the effect of pressure relief, thereby effectively protecting the pressure reduction tube bundle 6, reducing the impact of the gas pressure on its service life, and effectively ensuring the stability of the entire extraction and separation process.

[0037] The outer diameters of the multiple expansion tubes 63 are smaller than the outer diameter of the pressure relief tube 9, and the multiple expansion tubes 63 are not in compression contact with the pressure relief tube 9, so that the multiple expansion tubes 63 will not contact with the pressure relief tube 9 during the initial expansion, and the expansion tubes 63 have a certain expansion space, which is convenient for accelerating the exhaust speed.

[0038] See also Figure 7 The pressure relief pipe 9 includes a fixed pipe 91, a limit pipe 93 fixedly connected to the middle of the fixed pipe 91, and a pressure relief movable pipe 92 sleeved on the outside of one side end of the fixed pipe 91. The pressure relief movable pipe 92 and the fixed pipe 91 are sealed with each other. The inner walls of the pressure relief movable pipe 92 and the limit pipe 93 are fixedly connected with a bracket 13. An electric push rod 10 is installed between the two brackets 13. The extended end of the electric push rod 10 is connected to the bracket 13 on the pressure relief movable pipe 92. A plurality of evenly distributed pressure relief holes are drilled at the outer end of the fixed pipe 91 located in the pressure relief movable pipe 92. When the pressure is too large, the electric push rod 10 extends, so that the pressure relief movable pipe 92 gradually moves away from the limit pipe 93, so that the pressure relief holes are exposed. At this time, the gaseous carbon dioxide can be directly discharged to the outside, which can achieve a certain pressure relief effect and effectively relieve the gas pressure on the step-down tube bundle 6.

[0039] It is worth noting that the pressure relief holes on the fixed pipe 91 are concentrated on one side close to the limiting pipe 93, and the length of the fixed pipe 91 inside the pressure relief movable pipe 92 without pressure relief holes is not less than half of the overall length of the fixed pipe 91 inside the pressure relief movable pipe 92.

[0040] See also Figure 8A plurality of pressure sensors 12 distributed in an array are installed at the outer end of the limit tube 93. A hemispherical cover 11 is arranged outside the pressure sensor 12. The hemispherical cover 11 is fixedly connected to the limit tube 93. A control chip is installed inside the limit tube 93. The pressure sensor 12 and the electric push rod 10 are both connected to the control chip signal. When the plurality of expansion tubes 63 expand, they will gradually approach the pressure relief tube 9 and be squeezed and contacted with the pressure relief tube 9. At this time, the hemispherical cover 11 is gradually squeezed and deformed by the expansion tube 63 until the force data is displayed on the pressure sensor 12. When the plurality of pressure sensors 12 are all subjected to force and reach a predetermined threshold, it indicates that the plurality of expansion tubes 63 have expanded. At this time, after the control chip monitors the signal, it determines that the gas pressure is too high, and controls the electric push rod 10 to extend for pressure relief. During pressure relief, when the pressure values ​​on the plurality of pressure sensors 12 are lower than the threshold, the control chip controls the electric push rod 10 to reset, thereby stopping the pressure relief.

[0041] It is worth noting that the setting of the threshold value on the pressure sensor 12 is determined by the actual deformation force and pressure resistance of the expansion tube 63. During specific implementation, those skilled in the art may conduct multiple experiments to determine the threshold value.

[0042] The hemispherical cover 11 is an elastic hemispherical structure, and a bellows is connected to the middle of the pressure relief movable pipe 92. The length of the bellows is not less than 1 / 3 of the length of the pressure relief movable pipe 92, so that the compressible distance of the pressure relief movable pipe 92 is not too long, which effectively ensures that it is not easy to be directly separated from the fixed pipe 91. At the same time, the compressible distance is not too short, which is convenient for fully exposing multiple pressure relief holes for pressure relief.

[0043] On the basis of Example 1, this embodiment adds a pressure relief pipe 9 and its related structures, so that this solution can not only reduce the gas pressure on the single expansion tube 63 in Example 1, but also monitor the gas pressure in real time. When the pressure is too high, it can achieve automatic pressure relief, effectively ensure the stability of the entire extraction process, and reduce the hidden dangers caused by excessive pressure.

[0044] The above is only the best implementation method adopted by this application in combination with current actual needs, but the protection scope of this application is not limited to this.

Claims

1. A supercritical extraction separation device, comprising an extraction tank (1), a separation tank (2) and a recovery tank (3), wherein a fluid pipe (41) is connected between the extraction tank (1) and the separation tank (2), and a gas pipe (42) is connected between the extraction tank (1) and the recovery tank (3), characterized in that: A pressure reducing assembly is connected between the separation tank (2) and the recovery tank (3), the pressure reducing assembly comprising two transfer spherical tubes (5) respectively fixedly connected to the ends of the separation tank (2) and the recovery tank (3), and a pressure reducing tube bundle (6) connected between the two transfer spherical tubes (5), the outer cover of the pressure reducing tube bundle (6) is provided with a protective tube cover (7), the transfer spherical tube (5) comprises two hemispherical shells (51) threadedly connected to each other and a connecting tube (52) connected to the end of one of the hemispherical shells (51), the pressure reducing tube bundle (6) The end portion is connected to another hemispherical shell (51), the pressure-reducing tube bundle (6) comprises an embedded hemispherical layer (61) matched with the inner wall of the hemispherical shell (51), a plurality of through-hole tubes (62) fixedly connected to the end portion of the embedded hemispherical layer (61), and a plurality of expansion tubes (63) respectively fixedly connected between two opposite through-hole tubes (62) on the two hemispherical shells (51), a plurality of tube holes (8) are drilled on the hemispherical shell (51), and the plurality of through-hole tubes (62) respectively penetrate the plurality of tube holes (8).

2. A supercritical extraction separation device according to claim 1, characterized in that: The gas pressure in the extraction tank (1) is 7.39 MPa and the temperature is 31.2-50°C.

3. A supercritical extraction separation device according to claim 2, characterized in that: The through-hole tube (62) is a hard structure, the embedded hemispherical layer (61) and the expansion tube (63) are both elastic sealing structures, and the edge of the embedded hemispherical layer (61) is fixedly connected to the inner wall of the hemispherical shell (51).

4. The supercritical extraction separation equipment according to claim 1, characterized in that: The protective tube cover (7) is a symmetrical cylindrical structure with small ends and a large middle, and the protective tube cover (7) is made of a hard transparent material.

5. The supercritical extraction separation equipment according to claim 1, characterized in that: A pressure relief pipe (9) is fixedly connected between the two transfer ball tubes (5). The pressure relief pipe (9) is located in the middle of the plurality of expansion tubes (63), and both ends of the pressure relief pipe (9) are respectively connected to the two transfer ball tubes (5). The outer diameters of the plurality of expansion tubes (63) are smaller than the outer diameter of the pressure relief pipe (9), and the plurality of expansion tubes (63) are not in compression contact with the pressure relief pipe (9).

6. A supercritical extraction separation device according to claim 5, characterized in that: The pressure relief pipe (9) comprises a fixed pipe (91), a limit pipe (93) fixedly connected to the middle of the fixed pipe (91), and a pressure relief movable pipe (92) sleeved outside one side end of the fixed pipe (91); the pressure relief movable pipe (92) and the fixed pipe (91) are sealed with each other; the inner walls of the pressure relief movable pipe (92) and the limit pipe (93) are fixedly connected with a bracket (13); an electric push rod (10) is installed between the two brackets (13); the extended end of the electric push rod (10) is connected to the bracket (13) on the pressure relief movable pipe (92); and a plurality of evenly distributed pressure relief holes are drilled at the outer end of the fixed pipe (91) located inside the pressure relief movable pipe (92).

7. A supercritical extraction separation device according to claim 6, characterized in that: A plurality of pressure sensors (12) distributed in an array are installed at the outer end of the position limiting tube (93); a hemispherical cover (11) is provided outside the pressure sensor (12); the hemispherical cover (11) is fixedly connected to the position limiting tube (93); a control chip is installed inside the position limiting tube (93); and the pressure sensor (12) and the electric push rod (10) are both connected to the control chip signal.

8. The supercritical extraction separation equipment according to claim 7, characterized in that: The hemispherical cover (11) is an elastic hemispherical structure, and a bellows is connected to the middle of the pressure relief movable pipe (92), and the length of the bellows is not less than 1 / 3 of the length of the pressure relief movable pipe (92).

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