An oxygen removal device for a polymer solution

Abstract

The utility model belongs to liquid degassing technical field, concretely relates to a kind of oxygen removal device of polymer solution, including reaction kettle, the inside of reaction kettle is provided with stirring assembly, and the top of reaction kettle is provided with dissolved oxygen monitoring assembly, charging port, air inlet hole and air outlet hole, air inlet hole is connected with gas supply component, and the bottom of reaction kettle is provided with lower discharge valve, and lower discharge valve is connected with solution conveying component;The oxygen removal device of the present polymer solution realizes the efficient oxygen removal to high viscosity, easy foaming polymer solution by the synergistic effect between inert gas supply component, multilayer stirring assembly, on-line dissolved oxygen monitoring assembly and solution conveying component, is suitable for polymer solution containing surfactant, and can monitor and control dissolved oxygen concentration in polymer solution in real time during oxygen removal process, improve oxygen removal effect and polymer solution preparation efficiency.

Description

Technical Field

[0001] This utility model belongs to the field of liquid degassing technology, specifically relating to a deoxygenation device for a polymer solution. Background Technology

[0002] Polymer thickeners are widely used due to their high molecular weight and strong intermolecular interactions, which impart high viscosity and unique rheological properties to solutions. However, polymers face aging issues during use, leading to a decline in their performance. This is especially true when polymers are in solution, where the molecular chains are exposed to solvents and oxygen, making them more susceptible to oxidative degradation at high temperatures, resulting in deterioration of viscosity or rheological properties. To study the long-term aging stability of polymer solutions at high temperatures, it is necessary to simulate their state in low-oxygen or near-oxygen-free environments, which requires effectively eliminating the interference of oxygen molecules in the polymer solution.

[0003] Currently, deoxygenation of polymer solutions commonly employs vacuuming or inert gas displacement. However, these conventional methods have significant shortcomings when dealing with high-viscosity polymer solutions. Firstly, the extremely high viscosity of polymer solutions, typically ranging from hundreds to thousands of millipascal-seconds, makes it difficult for oxygen molecules to diffuse within the solution and effectively remove them via vacuum or gas flow. Secondly, surfactants are often added to these polymer solutions to achieve better thickening and reduce interfacial tension. This easily generates a large amount of stubborn foam during inert gas bubbling or vacuuming. This foam not only occupies reaction space and affects mass transfer efficiency but is also difficult to eliminate, causing significant inconvenience to subsequent operations. Furthermore, kinetic evaluation of the aging stability of polymer solutions requires precise control of the oxygen concentration to assess degradation behavior under different oxygen concentrations. However, existing devices generally lack effective online oxygen concentration monitoring methods, making it impossible to control the deoxygenation process in real time and accurately. Therefore, there is an urgent need in this field for a deoxygenation device that can efficiently and conveniently process high-viscosity, easily foaming polymer solutions and achieve online monitoring and control of oxygen concentration. Utility Model Content

[0004] To address the aforementioned shortcomings of existing technologies, this invention provides a deoxygenation device for polymer solutions, which solves the problem of low deoxygenation efficiency of existing deoxygenation technologies for high-viscosity polymers.

[0005] To achieve the above objectives, the technical solution adopted by this utility model is as follows: A deoxygenation device for a polymer solution is provided, including a reaction vessel. The reaction vessel is equipped with a stirring assembly inside. The top of the reaction vessel is equipped with a dissolved oxygen monitoring assembly, a feed port, an air inlet, and an air outlet. The air inlet is connected to a gas supply assembly. The bottom of the reaction vessel is equipped with a bottom discharge valve, which is connected to a solution conveying assembly.

[0006] The beneficial effects of adopting the above technical solution are as follows: This deoxygenation device for polymer solutions achieves efficient deoxygenation of high-viscosity, easily foaming polymer solutions through the synergistic effect of the gas supply component, multi-layer stirring component, online dissolved oxygen monitoring component, and solution delivery component. It is suitable for polymer solutions containing surfactants and can monitor and control the dissolved oxygen concentration in the polymer solution in real time during the deoxygenation process, improving the deoxygenation effect and polymer solution preparation efficiency. Specifically, the multi-layer stirring component inside the reactor can fully mix and stir the polymer solution during the deoxygenation process. It can pre-deoxygenate the low-viscosity solvent first, then add the polymer and continue stirring, achieving simultaneous polymer dissolution and deoxygenation, greatly improving deoxygenation efficiency. Simultaneously, multi-layer stirring can effectively break up foam on the surface of the polymer solution, making it suitable for polymer solutions containing surfactants or those prone to foaming. The online dissolved oxygen monitoring component installed at the top of the reactor can monitor the dissolved oxygen concentration in real time, ensuring precise control of the deoxygenation process and allowing operators to accurately judge the timing of polymer addition and the deoxygenation effect. The air inlet and inert gas supply component can stably supply inert gas, quickly replacing the air inside the reactor and effectively reducing the dissolved oxygen concentration. The vent outlet discharges displaced air and excess gas, maintaining stable pressure inside the reactor and ensuring a safe and effective deoxygenation process. Additionally, the bottom discharge valve at the bottom of the reactor connects to the solution conveying assembly, enabling convenient and controllable conveying and packaging of the deoxygenated polymer solution. This ensures the purity and stable flow rate of the polymer solution during transport, helps maintain a low oxygen concentration, and improves the efficiency and safety of polymer solution preparation.

[0007] Furthermore, the stirring assembly includes a stirring motor and a stirring shaft connected to the output end of the stirring motor. The stirring shaft is provided with multiple layers of blades, and a U-shaped stirring paddle is provided at the bottom end of the stirring shaft.

[0008] The beneficial effects of adopting the above technical solution are as follows: the stirring motor can drive the multi-layer blades on the stirring shaft to rotate. The multi-layer blades ensure that the polymer solution is fully mixed in the vertical direction, while the U-shaped stirring blade set at the bottom of the stirring shaft can penetrate deep into the bottom of the polymer solution, effectively breaking up any possible sediment layers or local high viscosity areas, enhancing the overall fluidity of the polymer solution, thereby improving the deoxygenation effect and solving the problem that the existing deoxygenation technology is not effective in treating high viscosity polymer solutions.

[0009] Furthermore, the gas supply assembly includes a gas supply device, the output end of which is connected to the input end of a first conduit. The output end of the first conduit is provided with a first port, which is connected to the input end of a second conduit. The output end of the second conduit is connected to an air inlet, and the second conduit extends into the interior of the reactor.

[0010] The beneficial effects of adopting the above technical solution are as follows: the gas supply component can ensure that inert gas is stably input into the reactor. The output end of the gas supply device is connected to the first port through the first conduit, and then extends into the reactor through the air inlet of the second conduit. This not only ensures the continuity and stability of the inert gas supply, but also allows the inert gas to directly enter the reactor, thereby effectively replacing the air in the reactor, significantly reducing the dissolved oxygen concentration in the polymer solution, and improving the deoxygenation efficiency and effect of the polymer solution.

[0011] Furthermore, a pressure reducing valve is installed on the first conduit, and a first ball valve is installed on the second conduit.

[0012] The beneficial effects of adopting the above technical solution are as follows: the pressure reducing valve can regulate the pressure of the inert gas output from the gas supply device, ensuring that the gas enters the reactor stably and avoiding splashing of polymer solution due to excessive gas pressure or insufficient gas pressure affecting the deoxygenation effect; while the first ball valve can quickly cut off or restore gas flow, making it convenient for operators to flexibly adjust the gas supply according to actual needs during the deoxygenation process, thereby controlling the gas flow rate when deoxygenating high-viscosity polymer solutions, improving deoxygenation efficiency and stability.

[0013] Furthermore, the gas supply assembly also includes a gas distributor, the input end of which is connected to a third conduit, the third conduit is connected to a second port, and the second port is located at the output end of the first conduit; the output end of the gas distributor is provided with multiple gas distributor needle valves, and the multiple gas distributor needle valves are respectively connected to the first puncture needle.

[0014] The beneficial effects of adopting the above technical solution are as follows: the input end of the gas distributor is connected to the second port on the output end of the first conduit via the third conduit, realizing a stable transmission of inert gas from the supply device to the gas distributor; and the output end of the gas distributor is equipped with multiple gas distributor needle valves, each of which can be independently controlled and connected to the first puncture needle, enabling the operator to simultaneously perform efficient inert gas replacement on multiple vials containing polymer solutions, effectively avoiding the problem of low deoxygenation efficiency caused by uneven gas distribution or cumbersome operation in traditional deoxygenation technology, and is suitable for large-scale, efficient deoxygenation treatment of high-viscosity polymer solutions.

[0015] Furthermore, a second ball valve is installed on the third conduit.

[0016] The beneficial effects of adopting the above technical solution are as follows: The second ball valve is installed on the third conduit connecting the gas distributor and the second port of the first conduit. It can quickly cut off or adjust the channel of inert gas flowing to the gas distributor, allowing the operator to independently control the gas supply status of the gas distributor. When it is necessary to pause deoxygenation or change containers, the gas path can be quickly shut off to avoid gas waste or excessive deoxygenation of polymer solutions. At the same time, during the operation of the device, the second ball valve can work with the pressure reducing valve and the first ball valve to achieve multi-stage pressure regulation, ensuring that polymer solutions of different viscosities can complete efficient deoxygenation at a suitable gas flow rate, which significantly improves the adaptability of the device to high-viscosity polymer solutions and the operational flexibility.

[0017] Furthermore, the dissolved oxygen monitoring component includes an online dissolved oxygen detector, the detection end of which extends into the interior of the reactor.

[0018] The beneficial effects of adopting the above technical solution are as follows: The detection end of the online dissolved oxygen detector is inserted into the polymer solution through the top of the reaction vessel, which can continuously collect dissolved oxygen concentration data and feed it back to the control system. This allows operators to dynamically monitor the deoxygenation progress and adjust the inert gas flow rate or stirring parameters in a timely manner, avoiding the oxygen concentration fluctuation error caused by traditional sampling and detection. It is suitable for scenarios where high-viscosity polymer solutions require long-term deoxygenation due to slow gas diffusion, ensuring the accuracy of the deoxygenation endpoint judgment, thereby improving the deoxygenation efficiency and the stability of the polymer solution quality.

[0019] Furthermore, the solution delivery assembly includes a peristaltic pump, the input end of which is connected to the output end of the lower discharge valve via a fourth conduit, the output end of which is connected to the second puncture needle via a fifth conduit, a third puncture needle is provided on one side of the second puncture needle, and the second and third puncture needles are connected to the vial.

[0020] The beneficial effects of adopting the above technical solution are as follows: by utilizing the pulsation-free and low-shear characteristics of the peristaltic pump, the stable transmission of the polymer solution can be ensured; the output end of the peristaltic pump is connected to the second puncture needle through the fifth conduit, and the needle tip of the second puncture needle penetrates below the liquid surface of the vial to inject the polymer solution. At the same time, the third puncture needle is set above the liquid surface of the vial to form a gas channel, effectively balancing the gas pressure of the vial and avoiding bubbles or leakage caused by pressure changes during the transport of the polymer solution. This not only solves the problem of difficult transport of high-viscosity polymer solutions due to poor fluidity, but also ensures the purity and oxygen concentration stability of the polymer solution after deoxygenation by independently controlling the liquid and gas phases through the two puncture needles, thereby improving the packaging efficiency and product quality.

[0021] Furthermore, the discharge valve and the fourth conduit, as well as the peristaltic pump and the fourth and fifth conduits, are all securely connected by clamps.

[0022] The beneficial effects of adopting the above technical solution are as follows: the ring-shaped clamp is detachable and has good sealing performance, which can effectively prevent leakage of high-viscosity polymer solutions during transportation due to pipeline loosening or poor sealing. At the same time, it avoids the viscous polymer solution residue and disassembly difficulties that may be caused by traditional threaded connections. Thus, it not only ensures the stability of oxygen concentration of the deoxygenated polymer solution during the transfer process, but also facilitates regular cleaning and maintenance, improving the reliability of the device operation and long-term efficiency.

[0023] Furthermore, the feed port is equipped with a sealing plug, the vent is connected to the sixth conduit, and the sixth conduit is equipped with a third ball valve.

[0024] The beneficial effects of adopting the above technical solution are as follows: the sealing plug can ensure that the feed port is completely closed when not in operation, effectively preventing external air from seeping into the reactor; and the vent is connected to the third ball valve through the sixth conduit, which allows the gas in the reactor to be discharged separately through the sixth conduit. The third ball valve, as a gas circuit switch, can control the exhaust rate by adjusting the opening to avoid polymer solution splashing, and can also be completely closed after deoxygenation to maintain an inert environment inside the reactor, thereby solving the problem of oxygen concentration rebound caused by insufficient air tightness during the deoxygenation process of high viscosity polymer solution.

[0025] In summary, the beneficial effects of the deoxygenation device for polymer solutions provided by this utility model are as follows: (1) The deoxygenation device integrates a stirring component, a dissolved oxygen monitoring component, a gas supply component and a solution delivery component to form a highly efficient deoxygenation system for high-viscosity polymer solutions. It can realize the entire process operation from pre-deoxygenation of polymer solutions, stirring and dissolving to packaging. Moreover, it can ensure the stability of the deoxygenation process through real-time monitoring and dynamic adjustment, thereby solving the problem of low deoxygenation efficiency of existing deoxygenation technologies for high-viscosity and easily foaming polymer solutions.

[0026] (2) The stirring component in the deoxygenation device achieves full mixing of high viscosity polymer solution through the combination of multi-layer blades and U-shaped stirring paddle. The multi-layer blades ensure uniform stirring of polymer solution in the vertical direction, while the U-shaped stirring paddle extends to the bottom of polymer solution in the reactor, which can effectively break the formed deposit layer or local high viscosity area, and enhance the overall fluidity of polymer solution. Thus, it not only improves deoxygenation efficiency, but is also suitable for polymer solutions containing surfactants or prone to foaming.

[0027] (3) The dissolved oxygen monitoring component in the deoxygenation device extends directly into the polymer solution inside the reactor through the detection end of the online dissolved oxygen detector, realizing real-time and continuous monitoring of dissolved oxygen concentration. This is beneficial for operators to adjust the inert gas flow rate or stirring parameters based on the monitoring data, ensuring the accuracy of the deoxygenation endpoint judgment.

[0028] (4) The gas supply component in the deoxygenation device achieves control of the inert gas flow rate through the coordinated use of the pressure reducing valve, the first ball valve, the second ball valve and the gas distributor. The pressure reducing valve can adjust the gas pressure to avoid the polymer solution splashing due to excessive gas pressure or the deoxygenation effect being affected by insufficient gas pressure. The first ball valve and the second ball valve are used to quickly cut off or restore the gas flow, which is convenient for operators to adjust flexibly according to actual needs. The gas distributor can simultaneously replace multiple vials with inert gas through multiple gas distributor needle valves, which improves the processing efficiency of large-scale deoxygenation of high-viscosity polymer solutions.

[0029] (5) The solution conveying component in the deoxygenation device is connected to the lower discharge valve, which can realize the pollution-free packaging of the polymer solution after deoxygenation. The non-pulsating and low-shear characteristics of the peristaltic pump can ensure the stable transmission of the polymer solution. The output end of the peristaltic pump is connected to the second puncture needle through the fifth conduit. The needle tip of the second puncture needle penetrates below the liquid surface of the vial to inject the polymer solution. At the same time, the third puncture needle is set above the liquid surface of the vial to form a gas channel, which effectively balances the gas pressure of the vial and avoids the generation of bubbles or leakage due to pressure changes during the transport of the polymer solution. This not only solves the problem of difficult transport of high viscosity polymer solutions due to poor fluidity, but also ensures the purity and oxygen concentration stability of the polymer solution after deoxygenation by independently controlling the liquid and gas phases through the two puncture needles, thereby improving the packaging efficiency and product quality. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 This is a schematic diagram showing the connection method and gas flow of the vial on the gas distributor in this utility model; The components include: 1. Gas supply device; 2. Pressure reducing valve; 3. Second ball valve; 4. First ball valve; 5. Third ball valve; 6. Online dissolved oxygen detector; 7. Stirring assembly; 71. Stirring motor; 72. Stirring shaft; 73. Multi-layer impeller; 74. U-shaped stirring impeller; 8. Lower discharge valve; 9. Clamp; 10. Peristaltic pump; 11. Vial; 12. Third puncture needle; 13. Second puncture needle; 14. First puncture needle; 15. Gas distributor needle valve; 16. Gas distributor; 17. First port; 18. Second port; 19. Second conduit; 20. Reactor; 21. Feed port; 22. First conduit; 23. Third conduit; 24. Fourth conduit; 25. Fifth conduit; 26. Sixth conduit; 27. Gas outlet; 28. Gas inlet; 29. ​​Sealing plug; 30. Fourth puncture needle. Detailed Implementation

[0031] The specific embodiments of this utility model are described below to enable those skilled in the art to understand this utility model. However, it should be understood that this utility model is not limited to the scope of the specific embodiments. For those skilled in the art, as long as various changes are within the spirit and scope of this utility model as defined and determined by the appended claims, these changes are obvious. All utility model creations utilizing the concept of this utility model are within the scope of protection.

[0032] Example 1 like Figures 1-2 As shown, the deoxygenation device for polymer solutions provided by this utility model includes a reaction vessel 20. A stirring assembly 7 is installed inside the reaction vessel 20. The top of the reaction vessel 20 is equipped with a dissolved oxygen monitoring assembly, a feed port 21, an air inlet 28, and an air outlet 27. The air outlet 27 is connected to a sixth conduit 26, and a third ball valve 5 is installed on the sixth conduit 26. A sealing plug 29 is installed at the feed port 21. The air inlet 28 is connected to a gas supply assembly. A lower discharge valve 8 is installed at the bottom of the reaction vessel 20 and is connected to a solution conveying assembly. This deoxygenation device for polymer solutions achieves efficient deoxygenation of high-viscosity, easily foaming polymer solutions through the synergistic effect of the inert gas supply assembly, the multi-layer stirring assembly 7, the online dissolved oxygen monitoring assembly, and the solution conveying assembly. It is suitable for polymer solutions containing surfactants and can monitor and control the dissolved oxygen concentration in the polymer solution in real time during the deoxygenation process, improving the deoxygenation effect and the efficiency of polymer solution preparation. The multi-layer stirring assembly 7 inside the reactor 20 can fully mix and stir the polymer solution during the deoxygenation process. It can pre-deoxygenate low-viscosity solvents before adding polymers and continuing stirring, achieving simultaneous polymer dissolution and deoxygenation, which greatly improves deoxygenation efficiency. At the same time, multi-layer stirring can also effectively break up foam on the surface of the polymer solution, making it suitable for polymer solutions containing surfactants or those prone to foaming. The online dissolved oxygen monitoring assembly at the top of the reactor 20 can monitor the dissolved oxygen concentration in real time, ensuring precise control of the deoxygenation process and enabling operators to accurately judge the timing of polymer addition and deoxygenation. The effects are as follows: the air inlet 28 and the inert gas supply component can stably supply inert gas, quickly replace the air in the reactor 20, and effectively reduce the dissolved oxygen concentration; the air outlet 27 can discharge the replaced air and excess gas, maintain the stable gas pressure in the reactor 20, and ensure the safety and effectiveness of the deoxygenation process; in addition, the bottom discharge valve 8 set at the bottom of the reactor 20 is connected to the solution conveying component, which can realize convenient and controllable conveying and packaging of the deoxygenated polymer solution, and can ensure the purity and flow stability of the polymer solution during the conveying process, which is conducive to maintaining a low oxygen concentration state and improving the efficiency and safety of polymer solution preparation.

[0033] like Figure 1As shown, the gas supply assembly includes a gas supply device 1, the output end of which is connected to the input end of a first conduit 22. A pressure reducing valve 2 is provided on the first conduit 22, and a first port 17 is provided on the output end of the first conduit 22. The first port 17 is connected to the input end of a second conduit 19, and the output end of the second conduit 19 is connected to an air inlet 28. The second conduit 19 extends into the interior of the reactor 20, and a first ball valve 4 is provided on the second conduit 19. In use, the output end of the gas supply device 1 is connected to the air inlet 28 of the reactor 20 via the first conduit 22. The pressure reducing valve 2 installed on the first conduit 22 can adjust the gas pressure to avoid the polymer solution splashing due to excessive gas pressure or the deoxygenation efficiency being affected by insufficient gas pressure. The first port 17 of the output end of the first conduit 22 is connected to the input end of the second conduit 19. The second conduit 19 extends into the reactor 20 and is equipped with a first ball valve 4. Through the rapid opening and closing function of the first ball valve 4, the gas flow state can be flexibly controlled. It can maintain a suitable gas flow rate during the deoxygenation process and can quickly cut off the gas path when needed to prevent excessive deoxygenation of the polymer solution or gas waste. This ensures the continuity and stability of the inert gas supply and improves the deoxygenation effect of the high-viscosity polymer solution.

[0034] like Figure 1 and Figure 2 As shown, the gas supply assembly also includes a gas distributor 16. The input end of the gas distributor 16 is connected to the third conduit 23. The third conduit 23 is provided with a second ball valve 3. The third conduit 23 is connected to a second port 18. The second port 18 is located at the output end of the first conduit 22. The output end of the gas distributor 16 is provided with a plurality of gas distributor needle valves 15. The plurality of gas distributor needle valves 15 are respectively connected to the first puncture needle 14. The input end of the gas distributor 16 is connected to the second port 18 of the output end of the first conduit 22 via the third conduit 23. The second ball valve 3 installed on the third conduit 23 can independently control the gas flow to the third conduit 23 of the distributor, realizing rapid switching of the gas supply state. At the same time, the output end of the gas distributor 16 is connected to multiple gas distributor needle valves 15, and each gas distributor needle valve 15 is connected to the first puncture needle 14, so that the operator can simultaneously and accurately introduce inert gas into multiple vials 11 containing polymer solutions. This avoids the problem of low deoxygenation efficiency caused by uneven gas distribution in traditional methods. Furthermore, the individual control of multiple gas distributor needle valves 15 improves the adaptability and operational flexibility of the deoxygenation device for large-scale processing of high-viscosity polymer solutions.

[0035] like Figure 1As shown, the stirring assembly 7 includes a stirring motor 71 and a stirring shaft 72 connected to the output end of the stirring motor 71. The stirring shaft 72 is equipped with multiple layers of impellers 73, and a U-shaped stirring paddle 74 is located at the bottom end of the stirring shaft 72. The stirring motor 71 drives the multiple layers of impellers 73 on the stirring shaft 72 to rotate. The multiple layers of impellers 73 ensure thorough mixing of the polymer solution in the vertical direction, while the U-shaped stirring paddle 74 at the bottom end of the stirring shaft 72 can penetrate deep into the bottom of the polymer solution, effectively breaking up any possible sediment layers or localized high-viscosity areas, enhancing the overall fluidity of the polymer solution, thereby improving the deoxygenation effect and solving the problem of poor treatment effect of existing deoxygenation technologies on high-viscosity polymer solutions.

[0036] like Figure 1 As shown, the dissolved oxygen monitoring component includes an online dissolved oxygen detector 6. The detection end of the online dissolved oxygen detector 6 extends into the interior of the reaction vessel 20, and a sealing rubber ring is provided between the online dissolved oxygen detector 6 and the reaction vessel 20. By inserting the detection end of the online dissolved oxygen detector 6 into the polymer solution from the top of the reaction vessel 20, dissolved oxygen concentration data can be continuously collected and fed back to the control system. This allows operators to dynamically monitor the deoxygenation progress and adjust the inert gas flow rate or stirring parameters in a timely manner, avoiding the oxygen concentration fluctuation errors caused by traditional sampling and detection. It is suitable for scenarios where high-viscosity polymer solutions require long-term deoxygenation due to slow gas diffusion, ensuring the accuracy of deoxygenation endpoint determination, thereby improving deoxygenation efficiency and the stability of polymer solution quality.

[0037] like Figure 1 As shown, the solution delivery assembly includes a peristaltic pump 10. The input end of the peristaltic pump 10 is connected to the output end of the lower discharge valve 8 through a fourth conduit 24. The output end of the peristaltic pump 10 is connected to the second puncture needle 13 through a fifth conduit 25. A third puncture needle 12 is provided on one side of the second puncture needle 13. The second puncture needle 13 and the third puncture needle 12 are connected to the vial 11. In addition, the lower discharge valve 8 and the fourth conduit 24, as well as the peristaltic pump 10 and the fourth conduit 24 and the fifth conduit 25, are all fastened together by clamps 9 made of metal. In use, the peristaltic pump 10's pulsation-free and low-shear characteristics ensure stable delivery of the polymer solution. The output end of the peristaltic pump 10 is connected to the second puncture needle 13 via the fifth conduit 25. The tip of the second puncture needle 13 penetrates below the liquid surface of the vial 11 to inject the polymer solution. At the same time, the third puncture needle 12 is positioned above the liquid surface of the vial 11 to form a gas channel, effectively balancing the gas pressure inside the vial 11 and preventing bubbles or leakage caused by pressure changes during polymer solution delivery. This not only solves the problem of difficult delivery of high-viscosity polymer solutions due to poor fluidity, but also ensures the purity and oxygen concentration stability of the deoxygenated polymer solution by independently controlling the liquid and gas phases through the two puncture needles, thereby improving packaging efficiency and product quality.

[0038] In summary, the deoxygenation device for polymer solutions in this embodiment integrates a stirring assembly 7, a dissolved oxygen monitoring assembly, a gas supply assembly, and a solution delivery assembly, forming a highly efficient deoxygenation system for high-viscosity polymer solutions. It can realize the entire process operation from pre-deoxygenation of polymer solutions, stirring and dissolving to packaging, and can ensure the stability of the deoxygenation process through real-time monitoring and dynamic adjustment, thereby solving the problem of low deoxygenation efficiency of existing deoxygenation technologies for high-viscosity, easily foaming polymer solutions.

[0039] Example 2 Based on Example 1, this embodiment proposes a method for replacing the inert gas in an empty vial 11 using an oxygen removal device based on the polymer solution, specifically including the following steps: S1. Close the first ball valve 4, seal the mouth of vial 11 with a rubber stopper, and press the outside of the rubber stopper with an aluminum cap to ensure the airtightness of vial 11; S2. Insert the first puncture needle 14 on the gas distributor 16 into the bottom of the vial 11. Set a fourth puncture needle 30 on one side of the first puncture needle 14. Insert the fourth puncture needle 30 into the vial 11, and the height of the tip of the fourth puncture needle 30 is higher than the height of the tip of the first puncture needle 14. S3. Open the second ball valve 3 and the gas distributor needle valve 15, and adjust the pressure reducing valve 2 to allow inert gas to enter the vial 11 from the gas supply device 1 through the first conduit 22, the third conduit 23, and the gas distributor 16, replacing the air in the vial 11.

[0040] S4. After the replacement is completed, close the gas distributor needle valve 15 and remove the first puncture needle 14 and the fourth puncture needle 30.

[0041] This replacement method ensures the airtightness of the vial 11 through a double-sealing structure of rubber stopper and aluminum cap. Combined with the synergistic effect of the first puncture needle 14 and the fourth puncture needle 30 on the gas distributor 16, it achieves efficient replacement of air in the vial 11 with inert gas. That is, inert gas is introduced through the first puncture needle 14 and air is discharged through the fourth puncture needle 30, avoiding the problems of uneven gas mixing or residual air in traditional methods. At the same time, by adjusting the pressure reducing valve 2 and the needle valve 15 of the gas distributor, the gas flow rate and replacement time can be precisely controlled to ensure that the oxygen concentration in the vial is reduced to the experimental requirements.

[0042] Example 3 Based on Example 1, this embodiment provides a method for deoxygenating a polymer solution, specifically including the following steps: S1. Equipment preparation: Connect the various structures according to Example 1, and confirm that the reactor 20 and the lower discharge valve 8 are in the closed state; S2. Replace the gas in the reactor 20: Open the first ball valve 4 and the third ball valve 5, adjust the pressure reducing valve 2, so that the inert gas generated by the gas supply device 1 enters the reactor 20 at a flow rate of 0.5 to 2 L / min. The replacement time is 10 min. At the same time as the replacement, open the lower discharge valve 8 to allow some of the inert gas to enter the fourth conduit 24, the fifth conduit 25 and the vial 11 connected to the fifth conduit 25 for pre-replacement. S3. Pre-deoxygenation of polymer solution: Close the lower discharge valve 8, add solvent through the feed port 21, and immerse the added solvent in the second conduit 19. Then turn on the stirring motor 71 and the online dissolved oxygen detector 6, and continuously introduce inert gas until the dissolved oxygen concentration drops to the target value. S4. Adding and dissolving polymer solution: Add high-viscosity polymer and surfactant through feed port 21. After feeding, seal feed port 21 with sealing plug 29. Then, adjust the flow rate of inert gas to 0.1 L / min or intermittently ventilate by adjusting the first ball valve 4 and the third ball valve 5. Stir continuously with stirring component 7 until the polymer is completely dissolved. S5. Polymer solution delivery and packaging: After the dissolved oxygen concentration detected by the online dissolved oxygen detector 6 reaches the standard, keep the first ball valve 4 and the third ball valve 5 open, open the lower discharge valve 8 and the peristaltic pump 10, and deliver the polymer solution to the replacement vial 11. At this time, the second puncture needle 13 is inserted into the vial 11 below the surface of the polymer solution, and the third puncture needle 12 is above the surface of the solution for venting. When the polymer solution level reaches 2 / 3 to 3 / 4 of the solvent in the vial 11, stop delivery, pull out the second puncture needle 13 and the third puncture needle 12, and seal the vial 11. S6. The sealed vial 11 can be reconnected to the gas distributor 16 for short-term deoxygenation via the third puncture needle 12.

[0043] This deoxygenation method for polymer solutions achieves highly efficient deoxygenation of high-viscosity, easily aerated polymer solutions through gas replacement, pre-deoxygenation of the polymer solution, and dynamic stirring and solvent encapsulation. It solves the problem of low deoxygenation efficiency of existing deoxygenation technologies for high-viscosity polymer solutions. Furthermore, real-time dissolved oxygen monitoring and gas regulation ensure the stability of the deoxygenation process, ultimately yielding a polymer solution with an oxygen concentration below 3 ppb. Specifically, step S1, by connecting the various structures according to Example 1 and confirming that the reactor 20 and the lower discharge valve 8 are in the closed state, ensures the initial airtightness and operational safety of the deoxygenation device. This provides a stable operating environment for subsequent gas replacement and polymer solution treatment, avoiding the problem of oxygen concentration rebound due to device leakage, while simplifying the operation process and improving experimental efficiency. Step S2, by opening the first ball valve 4 and the third ball valve 5 and adjusting the pressure reducing valve 2, allows the inert gas to be released at a rate of 0.5–2 ppm. A flow rate of L / min is introduced into the reactor 20, achieving efficient air replacement within the reactor 20. Simultaneously, through the lower discharge valve 8, some inert gas is introduced into the fourth conduit 24, the fifth conduit 25, and the vial 11 connected to the fifth conduit 25 for pre-replacement, preventing an increase in oxygen concentration due to residual air in the vial 11 during the subsequent polymer solution encapsulation process, thereby improving the thoroughness and uniformity of gas replacement. In step S3, after closing the lower discharge valve 8, solvent (such as pure water) is added through the feed port 21, and the stirring motor 71 and online dissolved oxygen detector are turned on. The measuring instrument 6 continuously introduces inert gas until the dissolved oxygen concentration drops to the target value, thus achieving pre-deoxygenation of the solvent. During use, the stirring component 7 enhances the contact efficiency between the gas and the polymer solution. Combined with real-time dissolved oxygen monitoring, this ensures precise control of the initial oxygen concentration of the solvent, providing a low-oxygen environment for subsequent polymer dissolution and deoxygenation, and avoiding a decrease in deoxygenation efficiency due to excessively high solvent oxygen content. In step S4, after adding the high-viscosity polymer and surfactant through the feeding port 21, the feeding port 21 is sealed, and the inert gas flow rate is reduced to 0 by adjusting the first ball valve 4 and the third ball valve 5.Aeration is carried out at a rate of 1 L / min or intermittently, while continuous stirring continues until the polymer is completely dissolved. This dynamic stirring and gas flow rate adjustment achieve uniform deoxygenation of the high-viscosity polymer solution, avoiding the oxygen diffusion difficulties caused by the high viscosity of the polymer solution. Furthermore, if the dissolved oxygen concentration in the reactor 20 increases during the dissolution process, the input of inert gas can be increased by adjusting the first ball valve 4 and the third ball valve 5. If foam is generated during the dissolution process, the stirring speed of the stirring assembly 7 can be adjusted to break up the foam, thereby ensuring the stability of the deoxygenation process and the controllability of the polymer solution quality. In step S5, by keeping the first ball valve 4 and the third ball valve 5 open, the discharge valve 8 and the peristaltic pump 10 are opened to transport the deoxygenated polymer solution to the replaced vial 11, and then through the second puncture needle... The dual-puncture needle structure of needles 13 and 12 enables injection below the liquid surface and venting above the liquid surface. This not only ensures stable transport of the polymer solution but also prevents oxygen concentration rise and bubble generation during polymer solution transport through independent liquid and gas phase channels, ultimately resulting in a polymer solution with stable oxygen concentration. This improves packaging efficiency and product quality. Step S6 selectively reconnects the packaged vial 11 to the gas distributor 16, using needles 12 and 30 for short-term deoxygenation. This further reduces the oxygen concentration of the polymer solution inside the vial 11, ensuring oxygen stability during long-term storage or experimentation. It prevents performance degradation of the polymer solution due to residual oxygen in the vial 11, making it particularly suitable for high-viscosity polymer solutions sensitive to oxygen concentration.

[0044] Example 4 This embodiment, based on Embodiment 3, provides a method for deoxygenation testing of a polymer solution with a viscosity of 1250 mPa•s. Following the deoxygenation method of Embodiment 3, the initial dissolved oxygen concentration was 4000 ppb. After deoxygenation, the online detector showed a decrease in dissolved oxygen concentration to 18 ppb. After packaging, a CHEMetrics micro dissolved oxygen test colorimetric tube was used for retesting, showing a dissolved oxygen concentration of 15–20 ppb. The polymer solution viscosity only decreased from 1250 mPa•s to 1242 mPa•s. Furthermore, by extending the gas replacement time and adjusting the stirring speed in real time, the dissolved oxygen concentration of the polymer solution was further reduced to below 3 ppb. Colorimetric tube testing showed a dissolved oxygen concentration range of 0–2.5 ppb. Therefore, the device in Embodiment 1 and the deoxygenation method in Embodiment 3 effectively remove dissolved oxygen from the polymer solution without affecting its viscosity, thus significantly improving the deoxygenation effect of high-viscosity polymer solutions.

Claims

1. A deoxygenation device for a polymer solution, characterized in that: The reactor includes a reaction vessel (20), which is equipped with a stirring assembly (7) inside. The top of the reaction vessel (20) is equipped with a dissolved oxygen monitoring assembly, a feed port (21), an air inlet (28) and an air outlet (27). The air inlet (28) is connected to a gas supply assembly. The bottom of the reaction vessel (20) is equipped with a bottom discharge valve (8), which is connected to a solution conveying assembly.

2. The deoxygenation device for polymer solution according to claim 1, characterized in that: The stirring assembly (7) includes a stirring motor (71) and a stirring shaft (72) connected to the output end of the stirring motor (71). The stirring shaft (72) is provided with multiple layers of blades (73), and a U-shaped stirring paddle (74) is provided at the bottom end of the stirring shaft (72).

3. The deoxygenation device for polymer solution according to claim 1, characterized in that: The gas supply assembly includes a gas supply device (1), the output end of which is connected to the input end of a first conduit (22), the output end of which is provided with a first port (17), the first port (17) is connected to the input end of a second conduit (19), the output end of which is connected to an air inlet (28), and the second conduit (19) extends into the interior of the reactor (20).

4. The deoxygenation device for polymer solution according to claim 3, characterized in that: The first conduit (22) is equipped with a pressure reducing valve (2), and the second conduit (19) is equipped with a first ball valve (4).

5. The deoxygenation device for polymer solution according to claim 3, characterized in that: The gas supply assembly also includes a gas distributor (16), the input end of which is connected to a third conduit (23), the third conduit (23) is connected to a second port (18), the second port (18) is located at the output end of the first conduit (22); the output end of the gas distributor (16) is provided with a plurality of gas distributor needle valves (15), and the plurality of gas distributor needle valves (15) are respectively connected to the first puncture needle (14).

6. The deoxygenation device for polymer solution according to claim 5, characterized in that: A second ball valve (3) is provided on the third conduit (23).

7. The deoxygenation device for polymer solution according to claim 1, characterized in that: The dissolved oxygen monitoring component includes an online dissolved oxygen detector (6), the detection end of which extends into the interior of the reactor (20).

8. The deoxygenation device for polymer solution according to claim 1, characterized in that: The solution delivery assembly includes a peristaltic pump (10), the input end of which is connected to the output end of the lower discharge valve (8) via a fourth conduit (24), and the output end of which is connected to a second puncture needle (13) via a fifth conduit (25). A third puncture needle (12) is provided on one side of the second puncture needle (13), and the second puncture needle (13) and the third puncture needle (12) are connected to a vial (11).

9. The deoxygenation device for polymer solution according to claim 1, characterized in that: The lower discharge valve (8) and the fourth conduit (24) are fastened together by clamps (9) as are the peristaltic pump (10) and the fourth conduit (24) and the fifth conduit (25).

10. The deoxygenation device for polymer solution according to claim 1, characterized in that: The feeding port (21) is provided with a sealing plug (29), the air outlet (27) is connected to the sixth conduit (26), and the sixth conduit (26) is provided with a third ball valve (5).

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