A nanocomposite polymer brush production device
By integrating magnetron plasma activation, continuous polymerization in honeycomb microchannels, and acoustic-fluid resonance separation into a nanocomposite polymer brush production system, the problems of low surface activation efficiency and low purity in the preparation of nanocomposite polymer brushes have been solved, realizing efficient, green, and continuous production of nanocomposite polymer brushes to meet the high-efficiency drag reduction requirements of well workover fluids in oil and gas fields.
Patent Information
- Application Number
- CN202511456379.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-13
- Publication Date
- 2026-02-03
- Estimated Expiration
- 2045-10-13
AI Technical Summary
Existing nanocomposite polymer brush preparation processes suffer from problems such as low surface activation efficiency, uneven grafting density, wide molecular weight distribution, low purity, and difficulty in achieving continuous production. These issues result in unstable drag reduction effects, making it difficult to meet the high-efficiency and green engineering requirements of oil and gas field workover fluids.
A nanocomposite polymer brush production system integrating magnetron plasma activation, continuous polymerization in a honeycomb microchannel, and acoustic-flow resonance separation is adopted. The nanoparticles are activated by a coaxial magnetron plasma reactor, polymerized in a honeycomb microchannel reactor, separated by an acoustic-flow resonance separation tower, and purified by a spray drying molding machine.
It achieves efficient surface activation, increased grafting density, and product purity of over 99% for nanocomposite polymer brushes, supports 24-hour continuous production, reduces energy consumption, and meets the high-efficiency and green requirements of oil and gas field workover fluids.
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Figure CN120919940B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of nanomaterial manufacturing equipment technology, specifically to a nanocomposite polymer brush production device. Background Technology
[0002] Workover fluid is an indispensable functional fluid in oil and gas field workover and wellbore maintenance operations. Its main functions include carrying cuttings, lubricating tools, stabilizing the wellbore, and preventing wellbore damage. With the increasing number of deep, ultra-deep, and challenging wells, more stringent requirements are being placed on the drag reduction performance, carrying capacity, and environmental adaptability of workover fluids. During workover operations, complex friction and resistance exist between the workover fluid and the wellbore wall, downhole tools, and cuttings surfaces. Insufficient drag reduction can easily lead to increased operational energy consumption, tool jamming, wellbore collapse, and other engineering risks, affecting operational safety and efficiency.
[0003] Currently, drag-reducing agents for well workover fluids mostly utilize traditional materials such as polymers, surfactants, or nanoparticles. However, polymers suffer from entangled molecular chains and poor dispersibility, leading to a decline in drag-reducing effects in extreme downhole environments such as high temperature and high salinity. While surfactants can improve fluid lubrication to some extent, their temperature resistance and durability are insufficient. Nanoparticles, due to their large specific surface area and high interfacial activity, are introduced into well workover fluid systems, but they tend to agglomerate and settle in high-salt and high-temperature environments, resulting in limited compatibility with the base fluid and unstable drag-reducing effects. Furthermore, existing drag-reducing agent preparation processes mostly involve intermittent chemical initiation or low-temperature plasma treatment, resulting in low density and uneven distribution of surface active groups in the products, as well as high levels of impurities, making it difficult to achieve low-energy consumption, high-efficiency, and continuous large-scale production.
[0004] Nanocomposite polymer brushes are interfacial functional materials with uniformly grafted polymer chains onto the surface of nanoparticles, possessing a "rigid core-flexible brush" structure. In workover fluids, they not only form a dense lubricating layer at the interface between the wellbore, tools, and cuttings, significantly reducing fluid friction, but also effectively inhibit cuttings agglomeration and improve carrying and cleaning capabilities. Related studies have shown that the steric hindrance and brush layer overlap of polymer brushes can maintain a super-lubricated state in harsh downhole environments, significantly superior to traditional drag-reducing agent systems. However, their large-scale application is limited by the activation efficiency, grafting density, and separation and purification levels of current preparation processes. Specifically, existing nanocomposite polymer brush drag-reducing agent technologies generally suffer from the following bottlenecks:
[0005] 1. Low surface activation efficiency and uneven distribution of active sites result in limited grafting density of the brush layer and unstable drag reduction effect.
[0006] 2. The graft polymerization process suffers from imprecise temperature control and a wide molecular weight distribution, making it difficult to achieve the requirements of high uniformity and high purity products.
[0007] 3. Traditional separation and purification methods are energy-intensive, result in significant product loss, have low recovery rates of effective drag-reducing agents, and exhibit large performance fluctuations between batches.
[0008] 4. The lack of continuous and intelligent production processes makes it difficult to meet the engineering requirements of modern oil and gas field workover fluids for high efficiency, greenness, and stability.
[0009] Therefore, there is an urgent need for a nanocomposite polymer brush production equipment with efficient surface activation, high uniformity polymerization, low energy consumption, high purity separation, and continuous production capabilities to promote the large-scale application of high-performance well workover fluid drag reducers. Summary of the Invention
[0010] Therefore, the purpose of this invention is to provide a nanocomposite polymer brush production device, which integrates magnetron plasma activation, continuous polymerization of honeycomb microchannels and acoustic-fluid resonance separation into a nanocomposite polymer brush production system. This system enables the continuous preparation of high-activity, high-purity, and low-cost drag-reducing materials for well workover fluids, providing strong technical support for the safety and efficiency of well workover operations in oil and gas fields.
[0011] To solve at least one of the above-mentioned technical problems, the technical solution provided by the present invention is:
[0012] A nanocomposite polymer brush production device comprises multiple production units connected by a transport mechanism, wherein the production unit includes:
[0013] Coaxial magnetron plasma reactor for activating nanoparticles;
[0014] A honeycomb microchannel reactor, used for the full reaction of nanoparticles and monomers, includes a honeycomb microchannel reactor body, a reactor inlet pipe, honeycomb cells, a liquid injection pump, a semiconductor temperature control plate, thermocouples, microchannel pores, a reactor outlet pipe, and a heat dissipation plate. The honeycomb microchannel reactor body is a hollow box-type structure, on which the reactor inlet pipe and reactor outlet pipe are installed. The liquid injection pump is installed on the reactor inlet pipe. Multiple sets of honeycomb cells are arrayed inside the honeycomb microchannel reactor body. The honeycomb cells are hollow, sealed containers with microchannel pores. Thermocouples and semiconductor temperature control plates are respectively installed on the outer surface of the honeycomb cells.
[0015] An acoustic-fluid resonance separation tower for separating nanopolymer brushes includes a separation tower inlet, a separation chamber, an Archimedes spiral channel, ultrasonic transducers, a heavy phase outlet, and a light phase outlet. The separation chamber, a downward-facing hollow cone, is vertically mounted on the tower base. Its bottom constricted section connects to an external container via the heavy phase outlet. A light phase outlet, also a constricted hollow cone, is located at the top of the separation chamber. An Archimedes spiral channel extending upwards is positioned on the outer surface of the separation chamber. The inlet at the bottom of the spiral channel connects to the separation tower inlet, while its top outlet extends into the separation chamber and points towards the light phase outlet. Multiple sets of ultrasonic transducers are spaced along the outer surface of the spiral channel.
[0016] Spray dryer for purifying nanopolymer brushes.
[0017] One embodiment of the present invention is that the coaxial magnetron plasma reactor includes a plasma reactor body, an air inlet, a double-layer quartz tube, an inner electrode, an outer electrode, a nanoparticle inlet, a magnetic field coil, and a discharge port. The sidewall of the plasma reactor body is a double-layer quartz tube, and an inner electrode is disposed inside it. An outer electrode is arranged in a mesh around the inner electrode. A magnetic field coil is disposed around the outside of the double-layer quartz tube. The plasma reactor body is provided with an air inlet and a discharge port at the bottom. A nanoparticle inlet is radially disposed on the surface of the double-layer quartz tube.
[0018] One embodiment of the present invention is that the spray drying forming device includes a forming tower, an emulsion inlet, a centrifugal atomizing disc, a hot air system, a fluidized bed cooler, a product outlet, and an exhaust port. The emulsion inlet and the hot air system are provided at the top of the forming tower, the centrifugal atomizing disc is provided inside the forming tower, the exhaust port is provided on the inner surface of the forming tower below the centrifugal atomizing disc, the product outlet is provided at the bottom of the forming tower, and the fluidized bed cooler with the exhaust port facing upward is also provided at the bottom of the forming tower.
[0019] Furthermore, the outlet of the fluidized cooler is angled upwards, and its axis can intersect with the axis of the product outlet.
[0020] One embodiment of the present invention is that a heat dissipation plate is provided on the honeycomb microchannel reactor body, the honeycomb unit array is arranged on the heat dissipation plate, the heat dissipation plate is connected to the semiconductor temperature control sheet, and the heat dissipation plate can transfer heat to the outside of the honeycomb microchannel reactor body.
[0021] One embodiment of the present invention is that an electrostatic demister is also provided at the outlet of the light phase.
[0022] One embodiment of the present invention is that the distance between adjacent ultrasonic transducers is 20 mm, the phase difference is 90°, the operating frequency of a single ultrasonic transducer is 40 kHz, and the power density is 2 W / cm².
[0023] One embodiment of the present invention is that the cross-section of the Archimedes spiral channel has a width of 2.0 mm and a depth of 1.0 mm, and the fluid velocity therein is 1.0 m / s.
[0024] One embodiment of the present invention is that a guide lip is provided at the outlet of the topmost part of the Archimedes spiral channel. The guide lip includes a guide lip inlet, a light phase outlet, and a heavy phase outlet. The guide lip inlet is connected to the outlet of the topmost part of the Archimedes spiral channel. The light phase outlet points to the light phase outlet, and the heavy phase outlet does not point to the light phase outlet. The guide lip inlet, the light phase outlet, and the heavy phase outlet are interconnected, thereby forming a γ-shaped branch channel inside the guide lip. The heavy phase outlet is located on one side of the outer end surface of the Archimedes spiral channel.
[0025] The technical effects achieved by this invention are:
[0026] (1) The present invention can achieve efficient surface activation of nanomaterials, which significantly improves the grafting density. Furthermore, the use of magnetron plasma to activate nanoparticles can effectively improve the density of the grafting polymerization initiation point and significantly enhance the compactness and stability of the polymer brush.
[0027] (2) The present invention introduces a honeycomb microchannel reactor, combined with a plasma micro-source and a precise temperature control system, to achieve rapid start-up and constant temperature control of the polymerization reaction, uniform transfer of plasma free radicals, high surface grafting efficiency, and high and uniform polymer brush density.
[0028] (3) This invention achieves the directional migration and enrichment of brush layer nanoparticles through the synergistic effect of sound field and Dean eddy current, without the need for additional fluidization equipment. Combined with electrostatic demister, it achieves liquid-solid separation and impurity removal, and the final product purity can reach over 99%.
[0029] (4) The present invention adopts full-process modular integration, supports 24-hour continuous operation, avoids the energy and material waste caused by frequent start-up and shutdown of traditional batch process; and the monomers and solvents that do not participate in the reaction are recycled through multi-level purification and reuse system to reduce waste liquid discharge.
[0030] (5) This invention surpasses existing technologies in terms of temperature control, reaction efficiency, material circulation, safety and environmental protection. It has high overall energy efficiency, and the product has a uniform brush layer structure and high purity. It provides a reliable technical solution for the large-scale green and intelligent preparation of nanocomposite polymer brushes. Attached Figure Description
[0031] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.
[0032] Figure 1 This is a schematic diagram of the coaxial magnetron plasma reactor in this invention;
[0033] Figure 2 This is a schematic diagram of the honeycomb microchannel reactor in this invention;
[0034] Figure 3 This is a schematic diagram of the acoustic-fluid resonance separation tower in this invention;
[0035] Figure 4 This is a schematic diagram of the spray drying forming device in this invention;
[0036] Figure 5 This is a schematic diagram of the structure of the cellular unit in this invention;
[0037] Figure 6 This is a top view of the separation cavity in this invention;
[0038] Figure 7 This is a schematic diagram of the flow guide lip in this invention;
[0039] In the diagram: 1-Plasma reactor body, 2-Air inlet, 3-Double-layer quartz tube, 4-Inner electrode, 5-Outer electrode, 6-Nanoparticle inlet, 7-Magnetic field coil, 8-Outlet, 9-Honeycomb microchannel reactor body, 10-Reactor inlet pipe, 11-Honeycomb unit, 12-Liquid injection pump, 13-Semiconductor temperature control plate, 14-Thermocouple, 15-Microchannel pore, 16-Reactor outlet pipe, 17-Heat dissipation plate, 18-Separation tower inlet, 19-Separation chamber, 20-Archimedes spiral flow channel 21-Ultrasonic transducer, 22-Electrostatic demister, 23-Heavy phase outlet, 24-Light phase outlet, 25-Forming tower, 26-Emulsion inlet, 27-Centrifugal atomizing disc, 28-Hot air system, 29-Fluidized cooler, 30-Product outlet, 31-Exhaust port, 32-Guide lip, 321-Guide lip inlet, 322-Light phase outlet, 323-Heavy phase outlet, 324-Light phase outlet flow extension line, 325-Heavy phase outlet flow extension line, 326-Angle of flow extension line. Detailed Implementation
[0040] The present invention will be further described in detail below with reference to the embodiments and accompanying drawings.
[0041] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention.
[0042] Example
[0043] A nanocomposite polymer brush production device consists of multiple production units connected by a transport mechanism. The transport mechanism can refer to conventional transport mechanisms in the prior art, such as conveyor belts, material pipes with conveying pumps, or other transfer equipment with material transfer capabilities.
[0044] The production unit includes:
[0045] Coaxial magnetron plasma reactor for activating nanoparticles, see [link / reference]. Figure 1 The coaxial magnetron plasma reactor in this embodiment includes a plasma reactor body 1, an air inlet 2, a double-layer quartz tube 3, an inner electrode 4, an outer electrode 5, a nanoparticle inlet 6, a magnetic field coil 7, and a discharge port 8. The sidewall of the plasma reactor body 1 is a double-layer quartz tube 3, inside which an inner electrode 4 is disposed. An outer electrode 5 surrounds the inner electrode 4 in a mesh pattern to generate plasma. The inner electrode 4 can be a molybdenum rod, and the outer electrode 5 is made of copper. The magnetic field coil 7 is disposed around the outside of the double-layer quartz tube 3 to apply a magnetic field to control the plasma, thereby forming a plasma activation zone. The plasma reactor body 1 is provided with an air inlet 2 to introduce the excited gas, which can be oxygen, helium, or a combination thereof. A discharge port 8 is provided at the bottom. A nanoparticle inlet 6 is radially disposed on the surface of the double-layer quartz tube 3. The nanoparticles enter the reaction interior from here through gas-solid suspension or airflow carrying and are activated in the plasma activation zone. The activated nanoparticles are collected at the discharge port 8 at the bottom.
[0046] The activated nanoparticles are fed into the honeycomb microchannel reactor by the transport mechanism and mixed with the remaining reactants and solvents for reaction. The method of adding reactants can refer to existing technologies. For example, when the transport mechanism is a pipeline, it can be mixed by a specially set mixing feeder on the pipeline, or it can be mixed externally and then fed into the honeycomb microchannel reactor.
[0047] The structure of the honeycomb microchannel reactor is as follows Figure 2As shown, the reactor used for polymer brush preparation reaction includes a honeycomb microchannel reactor body 9, a reactor inlet pipe 10, honeycomb units 11, a liquid injection pump 12, a semiconductor temperature control plate 13, a thermocouple 14, microchannel holes 15, a reactor outlet pipe 16, and a heat dissipation plate 17. The honeycomb microchannel reactor body 9 is a hollow box structure with the reactor inlet pipe 10 and the reactor outlet pipe 16 mounted on it. The liquid injection pump 12, which can be a screw pump, provides power to the feed, thereby precisely controlling the amount of feed and ensuring sufficient contact and dispersion of the reactants. The product after the reaction is completed is discharged through the reactor outlet pipe 16. Multiple sets of honeycomb units 11 are arrayed inside the honeycomb microchannel reactor body 9. (See [reference]). Figure 5 The honeycomb cell 11 is a hollow, sealed container with microchannel holes 15. Thermocouples 14 and semiconductor temperature control plates 13 are respectively disposed on the outer surface of the honeycomb cell 11. Two sets of microchannel holes 15 can be arranged opposite each other on the honeycomb cell 11. Fluid entering the honeycomb cell 11 will generate turbulence inside the honeycomb cell 11 due to changes in the flow channel, ensuring sufficient contact and mixing between the reactants, thereby significantly improving the reaction effect. After the reaction is complete, the fluid will move out of the honeycomb cell 11 with the liquid flow. Thermocouples 14 are used for real-time monitoring of the temperature in the honeycomb cell 11, while semiconductor temperature control plates 13 transmit signals through a semiconductor... The body heat effect precisely controls the temperature in each honeycomb cell 11. In this embodiment, a heat sink 17 is also provided on the honeycomb microchannel reactor body 9, and the honeycomb cells 11 are arrayed on the heat sink 17. The heat sink 17 is connected to the semiconductor temperature control plate 13, and the heat sink 17 can transfer heat to the outside of the honeycomb microchannel reactor body 9. The heat sink 17 can replace one side wall of the honeycomb microchannel reactor. The other end of the semiconductor temperature control plate 13 can be set to contact the heat sink 17, thereby transferring heat out of the honeycomb microchannel reactor and preventing it from accumulating in the honeycomb cells 11, which would cause changes in the reaction temperature. The thermocouple 14 and the semiconductor temperature control plate 13 can be uniformly electrically connected to an external central control system, referring to the prior art. The thermocouple 14 monitors the real-time temperature in the honeycomb cells 11, and the central control system controls the semiconductor temperature control plate 13 to adjust the temperature, ensuring that the temperature in each honeycomb cell 11 is maintained under suitable reaction temperature conditions, promoting the efficient progress of the polymer brush preparation reaction.
[0048] See Figure 3 , Figure 6The acoustic-fluid resonance separation tower is used for the separation and initial purification of nanopolymer brushes. The mixed product stream generated by the aforementioned reaction includes nanopolymer brushes, unreacted monomers, solvents, and other substances, which need to be separated. The separation tower includes a separation tower inlet 18, a separation chamber 19, an Archimedes spiral flow channel 20, an ultrasonic transducer 21, a heavy phase outlet 23, and a light phase outlet 24. The separation chamber 19 is vertically arranged on the base of the separation tower. The separation chamber 19 is a downward-facing hollow cone, and its bottom narrowed section can be connected to an external container through the heavy phase outlet 23. The top is provided with a light phase outlet 24, which is a hollow cone with a narrowed top diameter. An Archimedean spiral channel 20 extending upwards is provided on the outer surface of the separation chamber 19. The inlet at the bottom of the Archimedean spiral channel 20 is connected to the separation tower inlet 18, and its top outlet extends into the separation chamber 19 and points towards the light phase outlet 24. Multiple sets of ultrasonic transducers 21 are spaced along the outer surface of the Archimedean spiral channel 20. The separation tower inlet 18 at the bottom of the separation tower can be pumped into the mixed product stream via a transport mechanism. The mixed product stream flows along the Archimedean... The Archimedean spiral channel 20 spirals upwards, generating Dean vortices during this upward movement. Simultaneously, as the mixed product stream ascends, multiple sets of ultrasonic transducers 21, spaced apart on the outer surface of the Archimedean spiral channel 20, radiate sound. Nanopolymer brush particles with a density greater than that of the fluid are pushed towards the point of maximum sound pressure (antinode), while the solvent and molecular-level substances are almost unaffected, thus initiating initial separation within the Archimedean spiral channel 20. When the mixed product stream reaches the outlet at the very top of the Archimedean spiral channel 20, the nanopolymer brush particles... A significant velocity difference exists between the particles (heavy phase) and the remaining molecular-level substances in the solution—the heavy phase component is squeezed against the inner wall of the Archimedes spiral channel 20, where it aggregates, while the light phase remains fluidized. When the mixed product flows out of the top outlet, the heavy phase, due to its larger weight and volume, has a larger contact area with the channel and is easily blocked or jammed, unable to rise continuously. Upon entering the separation chamber 19, it quickly falls due to its own gravity and is collected at the heavy phase outlet 23. The light phase, without agglomeration, maintains its fluidized state well and can move at high speed along the direction of the top outlet to the top light phase outlet 24, and is discharged from the separation tower at the top of the outlet. During this process, the light phase is further captured by the electrostatic demister 22, which may carry extremely fine particles or droplets, allowing the light phase to be recovered and recycled for subsequent preparations, thus achieving effective collection of the nanopolymer brush.
[0049] In some embodiments, a guide lip 32 is provided at the outlet of the Archimedes spiral channel 20 at its highest point, see [reference needed]. Figure 7The guide lip 32 includes a guide lip inlet 321, a light phase outlet 322, and a heavy phase outlet 323. The guide lip inlet 321 is connected to the outlet at the top of the Archimedes spiral channel 20. The light phase outlet 322 points to the light phase outlet 24, while the heavy phase outlet 323 does not point to the light phase outlet 24. The guide lip inlet 321, the light phase outlet 322, and the heavy phase outlet 323 are interconnected, thereby forming a γ-shaped branch channel inside the guide lip 32. The heavy phase outlet 323 is located on one side of the outer end surface of the Archimedes spiral channel 20, that is, on the same side as the ultrasonic transducer 21. When the mixed product stream enters the guide lip 32 along the guide lip inlet 321, the heavy phase component is squeezed against the wall close to the inner side of the Archimedes spiral channel 20. During the flow, it will naturally enter the heavy phase outlet 323 and move away from the light phase outlet 24, eventually falling into the bottom of the separation chamber 19. The light phase in the mixed product stream will flow in the direction of least resistance - that is, it will be discharged along the light phase outlet 322 towards the light phase outlet 24, and enter the light phase outlet 24 with a high velocity, thereby further improving the separation effect of the heavy and light phases.
[0050] Preferred, Figure 7 The angle 326 formed between the extended flow lines 324 of the light phase outlet and 325 of the heavy phase outlet shown should be no less than 45°. Since the light phase outlet 322 points to the light phase outlet 24, in this case, the heavy phase outlet 323 and the light phase outlet 24 will have a significant angle, and the γ-shaped branch will have a larger area, making it easier for the heavy phase to collide with it. In this way, even if a few heavy phases may be drawn out from the light phase outlet 322 with the light phase flow, they will lose most of their kinetic energy due to the collision with the γ-shaped branch in advance, thus making it easier for them to decelerate and fall into the bottom of the separation chamber 19. This ensures that the γ-shaped flow channel inside the guide lip 32 can fully separate the light and heavy phases.
[0051] Preferably, in this embodiment, the ultrasonic transducers 21 are spaced 20mm apart and have a phase difference of 90°, thereby establishing a stable and controllable complete ultrasonic standing wave field inside the flow channel.
[0052] The operating frequency of a single ultrasonic transducer 21 is preferably 40 kHz, and the power density is preferably 2 W / cm², which is sufficient to generate significant acoustic radiation force on nanoparticles.
[0053] The Archimedes spiral channel 20 has a cross-sectional width of 2.0 mm and a depth of 1.0 mm, with a fluid velocity of 1.0 m / s. The channel rises around the bottom, providing ample reaction distance for the physical field. At the same time, the cross-sectional dimensions of the channel also provide sufficient space to separate the light and heavy phases, giving the fluid and particles enough room to move. When the fluid velocity is controlled at 1.0 m / s, the Dean vortex has the strongest sorting effect. Meanwhile, the fluid kinetic energy at the outlet is insufficient to resist the downward pull of gravity on the heavy phase, which is the key to optimizing and generating a strong and stable Dean vortex.
[0054] In some embodiments, the bottom cone angle of the separation chamber 19 is 60°, and the material of the inner surface lining is a smooth, inert material, such as polytetrafluoroethylene.
[0055] See Figure 4 A spray dryer for purifying nanopolymer brushes includes a forming tower 25, an emulsion inlet 26, a centrifugal atomizing disc 27, a hot air system 28, a fluidized bed cooler 29, a product outlet 30, and an exhaust port 31. The forming tower 25 is equipped with an emulsion inlet 26 and a hot air system 28 at its top. The nanopolymer brushes separated by the acoustic-fluid resonance separation tower are transported to the spray dryer for further purification via a transport mechanism. At this point, the heavy phase is a high-concentration solution formed by the nanopolymer brush particles and the fluid surrounding them, which is fed into the spray dryer through the emulsion inlet 26 at the top. The hot air system 28 and the emulsion inlet 26 at the top of the spray dryer are aligned downwards. The hot air system 28 can be a hot air generator from the prior art, so that the high-concentration solution is gradually heated during the descent.
[0056] The forming tower 25 is equipped with a centrifugal atomizing disc 27. The centrifugal atomizing disc 27 can accept the falling high-concentration solution and continuously centrifuge and eject the high-concentration solution, inertially separating the solid and liquid phases. At this time, the high temperature will cause the liquid phase to vaporize, ensuring that most of the solid phase, i.e., the nano polymer brush, continues to fall.
[0057] An exhaust port 31 is provided on the inner surface of the forming tower 25 below the centrifugal atomizing disc 27. The product outlet 30 is located at the bottom of the forming tower 25. A fluidizing cooler 29 with an upward-facing exhaust port is also provided at the bottom of the forming tower 25. The separated nanopolymer brushes continuously fall to the product outlet 30. During this process, the fluidizing cooler 29 will continuously blow out cold air upwards, carrying the vaporized liquid phase away from the forming tower 25 through the exhaust port 31, and continuously drying the surface of the nanopolymer brushes, thereby ensuring that dry and pure nanopolymer brushes can be obtained at the product outlet 30.
[0058] In some embodiments, the outlet of the fluidized bed cooler 29 is angled upwards, such as... Figure 4As shown, its axis can intersect with the axis of the product outlet 30, and while blowing out cold air upwards, it can also gather the nano-polymer brush towards the product outlet 30.
[0059] Based on this, the method of using the nanocomposite polymer brush production device includes the following steps:
[0060] Step S1: Nanoparticles (such as SiO2 nanoparticles) are introduced into a coaxial magnetron plasma reactor and activated by plasma excited by oxygen and helium. Under pulsed power supply excitation, helium and oxygen generate a large amount of atomic oxygen and excited-state helium in the discharge chamber, providing a highly efficient activation environment for the surface of SiO2 nanoparticles. The pulsed power supply frequency is 5~30kHz, the pulse width is 1~20μs, and the voltage is 5~15kV, preferably 10kHz frequency, 5μs pulse width, and 8kV. The SiO2 nanoparticles pass uniformly through the plasma zone in a gas flow manner, and the inert silyl ether bonds on their surface are broken, significantly increasing the hydroxyl density and creating abundant active sites for subsequent grafting reactions.
[0061] Step S2: The activated SiO2 nanoparticles are transported to the honeycomb microchannel reactor via a transport mechanism. During transport, the SiO2 nanoparticles are mixed with reactants (such as acrylamide (AM) and styrene-maleic anhydride copolymer (SMA) in a 7:3 ratio) in a specific ratio to form a precursor solution. The solution passes through the honeycomb unit 11 in the honeycomb microchannel reactor, where the particles and monomers are in full contact. The temperature control system of the reaction zone integrates a semiconductor temperature control chip 13 and a thermocouple 14 to achieve precise temperature control, greatly reducing branching or structural defects caused by local overheating. The product has a uniform brush layer structure, and the polymerization efficiency and conversion rate are significantly improved. The crude product is obtained by fully reacting in the honeycomb unit 11 and discharged from the reactor outlet pipe 16. The reaction time is between 35 and 45 min, and the reaction temperature is between 65 and 70 °C, preferably 70 °C, with a reaction time of 40 min.
[0062] Step S3: The crude product is transported to the acoustic-fluid resonance separation tower via a transport mechanism. Power is applied to make the crude product move upward from the inlet 18 of the separation tower along the Archimedes spiral channel 20. In the channel, the light and heavy phases are initially separated due to the influence of ultrasonic vibration. The light and heavy phases are further completely separated at the top of the Archimedes spiral channel 20. The heavy phase discharged from the heavy phase outlet 23 is collected.
[0063] Step S4: The heavy phase is transported to the spray dryer via a transport mechanism. The centrifugal atomizing disc 27 atomizes the material into micron-sized droplets. The hot air at the top of the tower contacts the droplets in the same direction to achieve instantaneous surface drying. Gradual cooling is performed until the internal moisture is removed, avoiding damage to the brush layer structure. This allows the heavy phase powder to cool rapidly and maintain excellent dispersibility, resulting in a nanocomposite polymer brush product.
[0064] Therefore, by introducing a honeycomb microchannel reactor into the nanocomposite polymer brush production device and the above steps in this invention, efficient grafting can be achieved on the polymer surface, ensuring the quality of polymer brush preparation. At the same time, the polymer brush nanoparticles and impurities are creatively separated by the synergistic effect of acoustic field and Dean eddy current, realizing the directional migration and enrichment of brush layer nanoparticles, which significantly improves the purity of the final product. Thus, a brand-new device is provided that can efficiently and effectively prepare nanocomposite polymer brushes.
[0065] In the description of this invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. They should not be construed as limitations on this invention.
[0066] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the embodiments of the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A nanocomposite polymer brush production device, characterized in that, It consists of multiple production units connected by a transport mechanism, wherein the production unit includes: Coaxial magnetron plasma reactor for activating nanoparticles; A honeycomb microchannel reactor, used for fully reacting nanoparticles and monomers, includes a honeycomb microchannel reactor body (9), a reactor inlet pipe (10), honeycomb units (11), a liquid injection pump (12), a semiconductor temperature control plate (13), a thermocouple (14), microchannel pores (15), a reactor outlet pipe (16), and a heat dissipation plate (17). The honeycomb microchannel reactor body (9) is a hollow box structure, on which the reactor inlet pipe (10) and the reactor outlet pipe (16) are provided. The liquid injection pump (12) is provided on the reactor inlet pipe (10). Multiple sets of honeycomb units (11) are arranged in an array inside the honeycomb microchannel reactor body (9). The honeycomb unit (11) is a hollow sealed container, on which microchannel pores (15) are provided. Thermocouples (14) and semiconductor temperature control plates (13) are respectively provided on the outer surface of the honeycomb unit (11). An acoustic-fluid resonance separation tower for separating nanopolymer brushes includes a separation tower inlet (18), a separation chamber (19), an Archimedes spiral channel (20), an ultrasonic transducer (21), a heavy phase outlet (23), and a light phase outlet (24). The separation chamber (19) is vertically arranged on the base of the separation tower. The separation chamber (19) is a downward-facing hollow cone. Its bottom narrowed section can be connected to an external container through the heavy phase outlet (23). The top of the separation chamber (19) is provided with a light phase outlet (24) that is a hollow cone with a narrowed top diameter. An Archimedes spiral channel (20) extending from bottom to top is provided on the outer surface of the separation chamber (19). The inlet at the bottom of the Archimedes spiral channel (20) is connected to the separation tower inlet (18), and its top outlet extends into the interior of the separation chamber (19) and points to the light phase outlet (24). Multiple sets of ultrasonic transducers (21) are spaced along the channel on the outer surface of the Archimedes spiral channel (20). Spray dryer for purifying nanopolymer brushes; The Archimedes spiral channel (20) has a cross-sectional width of 2.0 mm and a depth of 1.0 mm, and the fluid velocity within it is 1.0 m / s. At the top outlet of the Archimedes spiral channel (20), a guide lip (32) is provided. The guide lip (32) includes a guide lip inlet (321), a light phase outlet (322), and a heavy phase outlet (323). The guide lip inlet (321) is connected to the top outlet of the Archimedes spiral channel (20). The light phase outlet (322) points to the light phase outlet (24), while the heavy phase outlet (323) does not point to the light phase outlet (24). The guide lip inlet (321), the light phase outlet (322), and the heavy phase outlet (323) are interconnected, thereby forming a γ-shaped branch channel inside the guide lip (32). The heavy phase outlet (323) is located on one side of the outer end surface of the Archimedes spiral channel (20).
2. The nanocomposite polymer brush production device according to claim 1, characterized in that: The coaxial magnetron plasma reactor includes a plasma reactor body (1), an air inlet (2), a double-layer quartz tube (3), an inner electrode (4), an outer electrode (5), a nanoparticle inlet (6), a magnetic field coil (7), and a discharge port (8). The side wall of the plasma reactor body (1) is a double-layer quartz tube (3), and an inner electrode (4) is provided inside it. The outer electrode (5) surrounds the inner electrode (4) in a mesh. The magnetic field coil (7) is provided around the outside of the double-layer quartz tube (3). The plasma reactor body (1) is provided with an air inlet (2) and a discharge port (8) is provided at the bottom. The nanoparticle inlet (6) is radially provided on the surface of the double-layer quartz tube (3).
3. The nanocomposite polymer brush production device according to claim 1, characterized in that: The spray drying molding machine includes a molding tower (25), an emulsion inlet (26), a centrifugal atomizing disc (27), a hot air system (28), a fluidized bed cooler (29), a product outlet (30), and an exhaust port (31). The molding tower (25) is provided with an emulsion inlet (26) and a hot air system (28) at the top. The molding tower (25) is provided with a centrifugal atomizing disc (27) inside. An exhaust port (31) is provided on the inner surface of the molding tower (25) below the centrifugal atomizing disc (27). The product outlet (30) is provided at the bottom of the molding tower (25). A fluidized bed cooler (29) with an upward-facing exhaust port is also provided at the bottom of the molding tower (25).
4. The nanocomposite polymer brush production device according to claim 3, characterized in that: The outlet of the fluidized cooler (29) is set at an angle upward, and its axis can intersect with the axis of the product outlet (30).
5. The nanocomposite polymer brush production device according to claim 1, characterized in that: The honeycomb microchannel reactor body (9) is provided with a heat dissipation plate (17), and the honeycomb units (11) are arrayed on the heat dissipation plate (17). The heat dissipation plate (17) is connected to the semiconductor temperature control plate (13), and the heat dissipation plate (17) can transfer heat to the outside of the honeycomb microchannel reactor body (9).
6. The nanocomposite polymer brush production device according to claim 1, characterized in that: An electrostatic demister (22) is also provided at the light phase outlet (24).
7. The nanocomposite polymer brush production device according to claim 1, characterized in that: The adjacent ultrasonic transducers (21) are spaced 20 mm apart, have a phase difference of 90°, and operate at a frequency of 40 kHz with a power density of 2 W / cm².
Citation Information
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