A resin adsorption experimental device
By adopting a combined structure of extrusion column and pressure plate in the resin adsorption experimental device, the compaction of resin particles and bubble removal are achieved, solving the problems of low adsorption and elution efficiency and the influence of bubbles in the prior art, and significantly improving the separation efficiency.
Patent Information
- Application Number
- CN202310044681.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-01-30
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2043-01-30
AI Technical Summary
The prior art is difficult to achieve sufficient compaction of resin particles in resin adsorption experiments, resulting in low adsorption and elution efficiency, and difficulty in completely removing bubbles in the stock solution, making it easy to form holes or faults in the resin column.
A resin adsorption experimental device was designed, using a combined structure of an extrusion column and a pressure plate. The resin particles were compacted by the extrusion column, and bubbles in the stock solution were removed through the negative pressure in the inner cavity of the pressure plate.
The particle adsorption rate, thorough flushing degree and particle elution rate of the resin column are improved, ensuring the full compaction and dispersion of the resin particles, avoiding the influence of the adsorption process by bubbles in the stock solution, and significantly improving the separation efficiency.
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Figure CN116020171B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of adsorption separation, in particular to a resin adsorption experimental device. Background Art
[0002] The principle of resin adsorption is to use the porous structure of resin particles to adsorb specific particles in the solution to achieve the purpose of separation. It is widely used in sewage treatment, drug separation or purification. When conducting resin adsorption related experiments, the current common practice is to fill the glass tube with soaking liquid containing resin particles and make the resin particles dense, then wash the soaking liquid to form a resin adsorption column, and then add stock solution in turn to adsorb the particles in the stock solution, add flushing solution to flush the residual stock solution in the resin column, and add elution solution to elute the particles adsorbed in the resin particles.
[0003] In the above process, in the adsorption and elution process, we hope that the resin particles are as dense as possible and the gaps between the resin particles are as small as possible, so that the stock solution or the eluent can penetrate through the holes inside the resin particles instead of the gaps between the resin particles, so that the adsorbable particles in the stock solution can be fully adsorbed or the eluent can fully elute the adsorbed particles in the resin particles. In order to make the resin particles dense, the commonly used method is shaking or knocking the glass tube, such as the video material at the network link https: / / www.bilibili.com / video / av216978167 / , but this compaction method has limited compaction, and the gap ratio between the resin particles is still large. However, because it is too common, it has become a convention. After searching, no related devices and methods for further compacting the resin particles have been found.
[0004] As for the flushing process, the current focus is to fully wash away the residual stock solution inside and outside the resin particles. While considering fully washing away the stock solution in the pores inside the resin particles, the residual flushing liquid on the surface of the resin particles should also be fully considered to be thoroughly washed away. The former requires that the resin particles be as dense as possible so that the flushing liquid can flow through the inside of the resin particles, while the latter requires that the resin particles be fully dispersed so that the flushing liquid completely surrounds and soaks the resin particles. The current resin column always remains dense after being loaded, which results in the residual stock solution on the surface where the resin particles are squeezed against each other may not be completely rinsed away.
[0005] In addition, bubbles may be mixed in the stock solution, which may cause holes or even faults to form in the resin column during the adsorption process. Therefore, the bubbles in the stock solution should be removed as much as possible. The invention patent with application number: CN201711070586.9 discloses a device for removing bubbles. However, due to its complicated equipment and low integration, it is more suitable for industrial production equipment, but not suitable for adsorption experimental equipment. Summary of the invention
[0006] In order to further improve the particle adsorption rate, flushing thoroughness and particle elution rate of the resin column, and at the same time provide a solution for removing bubbles in a stock solution suitable for experimental equipment, the present invention provides a resin adsorption experimental device.
[0007] The technical solution includes a glass tube, a first liquid valve is installed at the lower end of the glass tube, and resin particles are densely filled in the glass tube to form a resin exchange column; a coaxial extrusion column is installed in the glass tube, and the extrusion column is formed by connecting a conical section at the bottom and a cylindrical section at the top, the conical section is thick at the bottom and thin at the top, a circular bottom plate is fixed at the lower end of the extrusion column, the diameter of the bottom plate is equal to the inner diameter of the glass tube, and the bottom plate is densely covered with first liquid holes that are transparent from top to bottom, a pressure plate is installed at the upper end of the glass tube, the pressure plate is a hollow circular plate, and an avoidance hole is opened in the center of the pressure plate, and the upper end of the cylindrical section of the extrusion column is connected from the avoidance hole to the bottom of the glass tube. The hole is passed through, the outer diameter of the pressure plate is equal to the inner diameter of the glass tube, and the bottom surface of the pressure plate is densely covered with second liquid holes, the top surface of the pressure plate is provided with a liquid filling port, and the top surface of the pressure plate is equipped with an exhaust pipe connected with its internal cavity, the exhaust pipe is connected with an air pump, and the air pump can form a negative pressure in the inner cavity of the pressure plate; a liquid channel is opened at the axis of the extrusion column, the upper end of the liquid channel is open and the lower end is closed, and liquid can be poured into the liquid channel from the upper end, and a plurality of groups of third liquid holes are evenly distributed along the axial direction on the side wall of the extrusion column, each group of third liquid holes includes a plurality of third liquid holes evenly distributed around the circumference, the inner end of each third liquid hole is connected with the liquid channel, and the outer end of the third liquid hole is higher than the inner end.
[0008] The upper surface of the bottom plate is paved with a filter screen, the aperture of which is smaller than the particle size of the resin particles.
[0009] The outer ends of each group of the third liquid holes are inclined in the clockwise direction and in the counterclockwise direction.
[0010] The conical section of the extrusion column is made of glass, and the cylindrical section is a metal tube with external threads. The lower end of the metal tube is fixedly connected to the upper end of the conical section via two mutually perpendicular pins. An internally threaded tube is screwed on the metal tube, and the lower end of the internally threaded tube contacts the upper end surface of the pressure plate.
[0011] The invention also comprises a liquid adding funnel, the lower end of which is inserted into the liquid adding hole, and the lower end of which is provided with a second liquid valve.
[0012] The upper end of the glass tube is provided with an extended first convex edge, and the glass tube can be inserted into the annular support frame through the first convex edge.
[0013] The upper end of the pressure plate is provided with an extended second convex edge, and the pressure plate can be supported on the upper end of the glass tube through the second convex edge.
[0014] The pressing plate is composed of two semicircular parts which are cut along the diameter. When installing, the two parts can be buckled on the external threaded tube from both sides and moved downward to be pressed into the upper end of the glass tube.
[0015] The present invention can improve the adsorption rate and elution rate of adsorbable particles in the stock solution, thoroughly clean the residual stock solution adhering to the resin particles, and achieve more efficient separation; the bubbles in the stock solution can be removed before adsorption to avoid the formation of holes or faults in the resin column during adsorption. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 It is a front cross-sectional view during the adsorption and elution process of the present invention.
[0017] Figure 2 It is a front cross-sectional view during the flushing process of the present invention.
[0018] Figure 3 It is a top sectional view of the position of the third liquid hole.
[0019] Figure 4 A three-dimensional view of one half of the pressure plate.
[0020] Figure 5 Schematic diagram of the filter mesh filled with resin particles.
[0021] Figure 6 for Figure 1 Enlarged view of position A in the middle.
[0022] Figure 7 for Figure 2 Enlarged view of position B in the middle. DETAILED DESCRIPTION
[0023] In conjunction with the accompanying drawings, the present invention comprises a glass tube 1, a first liquid valve 2 is installed at the lower end of the glass tube 1, resin particles are densely filled in the glass tube 1 to form a resin exchange column, the liquid to be separated is added from the upper end of the glass tube 1, and flows out from the lower end of the glass tube 1 after being adsorbed by the resin exchange column; a coaxial extrusion column 3 is installed in the glass tube 1, the extrusion column 3 is formed by connecting a conical section at the bottom and a cylindrical section at the top, the conical section is thick at the lower end and thin at the upper end, a circular bottom plate 4 is fixed at the lower end of the extrusion column 3, the diameter of the bottom plate 4 is equal to the inner diameter of the glass tube 1, and the bottom plate 4 is densely covered with first liquid holes 5 that are transparent from top to bottom, and the bottom plate 4 can carry the resin. The fat particles are formed by the first liquid hole 5, and the filtrate can seep down from the first liquid hole 5. A pressure plate 6 is installed on the upper end of the glass tube 1. The pressure plate 6 is a hollow circular plate, and a avoidance hole 7 is opened in the center of the pressure plate 6. The upper end of the cylindrical section of the extrusion column 3 passes through the avoidance hole 7. The outer diameter of the pressure plate 6 is equal to the inner diameter of the glass tube 1, and the bottom surface of the pressure plate 6 is densely covered with second liquid holes 8. The top surface of the pressure plate 6 is provided with a liquid adding port 9. The liquid to be separated is added into the pressure plate 6 from the liquid adding hole, and then seeps down through the second liquid hole 8. The top surface of the pressure plate 6 is provided with an air extraction pipe 10 connected to the internal cavity thereof. The air extraction pipe 10 is connected to an air pump 11, and the pressure can be made to Negative pressure is formed in the inner cavity of the plate 6. If there are bubbles in the liquid to be separated, the gas in the liquid will escape under the action of negative pressure after entering the pressure plate 6, thereby achieving the effect of defoaming and degassing, and avoiding the formation of faults during adsorption; the resin particles are filled between the bottom plate 4 and the pressure plate 6. After the resin particles are filled, the pressure plate 6 is fixed and does not move, and the extrusion column 3 and the bottom plate 4 are pulled upward, then the side wall of the extrusion column 3 will squeeze the resin particles around, so that the resin particles are dense; a liquid channel 12 is opened at the axis of the extrusion column 3, the upper end of the liquid channel 12 is open and the lower end is closed, and liquid can be poured into the liquid channel 12 from the upper end, and the side wall of the extrusion column 3 is along the axis There are multiple groups of third liquid holes 13 evenly distributed in the middle, and each group of third liquid holes 13 includes multiple third liquid holes evenly distributed around the circumference. The inner end of each third liquid hole 13 is connected to the liquid channel 12, and the outer end of the third liquid hole 13 is higher than the inner end. After the filtration is completed, the extrusion column 3 is moved downward, and the extrusion of the resin particles by the extrusion column 3 disappears. After the upper end of the liquid channel 12 is connected to the pressure water source, the water flow will flow out from the third liquid holes 13 through the liquid channel 12, and the water flow will push the resin particles upward to disperse the resin particles, so that each resin particle is completely wrapped by the flushing liquid and fully contacts with the flushing liquid to achieve comprehensive and thorough flushing, thereby avoiding residual filtrate on the surface or in the pores of the resin particles.
[0024] A filter screen 14 is paved on the upper surface of the bottom plate 4. The pore size of the filter screen 14 is smaller than the particle size of the resin particles. On the one hand, it can prevent the resin particles from spilling from the first liquid hole 5 to the bottom. On the other hand, during filtering, the resin particles fill the mesh of the filter screen 14, and the filtrate must penetrate through the resin particles in the mesh. This requires the filtrate to pass through the holes in the resin particles, thereby completely adsorbing the small amount of particles that have not been adsorbed in the filtrate.
[0025] The outer ends of each group of the third liquid holes 13 are inclined clockwise or counterclockwise. The third liquid holes 13 with the outer ends inclined upward and in the same circumferential direction can form a conical annular vortex flow, thereby completely dispersing the resin particles.
[0026] The conical section of the extrusion column 3 is made of glass, and the cylindrical section is a metal tube 15 with external threads. Glass has good chemical stability, and metal has good machining performance and strength to facilitate the processing and use of threads. The lower end of the metal tube 15 is fixedly connected to the upper end of the conical section through two mutually perpendicular pins 16. An internally threaded tube 17 is screwed on the metal tube 15. The lower end of the internally threaded tube 17 is in contact with the upper end surface of the pressure plate 6. By rotating the internally threaded tube 17, the extrusion column 3 can be pulled up and down.
[0027] The liquid adding funnel 18 is also included. The lower end of the liquid adding funnel 18 is inserted into the liquid adding hole, and the lower end of the liquid adding funnel 18 is equipped with a second liquid valve 19.
[0028] The upper end of the glass tube 1 is provided with an extended first flange 20 , through which the glass tube 1 can be inserted into the annular support frame.
[0029] The upper end of the pressing plate 6 is provided with an extended second flange 21 , and the pressing plate 6 can be supported on the upper end of the glass tube 1 through the second flange 21 .
[0030] The pressing plate 6 is composed of two semicircular parts cut along the diameter. When installed, the two parts can be buckled on the external threaded tube from both sides and moved downward to be pressed into the upper end of the glass tube 1.
[0031] When the present invention is used, the glass tube 1 is inserted into the annular support frame, the first convex edge 20 at the upper end of the glass tube 1 supports the glass tube 1, and then the extrusion column 3 is inserted into the glass tube 1 from the upper end, the bottom plate 4 is at the bottom and the outer edge of the bottom plate 4 is in contact with the inner wall of the glass tube 1, and then the pre-treated resin particles are filled into the glass tube 1 from the upper end of the glass tube 1. When filling, the glass tube 1 is shaken or the outer wall of the glass tube 1 is knocked to make the resin particles basically dense. After the filling is completed, the pressure plate 6 is buckled on the extrusion column 3 and pressed downward into the glass tube 1, and the pressure plate 6 is located below the internal threaded tube 17 , or first install the pressure plate 6 and then screw on the internal threaded tube 17, the second convex edge 21 on the pressure plate 6 is pressed on the first convex edge 20, and then fix the extrusion column 3 with one hand so that it cannot rotate, and screw the internal threaded tube 17 with the other hand, and pull the extrusion column 3 upward through the action of the thread. When pulling, the side wall of the tapered section of the extrusion column 3 will further completely compact the resin particles in the glass tube 1; when pulling the extrusion column 3, the extrusion column 3 is appropriately rotated to make the filter screen 14 on the bottom plate 4 rub against the bottom resin particles, so that the resin particles completely fill the mesh of the filter screen 14.
[0032] After filling and squeezing are completed, the lower end of the liquid adding funnel 18 is inserted into the liquid adding port 9 of the pressing plate 6, and then the air pump 11 is started, and the air suction pipe 10 starts to weep, and negative pressure is formed in the pressing plate 6. The raw liquid to be adsorbed and separated is added into the pressing plate 6 through the liquid adding funnel 18. After the raw liquid is added into the pressing plate 6, it seeps down through the second liquid hole 8 at the bottom of the pressing plate 6. If there are bubbles in the raw liquid, the gas in the raw liquid will escape in the negative pressure environment in the pressing plate 6, so that the gas in the raw liquid can avoid forming faults or holes during adsorption; the lower part of the pressing plate 6 When the liquid seeps through the resin column, the adsorbable particles in the stock solution are adsorbed by the resin pores. A small amount of the stock solution may seep through the gaps between the resin particles without passing through the pores inside the resin particles. When the stock solution seeps to the filter screen 14 at the bottom layer, since the mesh holes of the filter screen 14 are filled with resin particles one by one, it is easy to pass through the filter screen 14 and must pass through the pores inside the particles in the mesh holes, thus avoiding the incomplete adsorption of the adsorbable particles in the small amount of stock solution, thereby reducing the residual amount of adsorbable particles in the stock solution.
[0033] After the original liquid adsorption and filtration is completed, the resin particles are rinsed. First, the rinsing liquid is added through the liquid adding funnel 18. The cleaning liquid is generally pure distilled water. Most of the residual original liquid is rinsed away for a period of time. However, due to the dense squeezing between the resin particles, the outer wall of the resin particles may not be completely rinsed in place and the original liquid may remain. Then, the internal threaded tube 17 is screwed to move the extrusion column 3 downward, so that the space between the bottom plate 4 and the pressure plate 6 becomes larger to provide space for the dispersion of the resin particles. Then, the cleaning liquid is added into the glass tube 1 in two ways. One of the ways is still added through the liquid adding funnel 18, but the flow rate is reduced or even completely closed, and the other way is added from the liquid channel 12 in the extrusion column 3. The upper end of the rinse liquid is pumped into the liquid channel 12 by a pressure pump, and then rushed out through the third liquid hole 13 on the extrusion column 3. Due to the oblique setting of the third liquid holes 13, the liquid flow of the same group of third liquid holes 13 forms a conical vortex flow field in the glass tube 1, and the resin particles are fully dispersed in the flow field. Each particle is completely surrounded by the rinse liquid, so that the original liquid adhering to the outer wall of the particle is completely rinsed off, and the rinse liquid finally flows out from the lower end of the glass tube 1. If the pumping speed of the rinse liquid is greater than its outflow speed, the inner cavity of the pressure plate 6 has a buffering effect. When the rinse liquid in the inner cavity of the pressure plate 6 is about to be full, the pumping is temporarily stopped, and the pumping is continued after a part of the rinse liquid flows out.
[0034] After the flushing is completed, the internal threaded tube 17 is screwed again to restore the resin particles to a compacted state, and then the eluent is added through the liquid adding funnel 18 to elute the particles adsorbed in the resin particles.
[0035] The present invention can squeeze the resin particles to a dense state to the maximum extent during the adsorption and elution process through the extrusion effect of the extrusion column 3, reduce the gaps between the resin particles, allow the stock solution or the eluent to fully flow through the internal pores of the resin particles, and ensure that all the stock solution flows through the pores of the resin particles by filling the resin particles in the mesh of the filter 14, greatly improving the adsorption rate and elution rate of the adsorbable particles in the stock solution, and achieving a more efficient separation; during the flushing process, the resin particles are flushed from a dense state to a completely dispersed state by expanding the space and the impact of the water flow, so that each resin particle is completely surrounded by the flushing liquid, and the residual stock solution adhering to the resin particles is thoroughly washed away; furthermore, the negative pressure in the inner cavity of the pressure plate 6 can be used to remove bubbles in the stock solution before adsorption, avoiding the formation of holes or faults in the resin column during adsorption, and it is integrated with the compaction and dispersion scheme of the resin particles, and is suitable for experimental equipment.
Claims
1. A resin adsorption experimental device, comprising a glass tube (1), a first liquid valve (2) being installed at the lower end of the glass tube (1), and resin particles being densely packed in the glass tube (1) to form a resin exchange column; It is characterized in that A coaxial squeezing column (3) is installed in the glass tube (1). The squeezing column (3) is formed by connecting a conical section at the bottom and a cylindrical section at the top. The conical section is thick at the bottom and thin at the top. A circular bottom plate (4) is fixed at the bottom end of the squeezing column (3). The diameter of the bottom plate (4) is equal to the inner diameter of the glass tube (1). The bottom plate (4) is densely covered with first liquid holes (5) that are transparent from top to bottom. A pressure plate (6) is installed at the upper end of the glass tube (1). The pressure plate (6) is a hollow circular plate. The center of the pressure plate (6) is provided with an avoidance hole (7). The upper end of the cylindrical section passes through the avoidance hole (7), the outer diameter of the pressure plate (6) is equal to the inner diameter of the glass tube (1), and the resin particles are filled between the bottom plate (4) and the pressure plate (6). After the resin particles are filled, the pressure plate (6) is fixed and the extrusion column (3) and the bottom plate (4) are pulled upward, and the side wall of the extrusion column (3) squeezes the resin particles around, thereby making the resin particles dense; the bottom surface of the pressure plate (6) is densely covered with second liquid holes (8), the top surface of the pressure plate (6) is provided with a liquid filling port (9), and the top surface of the pressure plate (6) is provided with a The air extraction pipe (10) is connected to an air pump (11), and a negative pressure can be formed in the inner cavity of the pressure plate (6) through the air pump (11); a liquid channel (12) is opened at the axis of the extrusion column (3), the upper end of the liquid channel (12) is open and the lower end is closed, and liquid can be poured into the liquid channel (12) from the upper end; a plurality of groups of third liquid holes (13) are evenly distributed along the axial direction on the side wall of the extrusion column (3), each group of third liquid holes (13) includes a plurality of third liquid holes (13) evenly distributed around the circumference, the inner end of each third liquid hole (13) is connected to the liquid channel (12), and the outer end of the third liquid hole (13) is high At the inner end, the outer ends of each group of the third liquid holes (13) are inclined in a clockwise direction or in a counterclockwise direction; after the filtration is completed, the squeezing column (3) is moved downward, the squeezing of the resin particles by the squeezing column (3) disappears, and after the upper end of the liquid channel (12) is connected to the pressure water source, the water will flow out from the third liquid holes (13) through the liquid channel (12), and the water will push the resin particles upward to disperse the resin particles, so that each resin particle is completely wrapped by the flushing liquid, fully in contact with the flushing liquid to achieve comprehensive and thorough flushing, and avoid residual original liquid or eluent on the surface or pores of the resin particles; The upper surface of the bottom plate (4) is paved with a filter screen (14), and the pore size of the filter screen (14) is smaller than the particle size of the resin particles.
2. A resin adsorption experimental device according to claim 1, It is characterized in that The conical section of the extrusion column (3) is made of glass, and the cylindrical section is a metal tube (15) processed with an external thread. The lower end of the metal tube (15) is fixedly connected to the upper end of the conical section via two mutually perpendicular pins (16). An internally threaded tube (17) is screwed onto the metal tube (15), and the lower end of the internally threaded tube (17) contacts the upper end surface of the pressure plate (6).
3. A resin adsorption experimental device according to claim 1, It is characterized in that It also includes a liquid adding funnel (18), the lower end of which is inserted into the liquid adding hole, and a second liquid valve (19) is installed at the lower end of the liquid adding funnel (18).
4. A resin adsorption experimental device according to claim 1, It is characterized in that An outwardly extending first convex edge (20) is provided at the upper end of the glass tube (1), and the glass tube (1) can be inserted into the annular support frame via the first convex edge (20).
5. A resin adsorption experimental device according to claim 1, It is characterized in that The upper end of the pressure plate (6) is provided with an extended second convex edge (21), and the pressure plate (6) can be supported on the upper end of the glass tube (1) via the second convex edge (21).
6. A resin adsorption experimental device according to claim 1, It is characterized in that The pressure plate (6) is composed of two semicircular parts cut along the diameter. When installed, the two parts can be buckled on the external threaded tube from both sides and moved downward to be pressed into the upper end of the glass tube (1).
Citation Information
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