An interfacial polymerization method and apparatus for phase change microcapsules applied to cashmere fibers
Patent Information
- Application Number
- CN202611356415.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-09-03
- Publication Date
- 2026-10-30
AI Technical Summary
现有界面聚合法制备相变微胶囊通常在搅拌釜中进行,油相滴加入水相后,在旋转离心力作用下被甩向釜壁,导致釜底中心区域形成涡流盲区,物料在此处轴向流动极慢,几乎不参与主体循环,靠近釜壁的流体受壁面摩擦阻力影响,流速骤降,导致釜壁中上部会形成流体滑移层,导致油相液滴在此处停留时间过长,发生粘壁或聚并,虽然提高转速能增强湍流,将死区中的物料拽出来,但强行提速带来的极高剪切应力会直接撕裂乳化剂形成的界面膜,导致液滴发生聚并,且强剪切力还可能会直接击穿或剥离初生壳体,造成芯材泄漏,为此,我们提出一种应用于羊绒纤维的相变微胶囊的界面聚合方法及设备
1、本发明利用电机带动转盘转动,转盘带动转轴与搅拌杆进行圆周运动,通过往复螺槽与导向块的配合,转盘将一边转动一边进行上下往复运动,再通过齿轮与齿环的配合,转轴与搅拌杆将一边进行圆周运动一边进行自转,同时还将进行上下往复运动,提高对水相中油相的搅拌效率,促进相变微胶囊的形成,且搅拌的同时反应釜中的水流将进行无规则流动与碰撞,消除釜壁与釜底处的流动死区,使油相与水相的界面聚合反应更加彻底,且无需过高转速,防止产生过高的剪切力而影响界面聚合反应;
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Figure CN122999086A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of interfacial polymerization technology, specifically to an interfacial polymerization method and apparatus for phase change microcapsules applied to cashmere fibers. Background Technology
[0002] Phase change microcapsules are a type of smart material for thermal energy management. Their structure consists of two layers: a core material and a wall material. The core material is usually a phase change material such as paraffin or fatty acids, which can absorb or release a large amount of latent heat through solid-liquid transition at a specific temperature. The wall material is a stable polymer film that tightly wraps the core material to prevent leakage. Applying phase change microcapsules to cashmere involves attaching them to the fiber surface or embedding them inside the fiber. Their core function is to give cashmere intelligent temperature control, upgrading it from an ordinary thermal insulation product to an intelligent textile that actively regulates temperature. Interfacial polymerization is one of the most commonly used methods for preparing microcapsules. Its principle is that two highly reactive monomers are dissolved in water and an organic solvent, respectively, and a polymerization reaction occurs at the interface of the two liquids, instantly forming a film that encapsulates the core material. Existing interfacial polymerization methods for preparing phase change microcapsules are typically carried out in a stirred tank. After the oil phase droplets are added to the aqueous phase, they are thrown towards the tank wall under the action of centrifugal force, resulting in a vortex blind zone in the central region of the tank bottom. The material flows very slowly axially in this area and hardly participates in the main circulation. The fluid near the tank wall is affected by the frictional resistance of the wall surface, and the flow velocity drops sharply, resulting in the formation of a fluid slip layer in the upper part of the tank wall. This causes the oil phase droplets to stay in this area for too long, resulting in wall adhesion or agglomeration. Although increasing the rotation speed can enhance turbulence and pull the material out of the dead zone, the extremely high shear stress brought about by the forced acceleration can directly tear the interfacial film formed by the emulsifier, causing droplet agglomeration. Moreover, the strong shear force may also directly penetrate or peel off the nascent shell, causing core material leakage. To address this, we propose an interfacial polymerization method and equipment for phase change microcapsules of cashmere fibers. Summary of the Invention
[0003] The purpose of this invention is to provide an interfacial polymerization method and apparatus for phase change microcapsules applied to cashmere fibers, so as to solve the problems mentioned in the background art.
[0004] To achieve the above objectives, the present invention provides the following technical solution: an interfacial polymerization device for phase change microcapsules of cashmere fibers, comprising a reactor, a reactor cover fixedly installed on the upper end of the reactor, an inlet provided on the upper end of the reactor cover, a discharge outlet provided at the bottom of the reactor, a plurality of heating rings fixedly installed in the inner wall of the reactor for heating, an oil storage tank for holding the oil phase provided on one side of the reactor, a flow pump for conveying the oil phase fixedly installed at the bottom of the oil storage tank, an oil inlet hole provided on the inner wall of the reactor, and an oil delivery pipe fixedly connected between the output end of the flow pump and the oil inlet hole; A motor is fixedly installed on the upper end of the vessel lid. A turntable is provided at the output end of the motor. Several rotating shafts are rotatably installed on the lower end of the turntable. The rotating shafts are arranged in a circle. Several stirring rods are fixedly installed on each rotating shaft. A sleeve is fixedly installed on the lower end of the vessel lid. A reciprocating screw groove is provided on the inner wall of the sleeve. A guide block that mates with the reciprocating screw groove is fixedly installed on the outer ring of the turntable. A gear ring is fixedly installed on the inner wall of the sleeve. The height of the gear ring is greater than the height of the reciprocating screw groove. A gear that meshes with the gear ring is fixedly installed on each rotating shaft.
[0005] Preferably, the reactor is provided with a baffle to prevent liquid from splashing upwards. Each of the rotating shafts is rotatably connected to the baffle. A scraper for scraping off the oil phase on the inner wall of the reactor is fixedly installed at the lower end of the baffle. The scraper is arranged in a ring and abuts against the inner wall of the reactor.
[0006] Preferably, a plurality of rotating rings are rotatably mounted on the lower end of the baffle, and each rotating ring corresponds to a rotating shaft. Each rotating ring is sleeved on the corresponding rotating shaft, and a plurality of scrapers for scraping off the oil phase at the lower end of the baffle are fixedly mounted on each rotating ring. Each scraper is inclined and its upper end abuts against the lower end of the baffle.
[0007] Preferably, each of the rotating shafts is fitted with a sliding ring, which is located below the rotating ring. Each of the rotating shafts is fixedly installed with a plurality of guide strips for limiting the sliding ring. The density of each sliding ring is less than that of the aqueous phase. Each sliding ring is fixedly installed with a plurality of push plates at its upper end. Each rotating ring is fixedly installed with a plurality of baffles that cooperate with the push plates at its lower end. The push plates and baffles correspond one-to-one.
[0008] Preferably, when the guide block moves to the lowest end of the reciprocating screw groove, the baffle is located on the movement trajectory of the push plate, and the lower surface of the baffle plate is flush with the liquid surface in the reactor.
[0009] Preferably, a plurality of rubber rings are fixedly installed on the baffle plate. The rubber rings are funnel-shaped, wider at the top and narrower at the bottom, and the bottom of the rubber rings is located on the movement trajectory of the scraper.
[0010] Preferably, the oil inlet is located at the bottom of the reactor, a slide cylinder is slidably installed inside the oil inlet, a cover plate for sealing the oil inlet is provided on the top of the slide cylinder, and a plurality of outlet holes for releasing the oil phase are arranged in a ring on the slide cylinder.
[0011] Preferably, a liquid distribution rod is fixedly installed at the lower end of the cover plate. The liquid distribution rod is located inside the slide cylinder, and its lower end is set in an arc shape.
[0012] Preferably, the stirring rods on each of the rotating shafts are arranged in multiple rows of spirals.
[0013] An interfacial polymerization method for phase change microcapsules applied to cashmere fibers specifically includes the following steps: S1. Select appropriate raw materials to prepare aqueous and oil phases according to requirements, and inject the aqueous and oil phases into the reactor and oil storage tank respectively; S2. Start the flow pump to inject the oil phase in the oil storage tank into the reactor at a constant speed. The oil phase pushes the cover plate and slide cylinder upward, and after being dispersed by the arc surface of the uniform liquid rod, it flows into the reactor through the liquid outlet. S3. Start the motor. Through the cooperation of the reciprocating screw groove and the guide block, as well as the cooperation of the gear and the gear ring, the turntable drives the rotating shaft and the stirring rod to perform circular motion, rotation and up-down reciprocating motion, so as to efficiently stir the oil phase in the aqueous phase and promote the formation of phase change microcapsules. S4. The baffle intercepts the splashed oil and water phases. When the baffle descends to be level with the liquid surface, the baffle enters the push plate movement trajectory. The sliding ring drives the rotating ring to rotate, and the scraper scrapes off the oil phase adhering to the lower end of the baffle. S5. The rotating scraper generates water flow to flush the bottom of the baffle and the inner wall of the scraper. The scraper presses against the lower end of the rubber ring to close its hole, preventing the oil phase from entering the hole, and at the same time scrapes off the oil phase adhering to the lower surface of the rubber ring. S6. After the oil phase is fully introduced, continue to stir and heat to ensure that the wall material is fully cured and to prevent adhesion and agglomeration when the wall material is not fully cured, until the reaction is complete. S7. After the reaction is complete, cool the mixture and separate the microcapsules by centrifugation. Wash the microcapsules repeatedly with deionized water and ethanol to remove impurities, and finally dry them to obtain phase change microcapsules.
[0014] Compared with the prior art, the beneficial effects of the present invention are: 1. This invention utilizes a motor to drive a turntable to rotate, which in turn drives a rotating shaft and a stirring rod to perform circular motion. Through the cooperation of a reciprocating screw groove and a guide block, the turntable will rotate and perform up-and-down reciprocating motion simultaneously. Furthermore, through the cooperation of a gear and a gear ring, the rotating shaft and the stirring rod will perform circular motion and rotation simultaneously, as well as up-and-down reciprocating motion, thereby improving the stirring efficiency of the oil phase in the aqueous phase, promoting the formation of phase change microcapsules, and simultaneously causing the water flow in the reactor to flow and collide irregularly, eliminating the flow dead zones at the reactor wall and bottom, making the interfacial polymerization reaction between the oil phase and the aqueous phase more thorough, and without the need for excessively high rotation speed, preventing the generation of excessive shear force that would affect the interfacial polymerization reaction; 2. This invention utilizes a rotating shaft to drive the baffle and scraper to rotate while reciprocating up and down. When the guide block has not moved to the bottom of the reciprocating screw groove, the baffle is located above the liquid surface in the reactor, and the baffle's descent height is insufficient, so the baffle is not on the trajectory of the push plate. When the guide block moves to the bottom of the reciprocating screw groove, the baffle's descent height is sufficient, and the baffle will be on the trajectory of the push plate. The sliding ring will drive the push plate, baffle, and rotating ring to rotate together, and the scraper will perform a circular motion. The direction of the scraper's rotation is opposite to the direction of the baffle's movement, which facilitates the scraper to remove the oil phase adhering to the lower end of the baffle. At this time, the lower surface of the baffle is flush with the liquid surface in the reactor. The oil phase scraped off by the scraper will be integrated into the aqueous phase to continue the interfacial polymerization reaction. At the same time, the rotation of the scraper will also generate water flow to flush the bottom of the baffle and the inner wall of the scraper, preventing the oil phase from adhering to the baffle and the scraper. Attached Figure Description
[0015] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram of the electrothermal ring structure of the present invention; Figure 3 This is a schematic diagram of the internal structure of the reactor of the present invention; Figure 4 For the present invention Figure 3 Enlarged schematic diagram of the structure of region A in the middle; Figure 5 This is a schematic diagram of the slide cylinder and liquid distribution rod structure of the present invention; Figure 6 This is a schematic diagram of the internal structure of the sleeve of the present invention; Figure 7 For the present invention Figure 6 Enlarged schematic diagram of the structure of region B in the middle; Figure 8 This is a schematic diagram of the rotating ring and sliding ring structure of the present invention; Figure 9 For the present invention Figure 8 Enlarged schematic diagram of the structure of region C in the middle; Figure 10 This is a schematic diagram of the rubber ring structure of the present invention.
[0016] In the diagram: 1. Reactor; 2. Reactor lid; 3. Feed inlet; 4. Discharge outlet; 5. Heating ring; 6. Oil storage tank; 7. Flow pump; 8. Oil delivery pipe; 9. Oil inlet; 10. Cover plate; 11. Sliding cylinder; 12. Liquid outlet; 13. Uniform rod; 14. Motor; 15. Turntable; 16. Rotating shaft; 17. Stirring rod; 18. Guide block; 19. Gear; 20. Sleeve; 21. Gear ring; 22. Reciprocating screw groove; 23. Baffle plate; 24. Scraper; 25. Rotating ring; 26. Scraper; 27. Baffle; 28. Sliding ring; 29. Guide bar; 30. Push plate; 31. Rubber ring. Detailed Implementation
[0017] 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 some embodiments of the present invention, and not all embodiments. 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.
[0018] Please see Figure 1-10 This invention provides a technical solution: an interfacial polymerization device for phase change microcapsules of cashmere fibers, comprising a reactor 1, a reactor cover 2 fixedly installed on the upper end of the reactor 1, an inlet 3 provided on the upper end of the reactor cover 2, a discharge outlet 4 provided at the bottom of the reactor 1, several heating rings 5 fixedly installed in the inner wall of the reactor 1 for heating, an oil storage tank 6 for holding the oil phase provided on one side of the reactor 1, a flow pump 7 for conveying the oil phase fixedly installed at the bottom of the oil storage tank 6, an oil inlet 9 provided on the inner wall of the reactor 1, an oil delivery pipe 8 fixedly connected between the output end of the flow pump 7 and the oil inlet 9, the oil inlet 9 being located at the bottom of the reactor 1, a sliding cylinder 11 slidably installed inside the oil inlet 9, a cover plate 10 for sealing the oil inlet 9 provided on the top of the sliding cylinder 11, several outlet holes 12 for releasing the oil phase arranged in a ring on the sliding cylinder 11, and a liquid equalization rod 13 fixedly installed at the lower end of the cover plate 10. The uniform liquid rod 13 is located inside the slide cylinder 11, and its lower end is set in an arc shape. The flow pump 7 can draw out the oil phase from the oil storage tank 6 and apply a certain pressure. The oil phase is injected into the reactor 1 at a constant speed through the oil delivery pipe 8 and the oil inlet hole 9. When the oil phase is not injected, the pressure generated by the water phase in the reactor 1 pushes the cover plate 10 and the slide cylinder 11 downward, so that the cover plate 10 blocks the oil inlet hole 9. When the oil phase passes through the oil inlet hole 9, it pushes the cover plate 10 and the slide cylinder 11 upward. After passing through the arc surface of the uniform liquid rod 13, the oil phase flows evenly to the surrounding liquid outlet holes 12 and flows into the reactor 1 through the liquid outlet holes 12. The water phase flowing in the reactor 1 separates the oil phase into small droplets, and then the oil phase floats in the water phase. Since the oil inlet hole 9 is located at the bottom of the reactor 1, the oil phase floats a long distance and has enough time to react with the water phase, which facilitates the formation of phase change microcapsules and improves the efficiency of the interfacial polymerization reaction.
[0019] A motor 14 is fixedly installed on the upper end of the vessel lid 2. A turntable 15 is provided at the output end of the motor 14. Several rotating shafts 16 are rotatably installed on the lower end of the turntable 15. The rotating shafts 16 are arranged in a circle, and several stirring rods 17 are fixedly installed on each rotating shaft 16. The stirring rods 17 on each rotating shaft 16 are arranged in multiple rows of spirals. A sleeve 20 is fixedly installed on the lower end of the vessel lid 2. A reciprocating spiral groove 22 is provided on the inner wall of the sleeve 20. A guide block 18 that mates with the reciprocating spiral groove 22 is fixedly installed on the outer ring of the turntable 15. A gear ring 21 is fixedly installed on the inner wall of the sleeve 20. The height of the gear ring 21 is greater than the height of the reciprocating spiral groove 22. A gear 19 that meshes with the gear ring 21 is fixedly installed on each rotating shaft 16. After the motor 14 is started, it will drive the turntable 15 to rotate continuously. The turntable 15 will drive the rotating shafts 16 and stirring rods 17 to perform circular motion, passing through the reciprocating spiral groove 22. In conjunction with the guide block 18, the turntable 15 will rotate and reciprocate up and down. At the same time, since the height of the gear ring 21 is greater than the height of the reciprocating screw groove 22, the gear 19 and the gear ring 21 will always remain meshed. Through the cooperation of the gear 19 and the gear ring 21, the rotating shaft 16 and the stirring rod 17 will rotate in a circular motion and rotate on their own axis, while also reciprocating up and down, improving the stirring efficiency of the oil phase in the aqueous phase and promoting the formation of phase change microcapsules. Since the stirring rod 17 is arranged in multiple spiral rows, the water flow it generates can push the oil phase downward, slowing down the upward floating speed of the oil phase. At the same time, the water flow in the reactor 1 will flow and collide irregularly, eliminating the flow dead zone at the reactor wall and bottom, making the interfacial polymerization reaction between the oil phase and the aqueous phase more thorough, and without the need for excessively high rotation speed, to prevent excessive shear force from affecting the interfacial polymerization reaction.
[0020] The reactor 1 is equipped with a baffle 23 to prevent liquid from splashing upwards. Each rotating shaft 16 is rotatably connected to the baffle 23. A scraper 24 for scraping the oil phase on the inner wall of the reactor 1 is fixedly installed at the lower end of the baffle 23. The scraper 24 is arranged in a ring and abuts against the inner wall of the reactor 1. Several rotating rings 25 are rotatably installed at the lower end of the baffle 23. Each rotating ring 25 corresponds to one rotating shaft 16. Each rotating ring 25 is sleeved on the corresponding rotating shaft 16. Several scrapers 26 for scraping the oil phase at the lower end of the baffle 23 are fixedly installed on each rotating ring 25. Each scraper 26 is inclined and its upper end abuts against the lower end of the baffle 23. A sliding ring 28 is sleeved on each rotating shaft 16 and is located below the rotating ring 25. Several scrapers 28 are fixedly installed on each rotating shaft 16. A guide bar 29 is used to limit the sliding ring 28. The density of each sliding ring 28 is less than that of the aqueous phase. Several push plates 30 are fixedly installed on the upper end of each sliding ring 28, and several baffles 27 that cooperate with the push plates 30 are fixedly installed on the lower end of each rotating ring 25. The push plates 30 and baffles 27 correspond one-to-one. When the guide block 18 moves to the lowest end of the reciprocating screw groove 22, the baffles 27 are located on the movement trajectory of the push plates 30, and the lower surface of the baffle plate 23 is flush with the liquid surface in the reactor 1. Since the rotating shaft 16 performs a circular motion and a reciprocating motion, the baffle plate 23 and the scraper 24 will also rotate and perform a reciprocating motion. The rotating ring 25 and the scraper 24 will also perform a reciprocating motion along with the baffle plate 23. Since the sliding ring 28 is denser than the aqueous phase, the guide bar 29 is fixedly installed on the upper end of each sliding ring 28, and the baffles 29 are fixedly installed on the lower end of each sliding ring 28. The guide bar 29 is used to limit the ... Since the density of the liquid phase is less than that of the aqueous phase, the sliding ring 28 will always maintain the same height. When the guide block 18 has not moved to the bottom of the reciprocating screw groove 22, the baffle 23 is located above the liquid surface in the reactor 1. The baffle 23 does not descend sufficiently, and the baffle 27 is not located on the movement trajectory of the push plate 30. The sliding ring 28 and the push plate 30 rotate synchronously with the rotating shaft 16, while the rotating ring 25 and the scraper 26 do not rotate, reducing the wear between the scraper 26 and the baffle 23. Since the water flow in the reactor 1 will have irregular flow and collision, the oil phase floating to the surface of the aqueous phase is easily splashed by the water flow collision and adheres to the inner wall of the reactor 1 and the lower surface of the baffle 23. The baffle 23 can prevent the oil phase from splashing into the sleeve 20 and being difficult to remove. At the same time, the baffle 23 drives the scraper 24 to move up and down. During the process, the oil phase adhering to the inner wall of the reactor 1 can be scraped off. When the guide block 18 moves to the bottom of the reciprocating screw groove 22, the baffle 23 descends to a sufficient height, and the baffle 27 will be located on the movement trajectory of the push plate 30. The sliding ring 28 will drive the push plate 30, the baffle 27, and the rotating ring 25 to rotate together. The scraper 26 will perform a circular motion, and the rotation direction of the scraper 26 is opposite to the movement direction of the baffle 23, which facilitates the scraper 26 to scrape off the oil phase adhering to the lower end of the baffle 23. At this time, the lower surface of the baffle 23 is flush with the liquid surface in the reactor 1. The oil phase scraped off by the scraper 26 will be integrated into the aqueous phase to continue the interfacial polymerization reaction. At the same time, the rotation of the scraper 26 will also generate water flow to flush the bottom of the baffle 23 and the inner wall of the scraper 24, preventing the oil phase from adhering to the baffle 23 and the scraper 24.The lower end of the baffle 23 is not always flush with the liquid surface to prevent the baffle 23 and scraper 24 from continuously affecting the water flow and causing uneven mixing of the oil phase at the water phase surface. Several rubber rings 31 are fixedly installed on the baffle 23. The rubber rings 31 are funnel-shaped, wider at the top and narrower at the bottom. The bottom of the rubber rings 31 is located on the movement trajectory of the scraper 26. After the water phase is injected into the reactor 1 through the feed port 3, it will fall onto the baffle 23 and generate a certain pressure to make the rubber rings 31 expand downward, so that the water phase can pass through the rubber rings. The central hole of the rubber ring 31 allows the water phase to pass through, and the elasticity of the rubber ring 31 restores the hole. When the oil phase splashes, it is difficult for it to pass directly through the small hole of the rubber ring 31. The bottom of the rubber ring 31 is located on the movement trajectory of the scraper 26. During the rotation of the scraper 26, it will press against the lower end of the rubber ring 31 and lift it upward, closing the bottom hole of the rubber ring 31 and preventing the scraper 26 from scraping the oil phase into the hole of the rubber ring 31. At the same time, the oil phase adhering to the lower surface of the rubber ring 31 will be scraped off by the scraper 26.
[0021] Specifically, firstly, the prepared aqueous phase is injected into the reactor 1 through the feed inlet 3. The aqueous phase falls onto the baffle plate 23, generating a certain pressure that causes the rubber ring 31 to expand downwards, facilitating the passage of the aqueous phase through the central hole of the rubber ring 31. After the aqueous phase passes through, the elasticity of the rubber ring 31 allows the hole to return to its original state. Then, the flow pump 7 extracts the oil phase from the oil storage tank 6 and applies a certain pressure. The oil phase is injected into the reactor 1 at a constant speed through the oil delivery pipe 8 and the oil inlet 9. When the oil phase passes through the oil inlet 9, it pushes the cover plate 10 and the slide cylinder 11 upwards. After passing through the arc surface of the uniform liquid rod 13, the oil phase flows evenly to the surrounding liquid outlets 12 and flows into the reactor through the liquid outlets 12. Inside reactor 1, the flowing aqueous phase separates the oil phase into small droplets, which then float to the surface of the aqueous phase. Heating ring 5 is energized during the reaction to maintain the temperature within reactor 1 within a suitable range. Simultaneously, motor 14 starts, driving turntable 15 to rotate continuously. Turntable 15 drives shaft 16 and stirring rod 17 in circular motion, while also reciprocating up and down. Shaft 16 and stirring rod 17 simultaneously rotate and reciprocate, improving the stirring efficiency of the oil phase within the aqueous phase and promoting the formation of phase change microcapsules. During stirring, the water flow in reactor 1 is continuously... Regular flow and collisions eliminate dead zones in the flow at the vessel wall and bottom. The rotating ring 25 and scraper 24 reciprocate up and down together with the baffle 23. When the guide block 18 has not moved to the bottom of the reciprocating spiral groove 22, the baffle 23 is above the liquid surface in the reactor 1, and the baffle 23's descent height is insufficient. The baffle 27 is not on the trajectory of the push plate 30, and the rotating ring 25 and scraper 26 do not rotate. When the guide block 18 moves to the bottom of the reciprocating spiral groove 22, the baffle 23's descent height is sufficient, and the baffle 27 will be on the trajectory of the push plate 30. The sliding ring 28 will drive the push plate 30, baffle 27, and rotating ring 25 to rotate together, and the scraper 26 will rotate in a circular motion. During the rotation of the scraper 26, the oil phase adhering to the lower end of the baffle 23 is scraped off. At this time, the lower surface of the baffle 23 is flush with the liquid surface in the reactor 1. The oil phase scraped off by the scraper 26 will be integrated into the aqueous phase to continue the interfacial polymerization reaction. At the same time, the rotation of the scraper 26 will also generate water flow to wash the bottom of the baffle 23 and the inner wall of the scraper 24. When the oil phase splashes, it is difficult to pass directly through the small holes of the rubber ring 31. During the rotation of the scraper 26, it will press against the lower end of the rubber ring 31 and lift it upward, so that the bottom hole of the rubber ring 31 is closed, preventing the scraper 26 from scraping the oil phase into the hole of the rubber ring 31. At the same time, the oil phase adhering to the lower surface of the rubber ring 31 will be scraped off by the scraper 26.
[0022] An interfacial polymerization method for phase change microcapsules applied to cashmere fibers specifically includes the following steps: S1. Select appropriate raw materials to prepare aqueous and oil phases according to requirements, and inject the aqueous and oil phases into reactor 1 and oil storage tank 6 respectively; S2. Start the flow pump 7 to inject the oil phase in the oil storage tank 6 into the reactor 1 at a constant speed. The oil phase pushes the cover plate 10 and the slide cylinder 11 upwards. After being dispersed by the arc surface of the uniform liquid rod 13, it flows into the reactor 1 through the liquid outlet 12. S3. Start the motor 14. Through the cooperation of the reciprocating screw groove 22 and the guide block 18, and the cooperation of the gear 19 and the gear ring 21, the turntable 15 drives the rotating shaft 16 and the stirring rod 17 to perform circular motion, rotation and up-down reciprocating motion, so as to efficiently stir the oil phase in the aqueous phase and promote the formation of phase change microcapsules. S4. The baffle 23 intercepts the splashed oil and water phases. When the baffle 23 descends to be level with the liquid surface, the baffle 27 enters the movement trajectory of the push plate 30, the sliding ring 28 drives the rotating ring 25 to rotate, and the scraper 26 scrapes off the oil phase adhering to the lower end of the baffle 23. S5. The rotating scraper 26 generates water flow to flush the bottom of the baffle 23 and the inner wall of the scraper 24. The scraper 26 presses against the lower end of the rubber ring 31 to close its hole, preventing the oil phase from entering the hole, and at the same time scrapes off the oil phase adhering to the lower surface of the rubber ring 31. S6. After the oil phase is fully introduced, continue to stir and heat to ensure that the wall material is fully cured and to prevent adhesion and agglomeration when the wall material is not fully cured, until the reaction is complete. S7. After the reaction is complete, cool the mixture and separate the microcapsules by centrifugation. Wash the microcapsules repeatedly with deionized water and ethanol to remove impurities, and finally dry them to obtain phase change microcapsules.
[0023] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
[0024] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. An interfacial polymerization apparatus for phase change microcapsules of cashmere fibers, comprising a reactor (1) and a lid (2) fixedly installed on the upper end of the reactor (1), characterized in that: The upper end of the lid (2) is provided with a feed inlet (3), the bottom of the reactor (1) is provided with a discharge outlet (4), a number of heating rings (5) are fixedly installed in the inner wall of the reactor (1), an oil storage tank (6) for holding the oil phase is provided on one side of the reactor (1), a flow pump (7) for conveying the oil phase is fixedly installed at the bottom of the oil storage tank (6), an oil inlet hole (9) is provided on the inner wall of the reactor (1), and an oil delivery pipe (8) is fixedly connected between the output end of the flow pump (7) and the oil inlet hole (9). A motor (14) is fixedly installed on the upper end of the lid (2). A turntable (15) is provided at the output end of the motor (14). Several rotating shafts (16) are rotatably installed on the lower end of the turntable (15). The rotating shafts (16) are arranged in a circle. Several stirring rods (17) are fixedly installed on each rotating shaft (16). A sleeve (20) is fixedly installed on the lower end of the lid (2). A reciprocating screw groove (22) is provided on the inner wall of the sleeve (20). A guide block (18) that cooperates with the reciprocating screw groove (22) is fixedly installed on the outer ring of the turntable (15). A toothed ring (21) is fixedly installed on the inner wall of the sleeve (20). The height of the toothed ring (21) is greater than the height of the reciprocating screw groove (22). A gear (19) that meshes with the toothed ring (21) is fixedly installed on each rotating shaft (16).
2. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 1, characterized in that: The reactor (1) is provided with a baffle (23) to prevent liquid from splashing upwards. Each of the rotating shafts (16) is rotatably connected to the baffle (23). A scraper (24) for scraping off the oil phase on the inner wall of the reactor (1) is fixedly installed at the lower end of the baffle (23). The scraper (24) is arranged in a ring and abuts against the inner wall of the reactor (1).
3. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 2, characterized in that: The lower end of the baffle (23) is rotatably mounted with several rotating rings (25). Each rotating ring (25) corresponds to a rotating shaft (16). Each rotating ring (25) is sleeved on the corresponding rotating shaft (16). Each rotating ring (25) is fixedly mounted with several scrapers (26) for scraping off the oil phase at the lower end of the baffle (23). Each scraper (26) is inclined and its upper end abuts against the lower end of the baffle (23).
4. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 3, characterized in that: Each of the rotating shafts (16) is fitted with a sliding ring (28), which is located below the rotating ring (25). Each of the rotating shafts (16) is fixedly installed with several guide strips (29) for limiting the sliding ring (28). The density of each sliding ring (28) is less than that of water. Each of the sliding rings (28) is fixedly installed with several push plates (30) at the upper end. Each of the rotating rings (25) is fixedly installed with several baffles (27) that cooperate with the push plates (30) at the lower end. The push plates (30) and the baffles (27) correspond one-to-one.
5. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 4, characterized in that: When the guide block (18) moves to the lowest end of the reciprocating screw groove (22), the baffle (27) is located on the movement trajectory of the push plate (30), and the lower surface of the baffle plate (23) is flush with the liquid surface in the reactor (1).
6. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 5, characterized in that: Several rubber rings (31) are fixedly installed on the baffle (23). The rubber rings (31) are funnel-shaped with a wider top and a narrower bottom. The bottom of the rubber rings (31) is located on the movement trajectory of the scraper (26).
7. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 6, characterized in that: The oil inlet (9) is located at the bottom of the reactor (1). A slide cylinder (11) is slidably installed inside the oil inlet (9). A cover plate (10) for sealing the oil inlet (9) is provided on the top of the slide cylinder (11). Several outlet holes (12) for releasing the oil phase are arranged in a ring on the slide cylinder (11).
8. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 7, characterized in that: A liquid distribution rod (13) is fixedly installed at the lower end of the cover plate (10). The liquid distribution rod (13) is located inside the slide cylinder (11), and its lower end is set in an arc shape.
9. The interfacial polymerization apparatus for phase change microcapsules of cashmere fibers according to claim 8, characterized in that: The stirring rods (17) on each of the said rotating shafts (16) are arranged in multiple spiral rows.
10. An interfacial polymerization method for phase change microcapsules applied to cashmere fibers, characterized in that: The interfacial polymerization method using the interfacial polymerization equipment for phase change microcapsules of cashmere fibers as described in claim 9 specifically includes the following steps: S1. Select appropriate raw materials to prepare aqueous and oil phases according to requirements, and inject the aqueous and oil phases into the reactor (1) and oil storage tank (6) respectively; S2. Start the flow pump (7) to inject the oil phase in the oil storage tank (6) into the reactor (1) at a constant speed. The oil phase pushes the cover plate (10) and the slide cylinder (11) upward. After being dispersed by the arc surface of the uniform liquid rod (13), it flows into the reactor (1) through the liquid outlet (12). S3. Start the motor (14). Through the cooperation of the reciprocating screw groove (22) and the guide block (18) and the gear (19) and the gear ring (21), the turntable (15) drives the rotating shaft (16) and the stirring rod (17) to perform circular motion, rotation and up-down reciprocating motion, so as to efficiently stir the oil phase in the aqueous phase and promote the formation of phase change microcapsules. S4. The baffle (23) intercepts the splashed oil and water phases. When the baffle (23) descends to be level with the liquid surface, the baffle (27) enters the movement trajectory of the push plate (30), the sliding ring (28) drives the rotating ring (25) to rotate, and the scraper (26) scrapes off the oil phase adhering to the lower end of the baffle (23). S5. The rotating scraper (26) generates water flow to flush the bottom of the baffle (23) and the inner wall of the scraper (24). The scraper (26) presses against the lower end of the rubber ring (31) to close its hole, preventing the oil phase from entering the hole, and at the same time scrapes off the oil phase adhering to the lower surface of the rubber ring (31). S6. After the oil phase is fully introduced, continue to stir and heat to ensure that the wall material is fully cured and to prevent adhesion and agglomeration when the wall material is not fully cured, until the reaction is complete. S7. After the reaction is complete, cool the mixture and separate the microcapsules by centrifugation. Wash the microcapsules repeatedly with deionized water and ethanol to remove impurities, and finally dry them to obtain phase change microcapsules.
