Purification apparatus for monitoring online residual polyquaternary ammonium salt-51

Abstract

The utility model relates to polyquaternary ammonium salt -51 preparation technical field, concretely relates to the purification device of polyquaternary ammonium salt -51 of on -line monitoring monomer residue. Including the purification kettle, the bottom of ethanol storage tank, mixed solvent storage tank bottom and polyquaternary ammonium salt -51 solution tank bottom are connected respectively through pipeline to the top of purification kettle, and the top of mixed liquid recovery tank and polyquaternary ammonium salt -51 solution tank are connected respectively through pipeline to the bottom of purification kettle, be equipped with grating plate in the purification kettle, and grating plate edge and the inner wall of purification kettle slide and paste, and the fixed sliding rod has on grating plate, and sliding rod passes through the top of purification kettle and is sealed and is connected with the movable connection of purification kettle, and the sampling port is equipped with the closed sampler on the sampling port, and the sampling port is located above grating plate. The utility model realizes on -line sampling in the polyquaternary ammonium salt -51 purification process, and the monomer residual amount is detected on -line, and according to the sampling result, selects secondary purification or discharges material;The sampling process is closed, avoids solvent gas escape.

Description

Technical Field

[0001] This utility model relates to the field of polyquaternium-51 preparation technology, specifically to a purification device for polyquaternium-51 with online monitoring of monomer residues. Background Technology

[0002] Polyquaternium-51 is polymerized from 2-methacryloyloxyethyl phosphoric acid choline (MPC) and n-butyl methacrylate (BMA). It has excellent biocompatibility, film-forming properties and moisturizing properties, and is widely used in the fields of medicine, cosmetics and biomaterials.

[0003] As the applications of polyquaternium-51 expand to pharmaceutical-grade and high-purity applications, its purity, especially the residual amount of unreacted monomers (mainly 2-methacryloyloxyethyl phosphate and n-butyl methacrylate) from the synthesis process, has become a key indicator affecting product quality and performance. If the monomer impurity content in polyquaternium-51 is too high (≥50ppm), it may cause mucosal irritation or local allergic reactions; long-term exposure may cause harm to the human body, failing to meet the requirements for pharmaceutical-grade and daily chemical-grade raw materials.

[0004] Safety standards. Therefore, achieving efficient removal and precise control of residual monomers in polyquaternium-51 is one of the core requirements for its industrial application.

[0005] Currently, the purification of polyquaternium-51 mainly adopts the "precipitation separation" process. The precipitation separation process involves adding a crude polyquaternium-51 solution to a mixed solvent of acetone and ethyl acetate, causing the polymer to precipitate and separate from the monomers dissolved in the mixed solvent. However, this process has the problem of incomplete monomer separation (especially low-concentration residual monomers are easily carried along with polymer precipitation), and it is impossible to monitor the changing trend of monomer residues in real time during the production process. Timely online sampling and testing are required. However, during the sampling process, a large amount of gas volatilized from the solvent in the reactor will escape from the sampling port, which will affect the operating environment. Utility Model Content

[0006] The technical problem to be solved by this utility model is to propose a purification device for polyquaternium-51 with online monitoring of monomer residue. The device enables online sampling and detection of monomer residue during the purification process of polyquaternium-51, and selects secondary purification or discharge based on the sampling results. The sampling process is closed, avoiding the environmental impact caused by the escape of solvent gas.

[0007] The purification device for online monitoring of residual polyquaternium-51 monomers according to this utility model includes a purification kettle, a mixed solvent storage tank, an ethanol storage tank, a polyquaternium-51 solution tank, and a mixed liquid recovery tank. The top of the purification kettle is connected to the bottom of the ethanol storage tank, the bottom of the mixed solvent storage tank, and the bottom of the polyquaternium-51 solution tank via pipes. The bottom of the purification kettle is connected to the top of the mixed liquid recovery tank and the top of the polyquaternium-51 solution tank via pipes. A grid plate is provided inside the purification kettle, with the edge of the grid plate slidingly attached to the inner wall of the purification kettle. A sliding rod is fixed on the grid plate, which passes upward through the top of the purification kettle and is sealed and movablely connected to the purification kettle. A sampling port is provided on the side wall of the purification kettle, and a sealed sampler is provided on the sampling port. The sampling port is located above the grid plate.

[0008] Preferably, a feed pump is installed on the pipeline connecting the purification vessel and the polyquaternium salt-51 solution tank.

[0009] Preferably, the sealed sampler includes a sampling cylinder fixedly connected to the side wall of the purification vessel and arranged horizontally. A piston is provided inside the sampling cylinder, and a push rod is fixed to the outside of the piston. A scoop is provided on the push rod and is arranged perpendicular to the push rod downward. The scoop includes a fixed arm fixedly connected to the push rod and a movable arm hinged to the other end of the fixed arm by a torque spring. A sampling groove is provided at the end of the movable arm that is not connected to the fixed arm, and the opening direction of the sampling groove is perpendicular to the movable arm. A rotating block is rotatably connected to the push rod. The outer wall of the rotating block is sealed and movably connected to the inner wall of the sampling cylinder. An arc-shaped baffle that bends toward the push rod is provided on the side of the rotating block near the piston. When the rotating block rotates to the point where the arc-shaped baffle contacts the movable arm, the movable arm can slide along the inner side of the arc-shaped baffle.

[0010] Preferably, the hinge direction of the movable arm is perpendicular to the push rod.

[0011] Preferably, the push rod has a push handle at the end away from the piston.

[0012] Preferably, when the angle between the movable arm and the fixed arm is 180°, the length of the scoop is greater than the radius of the inner cavity of the sampling cylinder.

[0013] Preferably, a rotating rod is fixedly provided on the side of the rotating block away from the piston, and a rotating ring is provided in the middle of the rotating rod, which is movably sleeved on the push rod.

[0014] Preferably, the push rod is provided with a positioning hole one, and the rotating ring is provided with positioning holes two on both sides with the same inner diameter as the positioning hole one. Positioning pins are detachably provided in positioning holes one and positioning holes two.

[0015] Preferably, the locating pin is a bolt pin, and both locating hole one and locating hole two are provided with threads that are helically engaged with the locating pin.

[0016] Preferably, the movable arm is provided with a limiting rod, which is correspondingly set with the fixed arm and abuts against the fixed arm when the angle between the fixed arm and the movable arm is 180°, so that the angle between the fixed arm and the movable arm cannot exceed 180°.

[0017] Preferably, the upper end of the sliding rod passes through the purification vessel and is connected to a rotary lifting mechanism.

[0018] Preferably, the rotary lifting mechanism includes a rotary motor and an electric lifting mechanism. The output end of the rotary motor is fixedly connected to the upper end of the sliding rod, and the rotary motor is fixedly connected to the lifting part of the electric lifting mechanism. The electric lifting mechanism is preferably an electric lifting screw.

[0019] A mixture of acetone and ethyl acetate is added to the purification reactor. An ethanol solution of polyquaternium-51 is then pumped into the reactor, causing polyquaternium-51 to precipitate and be retained by a grid plate. The mixed solution is released from the bottom of the reactor and sampled through a sealed sampler. Monomer residue is detected using liquid chromatography. If the monomer residue is ≤50 ppm, production automatically proceeds to the next step. If the monomer residue is >50 ppm, ethanol is used to dissolve the polyquaternium-51 on the grid plate. The polyquaternium-51 solution is then pumped into a polyquaternium-51 solution tank. A mixture of acetone and ethyl acetate is then added to the purification reactor. The ethanol solution of polyquaternium-51 from the polyquaternium-51 solution tank is pumped into the purification reactor for secondary purification. The sampling and detection process is repeated until the online detection of monomer residue is ≤50 ppm.

[0020] The sampling process is as follows: When no sampling is being performed, the piston closes the sampling cylinder, the movable arm abuts against the arc-shaped baffle, and the angle between the movable arm and the fixed arm is less than 180°. The arc-shaped baffle overcomes the torque spring and restricts the movable arm within the arc-shaped baffle. The push rod is pushed along the sampling cylinder into the purification kettle until the sampling spoon is completely out of the sampling cylinder. During this process, the rotating block continuously seals the sampling cylinder to prevent gas from escaping from the purification kettle. The grid plate is then raised to near the lower end of the sampling port. Keeping the push rod stationary, rotate the rotating block around the push rod, causing the arc-shaped baffle to rotate until it no longer abuts against the movable arm. Under the action of the torque spring, the movable arm and the fixed arm form a 180° angle. Adjust the height of the grid plate so that the lowest point of the sampling slot opening is below the polyquaternium-51 precipitate. Rotate the grid plate to scrape the polyquaternium-51 precipitate into the sampling slot. Move the grid plate down and rotate the rotating block around the push rod until the arc-shaped baffle abuts against the movable arm. Continue rotating to overcome the force of the torque spring and retract the movable arm, making the angle between the movable arm and the fixed arm less than 180°. Pull the push rod outward until the rotating block and the scoop exit the sampling cylinder. Take out the sample from the sampling slot for testing. At this time, the piston is located inside the sampling cylinder, and the sampling cylinder remains closed.

[0021] Compared with the prior art, the beneficial effects of this utility model are:

[0022] 1. During the purification process of polyquaternium-51, online sampling and detection of monomer residues are implemented. After testing the monomer residues in the sample, if the residues are substandard, ethanol is injected from the ethanol storage tank into the purification vessel to dissolve the polyquaternium-51. The ethanol solution of polyquaternium-51 is then pumped into the polyquaternium-51 solution tank for secondary purification. Online sampling and testing, with direct secondary purification for unqualified monomer residues, greatly improves work efficiency.

[0023] 2. By setting up a sealed sampler, the sampling tube is always in a closed state during the sampling process, which avoids a large amount of solvent gas escaping from the purification vessel and reduces pollution to the operating environment. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the purification device for online monitoring of residual polyquaternium-51 monomers according to this utility model.

[0025] Figure 2 This is a schematic diagram of the external structure of the purification kettle;

[0026] Figure 3 This is a schematic diagram of a sealed sampler with the movable arm inside the arc-shaped baffle.

[0027] Figure 4 This is a schematic diagram of the cross-sectional structure of a sealed sampler with the movable arm inside the arc-shaped baffle.

[0028] Figure 5 This is a schematic diagram of a sealed sampler with the movable arm outside the arc-shaped baffle.

[0029] Figure 6 This is a schematic diagram of the cross-sectional structure of the sealed sampler with the movable arm outside the arc-shaped baffle.

[0030] Figure 7 This is a schematic diagram of the material scoop structure;

[0031] Figure 8 This is a schematic diagram of the material scoop from another angle;

[0032] Figure 9 This is a schematic diagram of the purification vessel in the closed sampler-unsampled state;

[0033] Figure 10 This is a schematic diagram of the purification vessel in the piston-driven state.

[0034] Figure 11 This is a schematic diagram of the purification kettle in the sampling state of a closed sampler;

[0035] In the diagram: 1. Purification vessel; 2. Mixed solvent storage tank; 3. Ethanol storage tank; 4. Polyquaternium-51 solution tank; 5. Mixed liquid recovery tank; 6. Grating plate; 7. Sliding rod; 8. Sampling port; 9. Feed pump; 10. Sampling cylinder; 11. Piston; 12. Push rod; 13. Fixed arm; 14. Torque spring; 15. Movable arm; 16. Sampling groove; 17. Rotating block; 18. Arc-shaped baffle; 19. Rotating rod; 20. Rotating ring; 21. Positioning hole one; 22. Positioning pin; 23. Rotary motor; 24. Electric lifting mechanism; 25. Push handle; 26. Limiting rod. Detailed Implementation

[0036] The present invention will now be described clearly and completely with reference to the accompanying drawings.

[0037] Example

[0038] like Figure 1 , Figure 2 As shown, the purification device for online monitoring of residual polyquaternium-51 monomers includes a purification kettle 1, a mixed solvent storage tank 2, an ethanol storage tank 3, a polyquaternium-51 solution tank 4, and a mixed liquid recovery tank 5. The top of the purification kettle 1 is connected to the bottom of the ethanol storage tank 3, the bottom of the mixed solvent storage tank 2, and the bottom of the polyquaternium-51 solution tank 4 via pipes. The bottom of the purification kettle 1 is connected to the top of the mixed liquid recovery tank 5 and the top of the polyquaternium-51 solution tank 4 via pipes. A grid plate 6 is provided inside the purification kettle 1, with its edge sliding against the inner wall of the purification kettle 1. A sliding rod 7 is fixed on the grid plate 6, passing upward through the top of the purification kettle 1 and being sealed and movablely connected to the purification kettle 1. A sampling port 8 is provided on the side wall of the purification kettle 1, and a sealed sampler is provided on the sampling port 8, which is located above the grid plate 6. A feed pump 9 is provided on the pipe connecting the purification kettle 1 and the polyquaternium-51 solution tank 4.

[0039] like Figure 1 , Figures 3-7As shown, the sealed sampler includes a sampling cylinder 10 fixedly connected to the side wall of the purification vessel 1 and horizontally arranged. A piston 11 is provided inside the sampling cylinder 10, and a push rod 12 is fixedly attached to the outside of the piston 11. A scoop is provided on the push rod 12, and the scoop is arranged perpendicularly downwards to the push rod 12. The scoop includes a fixed arm 13 fixedly connected to the push rod 12 and a movable arm 15 hinged to the other end of the fixed arm 13 via a torque spring 14. The hinge direction of the movable arm 15 is perpendicular to the push rod 12, and the movable arm 15 is not connected to the fixed arm 12. A sampling groove 16 is provided at one end of the arm 13, and the opening direction of the sampling groove 16 is perpendicular to the movable arm 15. A rotating block 17 is rotatably connected to the push rod 12. The outer wall of the rotating block 17 is sealed and movably connected to the inner wall of the sampling cylinder 10. An arc-shaped baffle 18 that bends toward the push rod 12 is provided on the side of the rotating block 17 near the piston 11. When the rotating block 17 rotates until the arc-shaped baffle 18 contacts the movable arm 15, the movable arm 15 can slide along the inner side of the arc-shaped baffle 18 to achieve the retraction of the movable arm 15. A push handle 25 is provided at the end of the push rod 12 away from the piston 11.

[0040] When the angle between the movable arm 15 and the fixed arm 13 is 180°, the length of the scoop is greater than the inner radius of the sampling cylinder 10.

[0041] A rotating rod 19 is fixedly provided on the side of the rotating block 17 away from the piston 11. A rotating ring 20 is provided in the middle of the rotating rod 19. The rotating ring 20 is movably sleeved on the push rod 12.

[0042] The push rod 12 is provided with a positioning hole 21, and the rotating ring 20 is provided with positioning holes 2 on both sides with the same inner diameter as the positioning hole 21. Positioning pins 22 are detachably provided in the positioning holes 21 and positioning holes 2.

[0043] The locating pin 22 is a bolt pin, and both the locating hole 1 21 and the locating hole 22 are provided with threads that are helically engaged with the locating pin 22.

[0044] like Figure 8 As shown, the movable arm 15 is provided with a limiting rod 26, which is correspondingly provided with the fixed arm 13. When the angle between the fixed arm 13 and the movable arm 15 is 180°, the limiting rod 26 abuts against the fixed arm 13, so that the angle between the fixed arm 13 and the movable arm 15 cannot be greater than 180°.

[0045] like Figure 1 As shown, the upper end of the sliding rod 7 passes through the purification vessel 1 and is connected to a rotary lifting mechanism. The rotary lifting mechanism includes a rotary motor 23 and an electric lifting mechanism 24. The output end of the rotary motor 23 is fixedly connected to the upper end of the sliding rod 7, and the rotary motor 23 is fixedly connected to the lifting part of the electric lifting mechanism 24; the electric lifting mechanism 24 is an electric lifting screw.

[0046] The working process is as follows: A mixed solution of acetone and ethyl acetate, stored in the mixed solvent storage tank 2, is added to the purification kettle 1. An ethanol solution of polyquaternium-51 from the polyquaternium-51 solution tank 4 is pumped into the purification kettle 1 via the feed pump 9. Polyquaternium-51 precipitates out and is retained by the grid plate 6. The mixed solution is discharged from the bottom of the purification kettle 1 into the mixed solution recovery tank 5. A sample is taken from the sampling port 8 using a closed sampler, and monomer residue is detected using liquid chromatography. If the monomer residue is ≤50ppm, production will automatically proceed to the next step. One process; if the monomer residue is >50ppm, ethanol is released from ethanol storage tank 3 to dissolve polyquaternium-51 on grid plate 6, then the polyquaternium-51 ethanol solution is pumped into polyquaternium-51 solution tank 4, and then a mixture of acetone and ethyl acetate is added to purification kettle 1 through mixed solvent storage tank 2. The polyquaternium-51 ethanol solution in polyquaternium-51 solution tank 4 is pumped into purification kettle 1 for secondary purification. After purification, the sampling and detection process is repeated until the online detection of monomer residue is ≤50ppm.

[0047] The sampling process is as follows: Figure 9 As shown, when no sampling is being performed, the piston 11 closes the sampling cylinder 10, the movable arm 15 abuts against the arc-shaped baffle 18, and the angle between the movable arm 15 and the fixed arm 13 is less than 180°. The arc-shaped baffle 18 overcomes the torque spring 14 to confine the movable arm 15 within the arc-shaped baffle 18. Positioning pins 22 are internally threaded into positioning holes 1 and 2, restricting the rotation of the rotating block 17. Pushing the push rod 12 along the sampling cylinder 10 into the purification vessel 1 until the sampling spoon is completely out of the sampling cylinder 10, the state at this time is as follows. Figure 10 As shown, during this process, the rotating block 17 continuously seals the sampling cylinder 10 to prevent gas from escaping from the purification vessel 1; the grid plate 6 is lifted up to near the lower end of the sampling port 8. Keeping the push rod 12 stationary, the positioning pin 22 is unscrewed, and the rotating block 17 rotates around the push rod 12 by rotating the rotating rod 19, causing the arc-shaped baffle 18 to rotate until it no longer abuts against the movable arm 15. Once the second positioning hole on the other side rotates to coincide with the first positioning hole 21, the positioning pin 22 is screwed in to fix it. Under the action of the torque spring 14, the movable arm 15 and the fixed arm 13 form a 180° angle. The electric lifting mechanism 24 is activated to adjust the height of the grid plate 6 so that the lowest point of the sampling slot 16 opening is below the polyquaternium-51 precipitate. At this time, the sealed sampler is in the following state: Figure 11As shown, the rotary motor 23 is started to rotate the grid plate 6, causing the polyquaternium-51 precipitate to be scraped into the sampling trough 16. The electric lifting mechanism 24 is started to move the grid plate 6 down, causing the rotating block 17 to rotate around the push rod 12, so that the arc-shaped baffle 18 rotates to abut against the movable arm 15. The rotation continues to overcome the force of the torque spring 14, causing the movable arm 15 to retract into the arc-shaped baffle 18, so that the angle between the movable arm 15 and the fixed arm 13 is less than 180°. The push rod 12 is pulled outward until the rotating block 17 and the scoop exit the sampling cylinder 10, and the sample in the sampling trough 16 is taken out for testing. At this time, the piston 11 is located inside the sampling cylinder 10, and the sampling cylinder 10 is still closed, completing the sealed sampling.

Claims

1. A purification device for polyquaternium-51 with online monitoring of monomer residues, characterized in that, The equipment includes a purification vessel (1), a mixed solvent storage tank (2), an ethanol storage tank (3), a polyquaternium-51 solution tank (4), and a mixed liquid recovery tank (5). The top of the purification vessel (1) is connected to the bottom of the ethanol storage tank (3), the bottom of the mixed solvent storage tank (2), and the bottom of the polyquaternium-51 solution tank (4) through pipes. The bottom of the purification vessel (1) is connected to the top of the mixed liquid recovery tank (5) and the top of the polyquaternium-51 solution tank (4) through pipes. The purification vessel (1) is equipped with a grid plate (6). The edge of the grid plate (6) slides against the inner wall of the purification vessel (1). A sliding rod (7) is fixed on the grid plate (6). The sliding rod (7) passes upward through the top of the purification vessel (1) and is sealed and movablely connected to the purification vessel (1). The side wall of the purification vessel (1) is equipped with a sampling port (8). A sealed sampler is provided on the sampling port (8). The sampling port (8) is located above the grid plate (6).

2. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 1, characterized in that, A feed pump (9) is installed on the pipeline connecting the purification vessel (1) and the polyquaternium salt-51 solution tank (4).

3. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 1, characterized in that, The sealed sampler includes a sampling cylinder (10) that is fixedly connected to the side wall of the purification vessel (1) and is horizontally arranged. A piston (11) is provided inside the sampling cylinder (10). A push rod (12) is fixed to the outside of the piston (11). A scoop is provided on the push rod (12). The scoop is set vertically downward to the push rod (12). The scoop includes a fixed arm (13) that is fixedly connected to the push rod (12) and a movable arm (15) that is hinged to the other end of the fixed arm (13) by a torque spring (14). A sampling groove (16) is provided at the end of the movable arm (15) that is not connected to the fixed arm (13). The opening direction of the sampling groove (16) is perpendicular to the movable arm (15). A rotating block (17) is rotatably connected to the push rod (12). The outer wall of the rotating block (17) is sealed and movably connected to the inner wall of the sampling cylinder (10). An arc-shaped baffle (18) that bends toward the push rod (12) is provided on the side of the rotating block (17) near the piston (11).

4. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 3, characterized in that, When the angle between the movable arm (15) and the fixed arm (13) is 180°, the length of the scoop is greater than the inner radius of the sampling cylinder (10).

5. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 4, characterized in that, A rotating rod (19) is fixedly provided on the side of the rotating block (17) away from the piston (11). A rotating ring (20) is provided in the middle of the rotating rod (19). The rotating ring (20) is movably sleeved on the push rod (12).

6. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 5, characterized in that, The push rod (12) is provided with a positioning hole 1 (21), and the rotating ring (20) is provided with positioning holes 2 on both sides with the same inner diameter as the positioning hole 1 (21). Positioning pins (22) are detachably provided in the positioning hole 1 (21) and positioning hole 2.

7. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 6, characterized in that, The positioning pin (22) is a bolt pin, and both positioning hole one (21) and positioning hole two are provided with threads that are helically engaged with the positioning pin (22).

8. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 3, characterized in that, The movable arm (15) is provided with a limiting rod (26), which is correspondingly provided with the fixed arm (13). When the angle between the fixed arm (13) and the movable arm (15) is 180°, the limiting rod (26) abuts against the fixed arm (13), so that the angle between the fixed arm (13) and the movable arm (15) cannot be greater than 180°.

9. The purification apparatus for online monitoring of residual polyquaternium-51 monomers according to claim 1, characterized in that, The upper end of the sliding rod (7) passes through the purification vessel (1) and is connected to a rotary lifting mechanism.

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