Purifying device for preparation of fluorinated liquid crystal monomer

Abstract

The invention belongs to the technical field of fluorinated liquid crystal monomer purification, particularly relates to a fluorinated liquid crystal monomer preparation and purification device, and aims to solve the problems of low efficiency, high energy consumption, impurity residue and complicated maintenance in the background technology, and provides the following scheme: the fluorinated liquid crystal monomer preparation and purification device comprises a primary purification tank, a heating mechanism for evaporating the fluorinated liquid crystal monomer is arranged outside the primary purification tank, a spray adjusting mechanism for atomizing the fluorinated liquid crystal monomer is arranged on the inner wall of the bottom of the primary purification tank, and a wiped film condensation mechanism is arranged on the inner wall of the top of the primary purification tank. The device disclosed by the invention has the characteristics that the wiped film condensation mechanism and the semiconductor chilling plate are in synergistic interaction, the graded adsorption mechanism is used for accurately removing impurities, the maintenance efficiency is improved by a modular disassembly and assembly part, and the spray adjusting mechanism is used for accurately controlling materials; the problems that a traditional device is low in efficiency, high in energy consumption, difficult to maintain and the like are solved.

Description

Technical Field

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

[0002] Fluorinated liquid crystal monomers are a type of key material widely used in liquid crystal displays (LCDs), optical devices, and advanced electronic devices. The introduction of fluorine atoms into their molecular structure significantly improves the chemical stability, dielectric anisotropy, and thermodynamic properties of the material, while reducing viscosity and rotational viscosity, allowing it to maintain excellent photoelectric response characteristics over a wide temperature range. The purity of fluorinated liquid crystal monomers directly affects the contrast, response speed, and service life of the display, so the purification technology in its preparation process is crucial.

[0003] Fluorinated liquid crystal monomers are the core raw materials for high-performance display materials (such as liquid crystal displays, flexible screens, etc.). Their purity directly affects the optical properties and stability of the final product. At present, the preparation process of fluorinated liquid crystal monomers generally has the following problems: Traditional fluorinated liquid crystal purification devices mostly use distillation, crystallization or single adsorption methods, which have the following defects: 1. Low efficiency: Conventional distillation equipment has limited evaporation area and insufficient condensation efficiency, resulting in a long purification cycle; 2. High energy consumption: The heating and cooling systems are designed to be separated, the heat recovery rate is low, and energy waste is serious; 3. Residual impurities: It is difficult for a single adsorption layer to specifically remove impurities of different polarities and molecular weights, which affects the purity of the product; 4. Complex maintenance: The equipment connection parts are fixed, which makes disassembly and assembly inconvenient. Replacing the adsorption material or cleaning the pipeline is time-consuming and labor-intensive.

[0004] 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

[0005] In view of 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, residual impurities and complex maintenance.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions: A purification device for preparing fluorinated liquid crystal monomers comprises a primary purification tank, wherein a heating mechanism for evaporating the fluorinated liquid crystal monomers is arranged on the outside of the primary purification tank, and a spray regulating mechanism for atomizing the 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 regulating 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 graded adsorption mechanism is arranged on one side of the primary purification tank, and disassembly parts are arranged between the graded adsorption mechanism and the drain pipe and at the bottom of the graded adsorption mechanism.

[0007] The scraping film condensation mechanism includes a condensation component, a scraping film component, a vibration control component, and a semiconductor refrigeration plate, wherein the condensation component is rotatably connected to the top inner wall of the primary purification tank, the scraping film component is arranged through the top of the condensation component, the vibration control component is arranged at the bottom of the scraping film component, and the vibration control component is located below the condensation component, and the semiconductor refrigeration plate is installed on the top outer wall of the condensation component.

[0008] Preferably, the condensation assembly includes a condensation collecting plate slidably connected to the top inner wall of the primary purification tank, a spiral groove opened on the bottom outer wall of the condensation collecting plate, a groove opened on the inner wall of the spiral groove, and a curved sealing plate welded to the bottom outer wall of the condensation collecting plate, wherein the curved sealing plates include two and both are slidably connected to the inner wall of the primary purification tank.

[0009] Preferably, the scraping assembly includes a reducer arranged at the top center of the primary purification tank, a traction sleeve fixedly connected to the output shaft of the reducer through a coupling, a rotating rod slidably connected to the inner wall of the traction sleeve, and a scraping frame welded to the outer wall of the bottom of the rotating rod, and the scraping frame is arranged below the condensation assembly and is welded to a symmetrically distributed rotating seat on the outer wall of the rotating rod, wherein symmetrically distributed limit blocks are arranged on the top of the outer wall of the rotating rod, and the limit blocks are slidably connected in the slide groove of the traction sleeve, and the scraping frame is tightly attached to the inner wall of the spiral groove.

[0010] The vibration control component includes a second center frame welded to the inner wall of the primary purification tank and a convex ball welded to the center disk of the second center frame, wherein the height of the convex ball is higher than the lowest position of the rotating seat, and the convex ball is located below the rotating seat. When the rotating seat rotates close to the convex ball, the convex ball contacts the rotating seat and triggers vibration.

[0011] Preferably, the semiconductor refrigeration plate comprises a cooling surface and a heat dissipation surface, wherein the cooling surface is located below the heat dissipation surface and the cooling surface is closely attached to the top outer wall of the condensation collection plate.

[0012] Through the above scheme, the scraping film condensation mechanism and the semiconductor refrigeration plate work together to enhance efficiency: the spiral groove of the condensation component is fitted with the scraping film frame, and the convex ball of the vibration control component periodically triggers the rotating seat to make the condensate film evenly distributed and quickly peeled off to avoid local scaling. The semiconductor refrigeration plate is directly attached to the condensation capture plate, the cooling surface is quickly cooled, and the heat dissipation surface recovers waste heat through the top heating cover, which significantly reduces energy consumption.

[0013] Preferably, the heating mechanism includes a heating interlayer, a temperature control controller, a top heating cover, an air intake hose, a heat return hose, and an exhaust pipe, wherein the heating interlayer is installed on the outer wall of the primary purification tank, the temperature control controller with its own electric heating rod is installed on one side of the outer wall of the heating interlayer, the top heating cover corresponds to the heat dissipation surface of the semiconductor refrigeration plate, the air intake hose is fixedly connected to one side of the outer wall of the top heating cover by a flange, the heat return hose is fixedly connected between the top heating cover and the heating interlayer by a flange, and the exhaust pipe is fixedly connected to one side of the outer wall of the heating interlayer.

[0014] Preferably, the spray adjustment mechanism includes a first center frame, an atomizing nozzle, a fluorinated liquid crystal feed pipe, a liquid separation joint, a valve core connecting rod, a driven gear, a central gear and a servo motor, wherein the first center frame is welded to the peripheral inner wall of the primary purification tank, the atomizing nozzle is fixedly connected to the top outer wall of the first center frame by screws, the fluorinated liquid crystal feed pipe is penetrated and fixed on the inner wall of the primary purification tank, the liquid separation 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, a gear box is fixedly connected to the center of the bottom outer wall of the primary purification tank by 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.

[0015] Through the above solution, the spray adjustment mechanism can accurately control the material: the servo motor is linked with the driven gear through the central gear to adjust the opening of the valve core connecting rod, control the flow rate and atomization particle size of the atomizing nozzle, and adapt to fluorinated liquid crystal raw materials with different viscosities.

[0016] Preferably, the graded adsorption mechanism comprises an adsorption column, an online monitoring component arranged at the bottom of the adsorption column, and a liquid crystal discharge pipe arranged at the bottom of the online monitoring component; The adsorption column comprises a secondary purification cylinder arranged on one side of the primary purification tank, and a silica gel layer, a molecular sieve layer and a MOF layer respectively filled in the secondary purification cylinder from top to bottom; The online monitoring component comprises 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.

[0017] Through the above scheme, the graded adsorption mechanism can accurately remove impurities: the silica gel layer, molecular sieve layer and MOF layer in the adsorption column are arranged in sequence, respectively adsorbing impurities of different polarities and sizes. The near-infrared spectrometer and conductivity sensor of the online monitoring component can provide real-time feedback of purity data to achieve dynamic optimization of adsorption parameters.

[0018] Preferably, the disassembly and assembly parts include a butt joint, a movable sleeve, a cylinder, a sealing plug and a limit 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 top outer wall of the crystallization module. A removable sealing cover is provided on the top of the secondary purification cylinder, one of the butt joint ends is fixed to the center position of the outer wall of the sealing cover, and the other butt joint end is fixedly connected to the bottom outer wall of the secondary purification cylinder. The movable sleeve is slidably connected between the fixed end and the butt joint 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 to the inside of the movable sleeve, and the limit ring is welded to the outer wall of the butt joint end.

[0019] Through the above solution, modular disassembly and assembly parts improve maintenance efficiency: the cylinder drives the movable sleeve to slide, so that the sealing plug and the limit ring can be quickly connected or separated, and the connection or replacement of the drain pipe and the graded adsorption mechanism can be completed without tools, which greatly shortens the downtime.

[0020] Preferably, connecting plates are welded to the outer walls on both sides of the condensation assembly, and a spring is fixedly connected between the connecting plate and the primary purification tank. A guide column is welded to the outer wall of the top of the primary purification tank inside the spring, and the guide column is slidably connected to the inner wall of the connecting plate.

[0021] Preferably, a waste pipe with a valve is installed on the outer wall of the bottom of the primary purification tank.

[0022] The beneficial effects of the present invention are: 1. The purification device for preparing fluorinated liquid crystal monomers of the present invention has a synergistic effect between the scraping film condensation mechanism and the semiconductor refrigeration sheet: 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 condensed liquid film is evenly distributed and quickly peeled off to avoid local scaling. The semiconductor refrigeration sheet is directly attached to the condensation capture plate, the cooling surface is quickly cooled, and the heat dissipation surface recovers waste heat through the top heating cover, which significantly reduces energy consumption; 2. The purification device for preparing fluorinated liquid crystal monomers of the present invention has a graded 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 of different polarities and sizes respectively, and the near-infrared spectrometer and conductivity sensor of the online monitoring component are combined to feedback purity data in real time to achieve dynamic optimization of adsorption parameters; 3. The purification device for preparing fluorinated liquid crystal monomers of the present invention has modular disassembly and assembly parts to improve maintenance efficiency: the cylinder drives the movable sleeve to slide, so that the sealing plug and the limit ring can be quickly connected or separated, and the connection or replacement of the discharge pipe and the graded adsorption mechanism can be completed without tools, which greatly shortens the downtime; 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, control the flow rate and atomization particle size of the atomizing nozzle, and adapt to fluorinated liquid crystal raw materials with different viscosities. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The overall structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention is shown in FIG. Figure 1 ; Figure 2 The overall structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention is shown in FIG. Figure 2 ; Figure 3 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 ; Figure 4 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 ; Figure 5 A schematic diagram of a graded adsorption mechanism of a purification device for preparing a fluorinated liquid crystal monomer proposed by the present invention; Figure 6 A schematic diagram of the vertical distribution of the spray adjustment mechanism and the scraping film condensation mechanism inside the primary purification tank of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention; Figure 7 A schematic diagram of a spray regulating mechanism of a purification device for preparing a fluorinated liquid crystal monomer proposed by the present invention; Figure 8 A schematic diagram of the motion trajectory of the spiral groove of the condensation collection plate and the film scraping frame of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention; Fig. 9 A schematic diagram of a scraped film condensation mechanism of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention; Fig.10 Schematic diagram of the split structure of the scraping condensation mechanism of the purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 1 ; Fig.11 Schematic diagram of the split structure of the scraping condensation mechanism of the purification device for preparing fluorinated liquid crystal monomers proposed by the present invention Figure 2 ; Fig.12 A schematic diagram of a condensation component of a purification device for preparing a fluorinated liquid crystal monomer proposed by the present invention; Fig.13 A schematic diagram of the three-layer structure of an adsorption column and the installation position of an online monitoring component of a purification device for preparing a fluorinated liquid crystal monomer proposed by the present invention; Fig.14 This is a schematic diagram of the disassembly and assembly structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention; Fig.15 This is a cross-sectional view of the disassembly and assembly structure of a purification device for preparing fluorinated liquid crystal monomers proposed by the present invention.

[0024] In the figure: 1. primary purification tank; 2. heating mechanism; 21. heating interlayer; 22. temperature control controller; 23. top heating cover; 24. air 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. valve core connecting rod; 36. driven gear; 37. center gear; 38. servo motor; 4. scraping film condensation mechanism; 41. condensation assembly; 411. condensation capture plate; 412. spiral groove; 413. groove; 414. arc surface sealing plate; 42. scraping film assembly; 421. reducer; 422. traction sleeve; 423. rotating rod; 424. scraping film frame; 425. Rotating seat; 43, vibration control part; 431, second center frame; 432, convex ball; 44, semiconductor refrigeration plate; 441, cooling surface; 442, heat dissipation surface; 5, liquid collecting bucket; 6, liquid discharge pipe; 7, graded adsorption mechanism; 71, adsorption column; 711, secondary purification cylinder; 712, silica gel layer; 713, molecular sieve layer; 714, MOF layer; 72, online monitoring component; 721, crystallization module; 722, near-infrared spectrometer; 723, conductivity sensor; 73, liquid crystal discharge pipe; 8, disassembly and assembly parts; 81, fixed end; 82, docking end; 83, movable sleeve; 84, cylinder; 85, sealing plug; 86, limit ring; 9, connecting piece; 10, spring; 11, guide column; 12, waste discharge pipe. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0026] Embodiment 1, refer to Figure 1-Figure 6A purification device for preparing fluorinated liquid crystal monomers comprises a primary purification tank 1, the outside of the primary purification tank 1 is provided with a heating mechanism 2 for evaporating the fluorinated liquid crystal monomers, and the bottom inner wall of the primary purification tank 1 is provided with a spray regulating mechanism 3 for atomizing the fluorinated liquid crystal monomers, the top inner wall of the primary purification tank 1 is provided with a scraping film condensation mechanism 4, the inside of the primary purification tank 1 is provided with a liquid collecting hopper 5 between the spray regulating mechanism 3 and the scraping film condensation mechanism 4, and the bottom outer wall of the liquid collecting hopper 5 is welded with a drain pipe 6, 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 drain pipe 6 and at the bottom of the graded adsorption mechanism 7.

[0027] In this embodiment, the primary purification tank 1 is a core container, which is covered with a heating interlayer 21 on the outside, and a spray adjustment mechanism 3, a liquid collecting hopper 5 and a scraping film condensation mechanism 4 are arranged from bottom to top inside. The heating interlayer 21 accurately adjusts the power of the electric heating rod through the temperature control controller 22 to stabilize the temperature in the tank at the evaporation point of the fluorinated liquid crystal (such as 120~150℃). The atomizing nozzle 32 atomizes the raw material into micron-sized droplets to increase the evaporation surface area; the scraping film condensation mechanism 4 drives the rotating rod 423 through the reducer 421 to drive the scraping film frame 424 to rotate along the spiral groove 412, forcing the condensed liquid film to flow and prevent crystallization blockage.

[0028] Example 2, refer to Figure 8-Figure 12 A purification device for preparing fluorinated liquid crystal monomers, wherein the scraping condensation mechanism 4 includes a condensation component 41, a scraping component 42, a vibration control component 43, and a semiconductor refrigeration sheet 44, wherein the condensation component 41 is rotatably connected to the top inner wall of the primary purification tank 1, the scraping 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 component 42, and the vibration control component 43 is located below the condensation component 41, and the semiconductor refrigeration sheet 44 is installed on the top outer wall of the condensation component 41.

[0029] The condensation assembly 41 includes a condensation collecting plate 411 slidably connected to the top inner wall of the primary purification tank 1, a spiral groove 412 opened on the bottom outer wall of the condensation collecting plate 411, a groove 413 opened 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 include two and both are slidably connected to the inner wall of the primary purification tank 1.

[0030] The scraper assembly 42 includes 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 scraper frame 424 welded to the outer wall of the bottom of the rotating rod 423, and the scraper frame 424 is arranged below the condensation assembly 41 and welded to a symmetrically distributed rotating seat 425 on the outer wall of the rotating rod 423, wherein a symmetrically distributed limit block is arranged on the top of the outer wall of the rotating rod 423, and the limit block is slidably connected in the slide groove of the traction sleeve 422, and the scraper frame 424 is tightly attached to the inner wall of the spiral groove 412, and the spiral groove 412 is located at the bottom of the condensation capture plate 411, and a scraper matching the spiral groove 412 is provided at the top of the scraper frame 424, and the number of spiral grooves 412 and scrapers corresponds one to one, and the scraper is embedded in the spiral groove 412 and rotates along its path.

[0031] The vibration control component 43 includes 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.

[0032] The semiconductor cooling plate 44 includes a cooling surface 441 and a heat dissipation surface 442 , wherein the cooling surface 441 is located below the heat dissipation surface 442 and is closely attached to the top outer wall of the condensation collection plate 411 .

[0033] In this embodiment, the condensation capture plate 411 is elastically connected to the guide column 11 through the spring 10 to adapt to thermal expansion and contraction deformation. The temperature of the cooling surface 441 of the semiconductor refrigeration plate 44 can be reduced to -10°C, so that the gaseous monomer can be quickly condensed; the waste heat of the heat dissipation surface 442 is introduced into the heating interlayer 21 through the heat return hose 25 to achieve energy recycling. The convex ball 432 of the vibration control component 43 periodically contacts with the rotating seat 425, generating small vibrations, which promotes the condensed liquid droplets to fall off into the liquid collecting bucket 5. The rotating seat 425 is a semicircular raised structure located on the outer wall of the bottom of the rotating rod 423. When the rotating rod 423 rotates, the rotating seat 425 periodically contacts the convex ball 432 of the vibration control component 43 to trigger vibration.

[0034] Example 3, refer to Figure 1 , Figure 3, a purification device for preparing fluorinated liquid crystal monomers, the heating mechanism 2 includes a heating interlayer 21, a temperature control controller 22, a top heating cover 23, an air intake hose 24, a heat reflux 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 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, and the top outer wall of the heat dissipation surface 442 is provided with heat dissipation fins distributed circumferentially along the top outer wall of the heat dissipation surface 442, the air intake hose 24 is fixedly connected to one side outer wall of the top heating cover 23 by a flange, the heat reflux hose 25 is fixedly connected between the top heating cover 23 and the heating interlayer 21 by a flange, and the exhaust pipe 26 is fixedly connected to one side outer wall of the heating interlayer 21.

[0035] In this embodiment, the heating interlayer 21 surrounds the tank body and is filled with a heatable medium. The temperature controller 22 adjusts the power of the electric heating rod, and the temperature accuracy is ±1° C. The top heating cover 23 is connected to the heating interlayer 21 through a heat return hose 25 to recover waste heat and reduce energy consumption.

[0036] Embodiment 4, referring to Figure 7 A purification device for preparing fluorinated liquid crystal monomers, wherein 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 is penetrated and fixed on the inner wall of the primary purification tank 1, and the liquid separation joint 34 is installed on the atomizing nozzle 32. Between the 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, and 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 with a gear box by screws, and 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.

[0037] 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 multiple atomizing nozzles 32 to form 10-50μm droplets to increase the evaporation surface area.

[0038] Example 5, refer to Figure 5 , Fig.13, a purification device for preparing fluorinated liquid crystal monomers, the graded adsorption mechanism 7 includes 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 includes a secondary purification cylinder 711 disposed on one side of the primary purification tank 1, 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 includes a crystallization module 721 disposed 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 .

[0039] In this embodiment, the silica gel layer 712 in the secondary purification cylinder 711 adsorbs polar impurities (such as water), the molecular sieve layer 713 intercepts macromolecular organic matter, and the MOF layer 714 selectively adsorbs impurities of specific functional groups. The crystallization module 721 induces the precipitation of trace impurities by cooling, the near-infrared spectrometer 722 monitors the change of chemical bonds, and the conductivity sensor 723 detects ion residues. The data is transmitted to the control system in real time to dynamically adjust the operating parameters of the adsorption column 71.

[0040] Example 6, refer to Figure 14-15 , a purification device for preparing fluorinated liquid crystal monomers, the disassembly component 8 includes a docking end 82, a movable sleeve 83, a cylinder 84, a sealing plug 85 and a limiting ring 86, the disassembly component 8 includes two, and each disassembly component 8 includes a fixed end 81, one of the fixed ends 81 is fixedly connected to the outer wall of one end of the discharge pipe 6, and the other fixed end 81 is fixedly connected to the top outer wall of the crystallization module 721. A removable sealing cover is provided on the top of the secondary purification cylinder 711, one of the docking ends 82 is fixed to 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, and 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 limiting ring 86 is welded to the outer wall of the docking end 82.

[0041] In this embodiment, when the adsorption column 71 needs to be replaced, the cylinder 84 retracts the piston rod, drives the movable sleeve 83 to slide toward the fixed end 81, the sealing plug 85 is separated from the docking end 82, the limit ring 86 releases the buckle, and the adsorption column 71 can be withdrawn 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 is sealed.

[0042] Reference Fig. 9The outer walls on both sides 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 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 piece 9.

[0043] Reference Figure 4 A waste pipe 12 with a valve is installed on the outer wall of the bottom of the primary purification tank 1.

[0044] Working principle: 1. 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, the atomizing nozzle 32 atomizes the liquid and sprays it into the heating area, and the heating interlayer 21 provides heat to promote the evaporation of the liquid monomer.

[0045] 2. Condensation and film scraping: The gaseous monomer rises to the condensation assembly 41 , and the semiconductor refrigeration plate 44 quickly cools it down to condense it into a liquid film. The film scraping frame 424 rotates along the spiral groove 412 to scrape off the liquid film, and the vibration control component 43 assists the liquid droplets to fall into the liquid collecting bucket 5 .

[0046] 3. Multi-stage adsorption purification: The condensate enters the graded adsorption mechanism 7 through the drain pipe 6, and passes through the silica gel layer 712, the molecular sieve layer 713 and the MOF layer 714 in turn to remove different impurities; the online monitoring component 72 analyzes the purity in real time, and the unqualified liquid is recycled back to the primary purification tank 1 for secondary treatment.

[0047] 4. 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.

[0048] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0049] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0050] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which 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).

2. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: The condensation assembly (41) includes a condensation collecting plate (411) slidably connected to the top inner wall of the primary purification tank (1), a spiral groove (412) opened on the bottom outer wall of the condensation collecting plate (411), a groove (413) opened 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 plate (414) includes two curved sealing plates (414) both of which are slidably connected to the inner wall of the primary purification tank (1).

3. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: 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 component (43) includes 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.

4. A purification device for preparing fluorinated liquid crystal monomers according to claim 1, characterized in that: 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).

5. 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).

6. 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.

7. 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).

8. 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).

9. 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).

10. 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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