A purification device for preparing fluorinated liquid crystal monomers

Abstract

The present invention belongs to the technical field of purification of fluorinated liquid crystal monomers, and in particular to a purification device for preparing fluorinated liquid crystal monomers. In view of the problems of low efficiency, high energy consumption, impurity residue, and complex maintenance proposed in the background technology, the following solutions are now proposed, including a primary purification tank. A heating mechanism for evaporating the fluorinated liquid crystal monomer is arranged outside the primary purification tank, and a spray adjustment mechanism for atomizing the fluorinated liquid crystal monomer is arranged on the inner wall of the bottom of the primary purification tank. A scraping film condensation mechanism is arranged on the inner wall of the top of the primary purification tank. The present invention has the characteristics of synergistic effect of the scraping film condensation mechanism and the semiconductor refrigeration sheet, precise impurity removal by the hierarchical adsorption mechanism, improved maintenance efficiency by modular disassembly parts, and precise material control by the spray adjustment mechanism. By integrating efficient evaporation, dynamic scraping film condensation, multi-stage adsorption, and intelligent monitoring technologies, the problems of low efficiency, high energy consumption, and difficult maintenance of traditional devices are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of purification of fluorinated liquid crystal monomers, and particularly to a purification device for preparing fluorinated liquid crystal monomers. Background Art

[0002] Fluorinated liquid crystal monomers are key materials widely used in liquid crystal displays (LCDs), optical devices, and advanced electronic devices. After introducing fluorine atoms into their molecular structures, the chemical stability, dielectric anisotropy, and thermodynamic properties of the materials are significantly improved, while the viscosity and rotational viscosity are reduced, enabling them to maintain excellent optoelectronic response characteristics over a wide temperature range. The purity of fluorinated liquid crystal monomers directly affects the contrast ratio, response speed, and service life of displays, so the purification technology in their preparation process is crucial.

[0003] As the core raw material of high-performance display materials (such as liquid crystal displays, flexible screens, etc.), the purity of fluorinated liquid crystal monomers directly affects the optical properties and stability of the final products. Currently, the preparation processes of fluorinated liquid crystal monomers generally have the following problems: Traditional fluorinated liquid crystal purification devices mostly use distillation, crystallization, or single adsorption methods, with the following defects:

[0004] I. Low efficiency: The evaporation area of conventional distillation equipment is limited, and the condensation efficiency is insufficient, resulting in a long purification cycle.

[0005] II. High energy consumption: The heating and cooling systems are separately designed, with low heat recovery rate and serious energy waste.

[0006] III. Impurity residue: A single adsorption layer is difficult to specifically remove impurities with different polarities and molecular weights, affecting the product purity.

[0007] IV. Complicated maintenance: The connection components of the equipment are fixed, making disassembly and assembly inconvenient, and it is time-consuming and laborious to replace the adsorption material or clean the pipeline.

[0008] The above problems limit the large-scale production and high-end applications of fluorinated liquid crystal monomers, and there is an urgent need for a purification device that is efficient, energy-saving, and easy to maintain. Summary of the Invention

[0009] Aiming at the deficiencies of the prior art, the present invention provides a purification device for preparing fluorinated liquid crystal monomers, which overcomes the deficiencies of the prior art and effectively solves the problems of low efficiency, high energy consumption, impurity residue, and complicated maintenance.

[0010] To achieve the above object, the present invention adopts the following technical solutions:

[0011] A purification device for preparing fluorinated liquid crystal monomers, comprising a primary purification tank. A heating mechanism for evaporating fluorinated liquid crystal monomers is arranged outside the primary purification tank, and a spray adjustment mechanism for atomizing fluorinated liquid crystal monomers is arranged on the inner wall of the bottom of the primary purification tank. A scraping film condensation mechanism is arranged on the inner wall of the top of the primary purification tank. A liquid collecting hopper is arranged inside the primary purification tank between the spray adjustment mechanism and the scraping film condensation mechanism, and a drain pipe is welded to the outer wall of the bottom of the liquid collecting hopper. A grading adsorption mechanism is arranged on one side of the primary purification tank, and disassembly parts are arranged between the grading adsorption mechanism and the drain pipe and at the bottom end of the grading adsorption mechanism.

[0012] The scraping film condensation mechanism includes a condensation component, a scraping film component, a vibration control part, and a semiconductor refrigeration sheet. Among them, the condensation component is rotatably connected to the inner wall of the top of the primary purification tank, the scraping film component penetrates through the top of the condensation component, the vibration control part is arranged at the bottom of the scraping film component and is located below the condensation component, and the semiconductor refrigeration sheet is installed on the outer wall of the top of the condensation component.

[0013] Preferably, the condensation component includes a condensation trapping plate slidably connected to the inner wall of the top of the primary purification tank, a spiral groove opened on the outer wall of the bottom of the condensation trapping plate, a groove opened on the inner wall of the spiral groove, and an arc-shaped sealing plate welded to the outer wall of the bottom of the condensation trapping plate. Among them, there are two arc-shaped sealing plates, and both are slidably connected to the inner wall of the primary purification tank.

[0014] Preferably, the scraping film component includes a speed reducer arranged at the center of the top of the primary purification tank, a traction sleeve fixedly connected to the output shaft of the speed reducer through a coupling, a rotating rod slidably connected to the inner wall of the traction sleeve, a scraping film frame welded to the outer wall of the bottom of the rotating rod, and symmetrically distributed rotating seats welded to the outer wall of the rotating rod. Among them, symmetrically distributed limiting blocks are arranged at the top of the outer wall of the rotating rod, and the limiting blocks are slidably connected in the chute of the traction sleeve, and the scraping film frame is closely attached to the inner wall of the spiral groove.

[0015] The vibration control part includes a second central frame welded to the inner wall of the primary purification tank and a convex ball welded to the central disc of the second central frame. Among them, the height of the convex ball is higher than the lowest position of the rotating seat, the convex ball is located below the rotating seat, and when the rotating seat rotates close to the convex ball, the convex ball contacts the rotating seat and triggers vibration.

[0016] Preferably, the semiconductor refrigeration sheet includes a cooling surface and a heat dissipation surface. Among them, the cooling surface is located below the heat dissipation surface and the cooling surface is closely attached to the outer wall of the top of the condensation trapping plate.

[0017] Through the above solution, the scraping film condensation mechanism and the semiconductor refrigeration sheet work synergistically: the spiral groove of the condensation component is designed to fit the scraping film frame, and the convex ball of the vibration control component periodically triggers the rotating seat, so that the condensate film is evenly distributed and quickly peeled off, avoiding local scaling. The semiconductor refrigeration sheet is directly attached to the condensation trapping plate, the cooling surface is quickly cooled, and the heat dissipation surface recovers the waste heat through the top heating cover, significantly reducing the energy consumption.

[0018] Preferably, the heating mechanism includes a heating interlayer, a temperature control controller, a top heating cover, an air inlet hose, a heat return hose, and an exhaust pipe. Among them, the heating interlayer is installed on the outer wall of the primary purification tank, the temperature control controller with an electric heating rod is installed on one outer wall of the heating interlayer, the top heating cover corresponds to the heat dissipation surface of the semiconductor refrigeration sheet, the air inlet hose is fixedly connected to one outer wall of the top heating cover through a flange, the heat return hose is fixedly connected between the top heating cover and the heating interlayer through a flange, and the exhaust pipe is fixedly connected to one outer wall of the heating interlayer.

[0019] Preferably, the spray adjustment mechanism includes a first central frame, an atomizing nozzle, a fluorinated liquid crystal feed pipe, a liquid distribution joint, a valve core connecting rod, a driven gear, a central gear, and a servo motor. Among them, the first central frame is welded to the inner peripheral wall of the primary purification tank, the atomizing nozzle is fixedly connected to the top outer wall of the first central frame through screws, the fluorinated liquid crystal feed pipe is fixedly penetrated through the inner wall of the primary purification tank, the liquid distribution joint is installed between the atomizing nozzle and the fluorinated liquid crystal feed pipe, the valve core connecting rod is rotatably connected to the bottom inner wall of the atomizing nozzle, the driven gear is installed on the outer wall of the valve core connecting rod, the central gear is meshed with the outer wall of the driven gear, the output shaft of the servo motor is fixedly connected to the inner wall of the central gear, the center of the bottom outer wall of the primary purification tank is fixedly connected with a gear box through screws, the servo motor is installed on the bottom outer wall of the gear box, and the valve core connecting rod is rotatably connected to the bottom inner wall of the gear box.

[0020] Through the above solution, the spray adjustment mechanism accurately controls the material: the servo motor is linked with the driven gear through the central gear, adjusts the opening of the valve core connecting rod, and controls the flow rate and atomization particle size of the atomizing nozzle to adapt to fluorinated liquid crystal raw materials with different viscosities.

[0021] Preferably, the fractional adsorption mechanism includes an adsorption column, an on-line monitoring component arranged at the bottom of the adsorption column, and a liquid crystal discharge pipe arranged at the bottom of the on-line monitoring component;

[0022] The adsorption column includes a secondary purification cylinder arranged on one side of the primary purification tank, a silica gel layer, a molecular sieve layer, and a MOF layer filled in the secondary purification cylinder from top to bottom;

[0023] The online monitoring component includes a crystallization module arranged on the outer wall of the bottom of the secondary purification cylinder, a near-infrared spectrometer installed on one side of the crystallization module, and a conductivity sensor installed on the other side of the crystallization module.

[0024] Through the above scheme, the fractional adsorption mechanism removes impurities precisely: the silica gel layer, molecular sieve layer, and MOF layer in the adsorption column are arranged in sequence to adsorb impurities with different polarities and sizes respectively. Combining the near-infrared spectrometer and conductivity sensor of the online monitoring component to real-time feedback the purity data, and realizing the dynamic optimization of adsorption parameters.

[0025] Preferably, the disassembly and assembly part includes a docking end, a movable sleeve, a cylinder, a sealing plug, and a limiting ring. There are two disassembly and assembly parts, and each disassembly and assembly part includes a fixed end. One of the fixed ends is fixedly connected to the outer wall of one end of the drain pipe, and the other fixed end is fixedly connected to the outer wall of the top of the crystallization module. The top of the secondary purification cylinder is provided with a detachable sealing cover. One of the docking ends is fixed at the center position of the outer wall of the sealing cover, and the other docking end is fixedly connected to the outer wall of the bottom of the secondary purification cylinder. The movable sleeve is slidably connected between the fixed end and the docking end. The cylinder is fixedly connected to the outer wall of the fixed end by bolts, the piston rod of the cylinder is installed on the outer wall of the movable sleeve, the sealing plug is welded inside the movable sleeve, and the limiting ring is welded on the outer wall of the docking end.

[0026] Through the above scheme, the modular disassembly and assembly part improves the maintenance efficiency: the cylinder drives the movable sleeve to slide, so that the sealing plug can be quickly docked or separated from the limiting ring, and the connection or replacement of the drain pipe and the fractional adsorption mechanism can be completed without tools, greatly shortening the downtime.

[0027] Preferably, connection pieces are welded on both outer walls of the condensation component, and springs are fixedly connected between the connection pieces and the primary purification tank. Guide columns are welded inside the springs on the outer wall of the top of the primary purification tank, and the guide columns are slidably connected to the inner walls of the connection pieces.

[0028] Preferably, a waste discharge pipe with a valve is installed on the outer wall of the bottom of the primary purification tank.

[0029] The beneficial effects of the present invention are as follows:

[0030] 1. For the purification device for preparing fluorinated liquid crystal monomers of the present invention, the scraping film condensation mechanism and the semiconductor refrigeration sheet cooperate to enhance the efficiency: the spiral groove of the condensation component is designed to fit the scraping film frame, and the convex balls of the vibration control part periodically trigger the rotating seat, so that the condensate film is evenly distributed and quickly peeled off, avoiding local scaling. The semiconductor refrigeration sheet is directly attached to the condensation trapping plate, the cooling surface is quickly cooled, and the heat dissipation surface recovers the waste heat through the top heating cover, significantly reducing the energy consumption;

[0031] 2. The purification device for preparing fluorinated liquid crystal monomers of the present invention has a hierarchical adsorption mechanism for precise impurity removal: the silica gel layer, molecular sieve layer, and MOF layer in the adsorption column are arranged in sequence to adsorb impurities with different polarities and sizes. Combining the near-infrared spectrometer and conductivity sensor of the on-line monitoring component to real-time feedback the purity data, realizing dynamic optimization of adsorption parameters;

[0032] 3. The purification device for preparing fluorinated liquid crystal monomers of the present invention has modular disassembly parts to improve maintenance efficiency: the cylinder drives the movable sleeve to slide, enabling the sealing plug to be quickly docked or separated from the limit ring. The connection or replacement of the drain pipe and the hierarchical adsorption mechanism can be completed without tools, greatly shortening the downtime;

[0033] 4. The purification device for preparing fluorinated liquid crystal monomers of the present invention has a spray adjustment mechanism for precise material control: the servo motor is linked with the driven gear through the central gear to adjust the opening of the valve core connecting rod, controlling the flow rate and atomization particle size of the atomizing nozzle to adapt to fluorinated liquid crystal raw materials with different viscosities. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 is a schematic diagram of the overall structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 1 ;

[0035] Figure 2 is a schematic diagram of the overall structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 2 ;

[0036] Figure 3 is a schematic diagram of the structure of the primary purification tank of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 1 ;

[0037] Figure 4 is a schematic diagram of the structure of the primary purification tank of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 2 ;

[0038] Figure 5 is a schematic diagram of the hierarchical adsorption mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0039] Figure 6 is a schematic diagram of the vertical distribution of the internal spray adjustment mechanism and the scraping film condensation mechanism of the primary purification tank of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0040] Figure 7 is a schematic diagram of the spray adjustment mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0041] Figure 8Schematic diagram of the movement trajectories of the spiral groove of the condensation trapping plate and the scraping film frame of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0042] Figure 9 Schematic diagram of the scraping film condensation mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0043] Figure 10 Schematic diagram of the split structure of the scraping film condensation mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 1 ;

[0044] Figure 11 Schematic diagram of the split structure of the scraping film condensation mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 2 ;

[0045] Figure 12 Schematic diagram of the condensation assembly of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0046] Figure 13 Schematic diagram of the three-layer structure of the adsorption column and the installation position of the on-line monitoring assembly of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0047] Figure 14 Schematic diagram of the disassembly and assembly part structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention;

[0048] Figure 15 Cross-sectional view of the disassembly and assembly part structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention.

[0049] In the figure: 1. Primary purification tank; 2. Heating mechanism; 21. Heating interlayer; 22. Temperature control controller; 23. Top heating hood; 24. Intake hose; 25. Heat reflux hose; 26. Exhaust pipe; 3. Spray adjustment mechanism; 31. First center frame; 32. Atomizing nozzle; 33. Fluorinated liquid crystal feed pipe; 34. Liquid separation joint; 35. Spool connecting rod; 36. Driven gear; 37. Center gear; 38. Servo motor; 4. Film scraping and condensation mechanism; 41. Condensation assembly; 411. Condensation trapping plate; 412. Spiral groove; 413. Groove; 414. Arc-shaped sealing plate; 42. Film scraping assembly; 421. Reducer; 422. Traction sleeve; 423. Rotating rod; 424. Film scraping frame; 425. Rotating seat; 43. Vibration control part; 431. Second center frame; 432. Convex ball; 44. Semiconductor refrigeration sheet; 441. Cooling surface; 442. Heat dissipation surface; 5. Liquid collecting hopper; 6. Drain pipe; 7. Classification adsorption mechanism; 71. Adsorption column; 711. Secondary purification cylinder; 712. Silica gel layer; 713. Molecular sieve layer; 714. MOF layer; 72. Online monitoring assembly; 721. Crystallization module; 722. Near-infrared spectrometer; 723. Conductivity sensor; 73. Liquid crystal discharge pipe; 8. Disassembly and assembly part; 81. Fixed end; 82. Docking end; 83. Movable sleeve; 84. Cylinder; 85. Sealing plug; 86. Limit ring; 9. Connecting piece; 10. Spring; 11. Guide post; 12. Waste discharge pipe. Detailed implementation mode

[0050] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments.

[0051] Example 1, referring to Figures 1 - 6 , a purification device for preparing fluorinated liquid crystal monomers, including a primary purification tank 1. A heating mechanism 2 for evaporating fluorinated liquid crystal monomers is arranged outside the primary purification tank 1. A spray adjustment mechanism 3 for atomizing fluorinated liquid crystal monomers is arranged on the inner wall of the bottom of the primary purification tank 1. A film scraping and condensation mechanism 4 is arranged on the inner wall of the top of the primary purification tank 1. A liquid collecting hopper 5 is arranged inside the primary purification tank 1 between the spray adjustment mechanism 3 and the film scraping and condensation mechanism 4. A drain pipe 6 is welded to the outer wall of the bottom of the liquid collecting hopper 5. A classification adsorption mechanism 7 is arranged on one side of the primary purification tank 1. Disassembly and assembly parts 8 are arranged between the classification adsorption mechanism 7 and the drain pipe 6 and at the bottom end of the classification adsorption mechanism 7.

[0052] In this embodiment, the primary purification tank 1 is the core container, which is externally coated with a heating sandwich layer 21. Inside, a spray adjustment mechanism 3, a liquid collection hopper 5, and a wiped-film condensation mechanism 4 are arranged from bottom to top. The heating sandwich layer 21 precisely adjusts the power of the electric heating rod through a temperature control controller 22 to keep the temperature in the tank stable at the evaporation point of the fluorinated liquid crystal (such as 120 - 150 °C). The atomizing nozzle 32 atomizes the raw material into micron-sized droplets to increase the evaporation surface area. The wiped-film condensation mechanism 4 drives the wiping film frame 424 to rotate along the spiral groove 412 by the reduction gear 421 driving the rotating rod 423, forcing the condensate film to flow and preventing crystallization blockage.

[0053] Embodiment 2, referring to Figures 8 - 12 , a purification device for preparing fluorinated liquid crystal monomers. The wiped-film condensation mechanism 4 includes a condensation component 41, a wiped-film component 42, a vibration control member 43, and a semiconductor refrigeration sheet 44. Among them, the condensation component 41 is rotatably connected to the inner wall of the top of the primary purification tank 1. The wiped-film component 42 is disposed through the top of the condensation component 41. The vibration control member 43 is arranged at the bottom of the wiped-film component 42 and is located below the condensation component 41. The semiconductor refrigeration sheet 44 is installed on the outer wall of the top of the condensation component 41.

[0054] The condensation component 41 includes a condensation trapping plate 411 slidably connected to the inner wall of the top of the primary purification tank 1, a spiral groove 412 opened on the outer wall of the bottom of the condensation trapping plate 411, a groove 413 opened on the inner wall of the spiral groove 412, and an arc-shaped sealing plate 414 welded to the outer wall of the bottom of the condensation trapping plate 411. Among them, there are two arc-shaped sealing plates 414, and both are slidably connected to the inner wall of the primary purification tank 1.

[0055] The wiped-film component 42 includes a reduction gear 421 disposed at the center of the top of the primary purification tank 1, a traction sleeve 422 fixedly connected to the output shaft of the reduction gear 421 through a coupling, a rotating rod 423 slidably connected to the inner wall of the traction sleeve 422, a wiping film frame 424 welded to the outer wall of the bottom of the rotating rod 423, and symmetrically distributed rotating seats 425 welded to the outer wall of the rotating rod 423. Among them, symmetrically distributed limit blocks are arranged at the top of the outer wall of the rotating rod 423, and the limit blocks are slidably connected in the chute of the traction sleeve 422. The wiping film frame 424 is closely attached to the inner wall of the spiral groove 412. The spiral groove 412 is located at the bottom of the condensation trapping plate 411. A scraper matching the spiral groove 412 is provided at the top end of the wiping film frame 424. The number of the spiral groove 412 and the scraper corresponds one by one. The scraper is embedded in the spiral groove 412 and rotates and moves along its path.

[0056] The vibration control member 43 includes a second central frame 431 welded to the inner wall of the primary purification tank 1 and a convex sphere 432 welded to the central disc of the second central frame 431. Among them, the height of the convex sphere 432 is higher than the lowest position of the rotating seat 425, and the convex sphere 432 is located below the rotating seat 425. When the rotating seat 425 rotates close to the convex sphere 432, the convex sphere 432 contacts the rotating seat 425 and triggers vibration.

[0057] The semiconductor refrigeration sheet 44 includes a cooling surface 441 and a heat dissipation surface 442. Among them, the cooling surface 441 is located below the heat dissipation surface 442 and the cooling surface 441 is closely attached to the top outer wall of the condensation trapping plate 411.

[0058] In this embodiment, the condensation trapping plate 411 is elastically connected to the guide post 11 through a spring 10 to adapt to thermal expansion and contraction deformation. The temperature of the cooling surface 441 of the semiconductor refrigeration sheet 44 can be reduced to -10 °C, enabling the gaseous monomer to quickly condense; the waste heat of the heat dissipation surface 442 is introduced into the heating sandwich 21 through the heat return hose 25 to achieve energy recycling. The convex sphere 432 of the vibration control member 43 periodically contacts with the rotating seat 425, generating a small vibration to promote the condensate droplets to fall off into the liquid collecting hopper 5. The rotating seat 425 is a semi-circular convex structure located on the bottom outer wall of the rotating rod 423. When the rotating rod 423 rotates, the rotating seat 425 periodically contacts the convex sphere 432 of the vibration control member 43, triggering vibration.

[0059] Embodiment Three, referring to Figure 1 、 Figure 3 A purification device for preparing fluorinated liquid crystal monomers, the heating mechanism 2 includes a heating sandwich 21, a temperature control controller 22, a top heating cover 23, an intake hose 24, a heat return hose 25, and an exhaust pipe 26. Among them, the heating sandwich 21 is installed on the outer wall of the primary purification tank 1, the temperature control controller 22 with an in-built electric heating rod is installed on one outer wall of the heating sandwich 21, the top heating cover 23 corresponds to the heat dissipation surface 442 of the semiconductor refrigeration sheet 44, and heat dissipation fins are arranged on the top outer wall of the heat dissipation surface 442 along the circumferential direction of the top outer wall of the heat dissipation surface 442. The intake hose 24 is fixedly connected to one outer wall of the top heating cover 23 through a flange, the heat return hose 25 is fixedly connected between the top heating cover 23 and the heating sandwich 21 through a flange, and the exhaust pipe 26 is fixedly connected to one outer wall of the heating sandwich 21.

[0060] In this embodiment, the heating sandwich 21 surrounds the tank body and is filled with a heatable medium. The power of the electric heating rod is adjusted by the temperature control controller 22, and the temperature accuracy is ±1 °C. The top heating cover 23 is communicated with the heating sandwich 21 through the heat return hose 25 to recover waste heat and reduce energy consumption.

[0061] Embodiment Four, referring to Figure 7, a purification device for preparing a fluorinated liquid crystal monomer. The spray adjustment mechanism 3 includes a first central frame 31, an atomizing nozzle 32, a fluorinated liquid crystal feed pipe 33, a liquid distribution joint 34, a valve core connecting rod 35, a driven gear 36, a central gear 37, and a servo motor 38. Among them, the first central frame 31 is welded to the inner peripheral wall of the primary purification tank 1, the atomizing nozzle 32 is fixedly connected to the top outer wall of the first central frame 31 by screws, the fluorinated liquid crystal feed pipe 33 is fixedly penetrated through the inner wall of the primary purification tank 1, the liquid distribution joint 34 is installed between the atomizing nozzle 32 and the fluorinated liquid crystal feed pipe 33, the valve core connecting rod 35 is rotatably connected to the bottom inner wall of the atomizing nozzle 32, the driven gear 36 is installed on the outer wall of the valve core connecting rod 35, the central gear 37 is meshed with the outer wall of the driven gear 36, and the output shaft of the servo motor 38 is fixedly connected to the inner wall of the central gear 37. The center of the bottom outer wall of the primary purification tank 1 is fixedly connected to a gear box by screws, the servo motor 38 is installed on the bottom outer wall of the gear box, and the valve core connecting rod 35 is rotatably connected to the bottom inner wall of the gear box.

[0062] In this embodiment, the servo motor 38 drives the central gear 37 to drive the driven gear 36 to rotate, and the opening of the atomizing nozzle 32 is adjusted through the valve core connecting rod 35. The liquid distribution joint 34 evenly distributes the raw materials of the fluorinated liquid crystal feed pipe 33 to a plurality of atomizing nozzles 32 to form 10 - 50 μm droplets, increasing the evaporation surface area.

[0063] Example Five, referring to Figure 5 、 Figure 13 , a purification device for preparing a fluorinated liquid crystal monomer. The fractional adsorption mechanism 7 includes an adsorption column 71, an on-line monitoring component 72 arranged at the bottom of the adsorption column 71, and a liquid crystal discharge pipe 73 arranged at the bottom of the on-line monitoring component 72;

[0064] The adsorption column 71 includes a secondary purification cylinder 711 arranged on one side of the primary purification tank 1, a silica gel layer 712, a molecular sieve layer 713, and a MOF layer 714 filled in the secondary purification cylinder 711 from top to bottom;

[0065] The on-line monitoring component 72 includes a crystallization module 721 arranged on the bottom outer wall of the secondary purification cylinder 711, a near-infrared spectrometer 722 installed on one side of the crystallization module 721, and a conductivity sensor 723 installed on the other side of the crystallization module 721.

[0066] In this embodiment, the silica gel layer 712 in the secondary purification cylinder 711 adsorbs polar impurities (such as moisture), the molecular sieve layer 713 intercepts macromolecular organic substances, and the MOF layer 714 selectively adsorbs specific functional group impurities. The crystallization module 721 induces the precipitation of trace impurities by cooling, the near-infrared spectrometer 722 monitors the chemical bond changes, the conductivity sensor 723 detects the ion residues, and the data is transmitted to the control system in real time to dynamically adjust the operating parameters of the adsorption column 71.

[0067] Example VI. Refer to Figures 14 - 15 , a purification device for preparing fluorinated liquid crystal monomers, the disassembly and assembly part 8 includes a docking end 82, a movable sleeve 83, a cylinder 84, a sealing plug 85 and a limiting ring 86. There are two disassembly and assembly parts 8, and each disassembly and assembly part 8 includes a fixed end 81. One of the fixed ends 81 is fixedly connected to the outer wall of one end of the drain pipe 6, and the other fixed end 81 is fixedly connected to the top outer wall of the crystallization module 721. The top of the secondary purification cylinder 711 is provided with a detachable sealing cover. One of the docking ends 82 is fixed at the center position of the outer wall of the sealing cover, and the other docking end 82 is fixedly connected to the bottom outer wall of the secondary purification cylinder 711. The movable sleeve 83 is slidably connected between the fixed end 81 and the docking end 82. The cylinder 84 is fixedly connected to the outer wall of the fixed end 81 by bolts. The piston rod of the cylinder 84 is installed on the outer wall of the movable sleeve 83. The sealing plug 85 is welded inside the movable sleeve 83, and the limiting ring 86 is welded on the outer wall of the docking end 82.

[0068] In this embodiment, when the adsorption column 71 needs to be replaced, the cylinder 84 contracts the piston rod, drives the movable sleeve 83 to slide towards the fixed end 81, the sealing plug 85 disengages from the docking end 82, the limiting ring 86 releases the buckle, and the adsorption column 71 can be pulled out as a whole. After the new adsorption column 71 is installed, the cylinder 84 pushes the movable sleeve 83 to reset, and the sealing plug 85 presses the docking end 82 to ensure the pipeline seal.

[0069] Refer to Figure 9 , both outer walls of the condensation component 41 are welded with connecting pieces 9, and a spring 10 is fixedly connected between the connecting piece 9 and the primary purification tank 1. A guide post 11 is welded inside the spring 10 on the top outer wall of the primary purification tank 1, and the guide post 11 is slidably connected to the inner wall of the connecting piece 9.

[0070] Refer to Figure 4 , the bottom outer wall of the primary purification tank 1 is provided with a waste discharge pipe 12 with a valve.

[0071] Working principle:

[0072] I. Raw material atomization and evaporation: The fluorinated liquid crystal raw material enters the spray adjustment mechanism 3 through the fluorinated liquid crystal feed pipe 33. The servo motor 38 adjusts the valve core opening degree, and the atomizing nozzle 32 atomizes the liquid and sprays it into the heating zone. The heating sandwich 21 provides heat to promote the evaporation of the liquid monomer.

[0073] II. Condensation and film scraping: The gaseous monomer rises to the condensation component 41. The semiconductor refrigeration sheet 44 rapidly cools it to condense it into a liquid film. The film scraping frame 424 rotates along the spiral groove 412 to scrape the liquid film, and the vibration control part 43 assists the liquid droplets to fall into the liquid collecting hopper 5.

[0074] III. Multi-stage adsorption purification: The condensate enters the fractional adsorption mechanism 7 through the drain pipe 6, and successively passes through the silica gel layer 712, the molecular sieve layer 713, and the MOF layer 714 to remove different impurities; the on-line monitoring component 72 analyzes the purity in real time, and the unqualified liquid is recycled to the primary purification tank 1 for secondary treatment.

[0075] IV. Finished product discharge and waste cleaning: The purified liquid crystal is collected through the liquid crystal discharge pipe 73, and the residual waste liquid at the bottom of the tank is regularly discharged through the waste discharge pipe 12.

[0076] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present invention.

[0077] In addition, the terms "first" and "second" are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of the present invention, "a plurality" means two or more, unless otherwise specifically defined.

[0078] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution of the present invention and its inventive concept, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.

Claims

1. A purification device for preparing fluorinated liquid crystal monomers, comprising a primary purification tank (1), characterized in that: The primary purification tank (1) is provided with a heating mechanism (2) for evaporating the fluorinated liquid crystal monomer on the outside, and a spray regulating mechanism (3) for atomizing the fluorinated liquid crystal monomer is provided on the inner wall of the bottom of the primary purification tank (1), a scraping film condensation mechanism (4) is provided on the inner wall of the top of the primary purification tank (1), a liquid collecting hopper (5) is provided inside the primary purification tank (1) between the spray regulating mechanism (3) and the scraping film condensation mechanism (4), and a liquid drain pipe (6) is welded to the outer wall of the bottom of the liquid collecting hopper (5), a graded adsorption mechanism (7) is provided on one side of the primary purification tank (1), and a disassembly component (8) is provided between the graded adsorption mechanism (7) and the liquid drain pipe (6) and at the bottom of the graded adsorption mechanism (7); The scraping film condensation mechanism (4) comprises a condensation component (41), a scraping film component (42), a vibration control component (43), and a semiconductor cooling plate (44), wherein the condensation component (41) is rotatably connected to the top inner wall of the primary purification tank (1), the scraping film component (42) is arranged through the top of the condensation component (41), the vibration control component (43) is arranged at the bottom of the scraping film component (42), and the vibration control component (43) is located below the condensation component (41), and the semiconductor cooling plate (44) is installed on the top outer wall of the condensation component (41); The condensation assembly (41) comprises a condensation collecting plate (411) slidably connected to the top inner wall of the primary purification tank (1), a spiral groove (412) provided on the bottom outer wall of the condensation collecting plate (411), a groove (413) provided on the inner wall of the spiral groove (412), and a curved sealing plate (414) welded to the bottom outer wall of the condensation collecting plate (411), wherein the curved sealing plates (414) comprise two and are both slidably connected to the inner wall of the primary purification tank (1); The film scraping assembly (42) comprises a reducer (421) arranged at the top center of the primary purification tank (1), a traction sleeve (422) fixedly connected to the output shaft of the reducer (421) through a coupling, a rotating rod (423) slidably connected to the inner wall of the traction sleeve (422), and a film scraping frame (424) welded to the outer wall of the bottom of the rotating rod (423), and the film scraping frame (424) is arranged below the condensation assembly (41) and welded to the outer wall of the rotating rod (423) symmetrically distributed rotating seats (425), wherein the top of the outer wall of the rotating rod (423) is provided with symmetrically distributed limit blocks, and the limit blocks are slidably connected in the slide groove of the traction sleeve (422), and the film scraping frame (424) is closely attached to the inner wall of the spiral groove (412); The vibration control member (43) comprises a second center frame (431) welded to the inner wall of the primary purification tank (1), and a convex ball (432) welded to the center disk of the second center frame (431), wherein the height of the convex ball (432) is higher than the lowest position of the rotating seat (425), and the convex ball (432) is located below the rotating seat (425). When the rotating seat (425) rotates close to the convex ball (432), the convex ball (432) contacts the rotating seat (425) and triggers vibration; The semiconductor refrigeration plate (44) comprises a cooling surface (441) and a heat dissipation surface (442), wherein the cooling surface (441) is located below the heat dissipation surface (442) and the cooling surface (441) is closely attached to the top outer wall of the condensation collection plate (411).

2. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The heating mechanism (2) comprises a heating interlayer (21), a temperature control controller (22), a top heating cover (23), an air intake hose (24), a heat return hose (25), and an exhaust pipe (26), wherein the heating interlayer (21) is installed on the outer wall of the primary purification tank (1), the temperature control controller (22) with its own electric heating rod is installed on one side of the outer wall of the heating interlayer (21), the top heating cover (23) corresponds to the heat dissipation surface (442) of the semiconductor refrigeration plate (44), the air intake hose (24) is fixedly connected to one side of the outer wall of the top heating cover (23) through a flange, the heat return hose (25) is fixedly connected between the top heating cover (23) and the heating interlayer (21) through a flange, and the exhaust pipe (26) is fixedly connected to one side of the outer wall of the heating interlayer (21).

3. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The spray adjustment mechanism (3) comprises a first central frame (31), an atomizing nozzle (32), a fluorinated liquid crystal feed pipe (33), a liquid separation joint (34), a valve core connecting rod (35), a driven gear (36), a central gear (37) and a servo motor (38), wherein the first central frame (31) is welded to the peripheral inner wall of the primary purification tank (1), the atomizing nozzle (32) is fixedly connected to the top outer wall of the first central frame (31) by screws, the fluorinated liquid crystal feed pipe (33) penetrates and is fixed to the inner wall of the primary purification tank (1), and the liquid separation joint (34) is installed on the atomizing nozzle (32). ) and the fluorinated liquid crystal feed pipe (33), the valve core connecting rod (35) is rotatably connected to the bottom inner wall of the atomizing nozzle (32), the driven gear (36) is installed on the outer wall of the valve core connecting rod (35), the center gear (37) is meshed with the outer wall of the driven gear (36), the output shaft of the servo motor (38) is fixedly connected to the inner wall of the center gear (37), the center of the bottom outer wall of the primary purification tank (1) is fixedly connected to a gear box by screws, the servo motor (38) is installed on the bottom outer wall of the gear box, and the valve core connecting rod (35) is rotatably connected to the bottom inner wall of the gear box.

4. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The graded adsorption mechanism (7) comprises an adsorption column (71), an online monitoring component (72) arranged at the bottom of the adsorption column (71), and a liquid crystal discharge pipe (73) arranged at the bottom of the online monitoring component (72); The adsorption column (71) comprises a secondary purification cylinder (711) arranged on one side of the primary purification tank (1), and a silica gel layer (712), a molecular sieve layer (713) and a MOF layer (714) respectively filled in the secondary purification cylinder (711) from top to bottom; The online monitoring component (72) comprises a crystallization module (721) arranged on the outer wall of the bottom of the secondary purification cylinder (711), a near-infrared spectrometer (722) installed on one side of the crystallization module (721), and a conductivity sensor (723) installed on the other side of the crystallization module (721).

5. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The disassembly component (8) comprises a docking end (82), a movable sleeve (83), a cylinder (84), a sealing plug (85) and a limiting ring (86). The disassembly component (8) comprises two, and each disassembly component (8) comprises a fixed end (81), one of the fixed ends (81) is fixedly connected to the outer wall of one end of the drain pipe (6), and the other fixed end (81) is fixedly connected to the top outer wall of the crystallization module (721). A detachable sealing cover is provided on the top of the secondary purification cylinder (711). One of the docking ends (82) is fixedly connected to the outer wall of the top of the secondary purification cylinder (711). The end (82) is fixed to the center position of the outer wall of the sealing cover, the other butt end (82) is fixedly connected to the bottom outer wall of the secondary purification cylinder (711), the movable sleeve (83) is slidably connected between the fixed end (81) and the butt end (82), the cylinder (84) is fixedly connected to the outer wall of the fixed end (81) by bolts, the piston rod of the cylinder (84) is installed on the outer wall of the movable sleeve (83), the sealing plug (85) is welded to the inside of the movable sleeve (83), and the limit ring (86) is welded to the outer wall of the butt end (82).

6. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The outer walls of both sides of the condensation component (41) are welded with connecting plates (9), and a spring (10) is fixedly connected between the connecting plate (9) and the primary purification tank (1). A guide column (11) is welded on the top outer wall of the primary purification tank (1) inside the spring (10), and the guide column (11) is slidably connected to the inner wall of the connecting plate (9).

7. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: A waste discharge pipe (12) with a valve is installed on the outer wall of the bottom of the primary purification tank (1).

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