Strip-shaped flaky crystal form alkyl cyclohexylphenol as well as preparation method and equipment thereof

Abstract

The invention discloses strip-shaped flaky crystal form alkyl cyclohexylphenol as well as a preparation method and equipment thereof, and relates to the technical fields of an organic compound crystallization process and liquid crystal material preparation. According to the invention, through the original eddy current enhanced crystallization and pulse type supersaturation degree regulation and control technology, the leapfrogging progress of grain size uniformity is realized, and the crystal form has the characteristics of large size and high purity. According to the preparation method, integrated equipment is adopted, an eddy field and solvent pulse supplementing technology is utilized in a spiral reducing pipeline, the crystallization process is accurately controlled, the crystal size distribution is uniform, the equipment integrates temperature, centrifugation and a liquid supplementing automatic adjusting system, and ultrasonic real-time monitoring is matched, so that the high-stability strip-shaped flaky crystal can be produced; the method solves the problems of low efficiency and non-uniform crystal form of the traditional process, and is particularly suitable for large-scale preparation of high-precision liquid crystal display material intermediates.

Description

Technical Field

[0001] The invention relates to the technical field of organic compound crystallization technology and liquid crystal material preparation, in particular to a strip-shaped flaky crystal type alkylcyclohexylphenol and a preparation method and equipment thereof. Background Art

[0002] Alkylcyclohexylphenol is a key intermediate in the preparation of high-performance liquid crystal display materials. The regularity of its crystal structure is directly related to the orientation accuracy and optical uniformity of liquid crystal molecules. In the manufacture of ultra-high-definition display panels, the high purity and low defectivity of this material can significantly reduce undesirable phenomena such as screen bright spots and color shift, playing an irreplaceable role in promoting 8K and higher resolution display technology and the mass production of flexible screens. As emerging fields such as virtual reality and in-vehicle displays continue to escalate in terms of display quality, market demand for high-purity and morphologically controllable alkylcyclohexylphenol crystals continues to rise, driving innovation in the research and development of this material and its preparation technology.

[0003] Current industrial production primarily utilizes a batch crystallization process, relying on manual experience to adjust the solution supersaturation. Traditional gradient cooling methods, due to the operator's extensive control of supersaturation (S < 1.1), result in a discrete grain size distribution and a lattice consistency index that consistently remains below the industry standard lower limit. Taking a typical multi-reactor cascade process as an example, a single batch production cycle can last up to twelve hours, with a grain length deviation rate exceeding one-third, severely restricting production efficiency and product consistency. The dynamic mismatch between the solvent evaporation rate and the temperature field further exacerbates process out-of-control. Supersaturation in localized regions of the system suddenly increases above a critical value, triggering explosive nucleation, with the nucleus density per unit volume far exceeding the normal growth threshold. This abnormal nucleation not only deteriorates crystal size uniformity but also induces lattice distortion, forming numerous structural defects.

[0004] In response to the above problems, the invention patent with publication number CN103553878B proposes a crystallization scheme using multi-stage gradient cooling combined with mechanical stirring. It is to react benzyloxy bromobenzene compounds with magnesium chips in a solvent to obtain benzyloxyphenyl magnesium bromide, which is then reacted with raw material A, and then acid hydrolyzed to obtain compound B; compound B is subjected to a series of processes such as reflux dehydration in an organic solvent and an organic acid system to obtain compound C; in an organic solvent with a pH of 6.5-7.5, compound C is hydrogenated in the presence of a catalyst to obtain a cis-trans compound D; the cis-trans compound D is isomerized in an organic solvent and a strong alkaline system to obtain a trans product, and then an alkylcyclohexylphenol liquid crystal intermediate compound is obtained through a series of processes, but this technology has problems with crystal nucleus density and morphology. Defects of poor control: its cooling gradient preset mode cannot respond to real-time supersaturation changes. When the solvent evaporation rate fluctuates, it will still cause local supersaturation overload. Experimental data show that its crystal nucleus density is still as high as 2-3 times the conventional value; although the shear force generated by mechanical stirring can improve the mass transfer efficiency, it will destroy the directional growth of the crystal (001) plane, resulting in a discrete aspect ratio of more than 40% in the obtained crystal form, which is difficult to meet the morphological requirements of the strip-shaped flake crystal form; in order to achieve multi-stage temperature control, an additional cooling module must be configured, which increases the energy consumption per unit product to 2.8kW·h / kg. Although it is better than the traditional multi-reactor process, it is still more than 40% higher than the industry's advanced energy efficiency standards.

[0005] Existing kettle crystallizers lack the ability to dynamically adjust parameters, preventing continuous coordinated control of nucleation, crystal growth, and exfoliation processes. This has resulted in batch yields consistently hovering below 80%. While multi-kettle series designs attempt to compensate for the inefficiency of single kettles, they increase equipment footprint by 50% and increase energy consumption per unit product by 1.6 times the industry's energy efficiency standard, becoming a key obstacle to the industry's green upgrade.

[0006] Therefore, we propose an alkylcyclohexylphenol strip-shaped flake crystal form and its preparation method and special equipment to solve the above problems. Summary of the Invention

[0007] The purpose of the present invention is to provide a strip-shaped flaky crystalline alkylcyclohexylphenol and a preparation method and equipment thereof in order to solve the technical problems in the background technology.

[0008] To achieve the above object, the present invention provides the following technical solution: a method for preparing strip-shaped flaky crystal-type alkylcyclohexylphenol, comprising the following steps: S1: dissolving alkylcyclohexylphenol and solvent at a mass ratio of 1:1.2-1.6 at elevated temperature to form a supersaturated solution; S2: introducing the solution prepared in step S1 into a spiral tapered pipe with a centrifugal function, maintaining the pipe temperature and starting the centrifugal rotation to move the solution along the pipe wall, forming a vortex crystallization environment in the pipe; S3: Pulse-feed a supersaturated solution of alkylcyclohexylphenol into the pipeline at a rate of 0.5-2 mL / min, controlling the supersaturation of the solution S = 1.2-1.5 to induce Ostwald ripening; S4: Repeat steps S2 and S3 to perform multi-stage dynamic crystallization, allowing the crystallization solution to circulate in the spiral tapering pipe 3 to 5 times until the crystal length reaches 9 to 17 mm and the width reaches 2 to 5.5 mm; S5: Start the scraping mechanism to peel off the crystals, centrifuge and then dry to obtain strip-shaped alkylcyclohexylphenol crystals.

[0009] As a further embodiment of the present invention: the heating and dissolving in step S1 is carried out at a temperature within the range of 65 to 80° C.; the added solvent is ethanol; As a further solution of the present invention: the diameter contraction ratio of the spiral tapered pipe in step S2 is 2:1 to 4:1, the pipe temperature is maintained at 45 to 65° C., and the centrifugal speed is started at 80 to 120 rpm.

[0010] As a further solution of the present invention: in step S3, the supplementary acceleration satisfies the formula v=20V / t, where V is the volume of the reactor (mL) and t is the current crystallization time (min).

[0011] A preparation device for strip-shaped flake crystal alkylcyclohexylphenol, steps S1 to S4 are completed in an integrated device, the integrated device includes a connecting pipe, two sides of the connecting pipe are fixedly connected to a liquid feed pipe and a solid feed port, a condenser is installed at the top of the connecting pipe, the bottom end of the connecting pipe is fixedly connected to a reaction chamber, the bottom end of the reaction chamber is fixedly connected to a discharge pipe, the bottom end of the discharge pipe is fixedly connected to a centrifugal chamber, a spiral tapered pipe is installed inside the centrifugal chamber, the bottom end of the centrifugal chamber is fixedly connected to a mounting seat, the bottom end of the mounting seat is installed with a collecting bucket, the inner cavity of the collecting bucket is provided with a filter basket, the outer wall of the reaction chamber is installed with a heating jacket, the outer wall of the centrifugal chamber is installed with an insulation jacket, one side outer wall of the mounting seat is fixedly connected to a leaching pipe, and one side outer wall of the reaction chamber is fixedly connected to an air inlet pipe; The transmission mechanism that this second motor is connected with this second motor is that the transmission mechanism that this second motor is connected with this second motor is that the transmission mechanism that this second motor is connected with this second motor is that the transmission mechanism that this second motor is connected with this second motor is that the transmission mechanism that this second motor is connected with this second motor is that the transmission mechanism that this second motor is connected with this second motor is that

[0012] The top end face of said sliding panel also is provided with an interlock plate, and the interlock plate is connected with a up-down knob. The interlock plate is connected with a up-down knob on the second rotatable plate, and the up-down knob has a first end in threaded connection to the first end of the sliding panel and a second end in threaded connection to the first end of the sliding panel.

[0013] As a further solution of the present invention: the scraping mechanism includes a third motor, the third motor is installed at the bottom end of the collecting bucket, the output end of the third motor is connected to a connecting shaft, the top of the connecting shaft is fixedly connected to a square rod, the square rod is rotatably connected to the top of the support seat, the bottom of the filter basket is rotatably connected to the rotating disk, the bottom end of the rotating disk is provided with a square groove, the top of the rotating disk is fixedly connected to a vertical rod, the outer wall of the vertical rod is symmetrically fixedly connected to a cross rod, the outer wall of the cross rod is slidably connected to the scraper, and the outer wall of the scraper is obliquely fixedly connected to a guide frame with a strip guide groove, the inner part of the vertical rod is slidably connected to a cross extending from the vertical rod, and the two ends of the vertical rod are symmetrically fixedly connected to sliding rods, the sliding rod is slidably connected to the inner wall of the strip guide groove, and the top of the cross is fixedly connected to the lower pressure cylinder.

[0014] As a further solution of the present invention: the outer wall of the annular plate fits with the inner wall of the placement groove, the inner wall of the slot fits with the outer wall of the insertion rod, the inner wall of the connecting groove fits with the outer wall of the connecting rod, and the protruding end of the fixing block is provided with a bevel and the outer wall of the protruding end fits with the inner wall of the fixing groove.

[0015] As a further solution of the present invention: the fixing block is in an L-shape, and a threaded hole is provided on the outer wall of the push plate, and the threaded hole matches the threaded rod.

[0016] As a further solution of the present invention: the outer wall of the square rod is in contact with the inner wall of the square groove, and the inner wall of the strip guide groove is in contact with the outer wall of the slide rod.

[0017] Compared with the prior art, the present invention has the following beneficial effects: 1. The alkylcyclohexylphenol strip-shaped flake crystal form and preparation method of the present invention achieve a leap forward in grain size uniformity through original eddy current enhanced crystallization and pulsed supersaturation control technology, completely solving the core pain points of poor thermal stability of the crystal form and excessive solvent residue in traditional processes.

[0018] 2. The alkylcyclohexylphenol strip-shaped flake crystal form and preparation method of the present invention support multi-dimensional adjustment such as pipeline contraction ratio (2:1-4:1) and supplementary acceleration (0.5-2mL / min) through flexible design of process parameters. It can be customized to produce crystals of different specifications of 9-17mm, adapting to the needs of emerging display devices such as flexible screens and VR helmets, and providing core material guarantee for the ultra-high-definition display industry.

[0019] 3. The integrated dynamic crystallization equipment of the present invention compresses the single-batch production cycle from 12 hours to 7.2 hours, improves efficiency by 40%, reduces comprehensive production costs by 30%, and reduces equipment footprint by 40%, achieving a synergistic breakthrough in high efficiency and low cost.

[0020] 4. In order to match the improved process, the present invention designs an integrated device. The integrated device is equipped with an installation mechanism and a scraping mechanism to place the filter basket into the collection barrel until the bottom end of the filter basket contacts the support seat, the annular plate is displaced into the placement groove, and the insertion rod is inserted into the slot to position the filter basket. Then, the collection barrel is moved so that the first docking plate and the second docking plate are aligned, the connecting rod is inserted into the connecting groove, and the fixing block is engaged into the fixing groove under the elastic force of the first spring. The collection barrel and the filter basket are installed, which facilitates rapid installation and disassembly of the filter basket. When the filter basket is installed, the solution in the filter basket is centrifuged by the rotation of the scraper; after the filter basket is disassembled, the crystals on the inner wall of the filter basket are scraped off by the rotation of the scraper. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a schematic structural diagram of the integrated device of the present invention; Figure 2 This is a schematic diagram of the internal structure of the integrated device of the present invention; Figure 3 This is a schematic diagram of the internal structure of the reaction chamber of the integrated device of the present invention; Figure 4 This is a schematic diagram of the internal structure of the mounting base of the integrated device of the present invention; Figure 5 This is a schematic diagram of the installation of the collection bucket of the integrated device of the present invention; Figure 6 For the integrated device of the present invention Figure 5 Enlarged view of point A in the middle; Figure 7 This is a schematic diagram of the installation of the filter basket of the integrated device of the present invention; Figure 8 This is a schematic diagram of the internal structure of the filter basket of the integrated device of the present invention; Figure 9 This is a schematic diagram of the internal structure of the vertical rod of the integrated equipment described in the present invention.

[0022] In the figure: 1. connecting pipe; 2. liquid feed pipe; 3. solid feed port; 4. reaction chamber; 5. discharge pipe; 6. centrifugal chamber; 7. spiral tapered pipe; 8. mounting mechanism; 801. first docking plate; 802. second docking plate; 803. connecting rod; 804. fixing groove; 805. connecting groove; 806. fixing block; 807. first spring; 808. push plate; 809. threaded rod; 810. rotating column; 811. annular plate; 812. slot; 813. placement groove; 814. insert rod; 815. support seat; 9. scraping mechanism; 901. third motor; 902. connecting Shaft; 903, square rod; 904, rotating disk; 905, square groove; 906, vertical rod; 907, horizontal rod; 908, scraper; 909, guide frame; 910, cross; 911, slide bar; 912, lower pressure cylinder; 10, filter basket; 11, condenser; 12, heating jacket; 13, insulation jacket; 14, rinse pipe; 15, air inlet pipe; 16, baffle; 17, limit rod; 18, screw; 19, first motor; 20, filter plate; 21, rotating plate; 22, first bevel gear; 23, second bevel gear; 24, second motor; 25, mounting base; 26, collecting bucket. DETAILED DESCRIPTION

[0023] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0024] In the description of the present invention, it should be noted that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside" and the like indicate positions or positional relationships based on the positions 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 devices or components referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are only used for descriptive purposes and should not be understood as indicating or implying relative importance. In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", and "set" should be understood in a broad sense, for example, they can be fixedly connected, detachably connected, or connected in one piece; they can be mechanically connected or electrically connected; they can be directly connected, or indirectly connected through an intermediate medium, or they can be internal connections between two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. The following describes an embodiment of the present invention based on its overall structure.

[0025] Example 1

[0026] In an embodiment of the present invention, a method for preparing a strip-shaped flaky crystal-type alkylcyclohexylphenol comprises the following steps: S1. Dissolve 200 kg of alkylcyclohexylphenol (purity up to 99.5%) and 280 kg of ethanol (60°C ± 1°C) in a reactor; S2, the solution enters a three-stage spiral tapered pipe (contraction ratio 3:1) at a flow rate of 2 m / s, and ultrasonic monitoring (frequency 35 kHz) is turned on; S3, according to the formula v = 20 × 500000 mL / 20 min = 500 mL / min pulse addition of alkylcyclohexylphenol supersaturated solution, maintaining S = 1.4; S4, after 120 min of continuous crystallization, the grain size was 15 ± 1 mm × 4 ± 0.3 mm, and XRD analysis showed that the characteristic peak intensity deviation was <5%; S5, centrifugation (3000 rpm) and vacuum drying (50 ° C / 2 h), HPLC purity 99.99%, solvent residue <100 ppm.

[0027] Please refer to Figures 1 to 9 , a preparation device for strip-shaped flake crystal alkylcyclohexylphenol, steps S1 to S4 are completed in an integrated device, the integrated device includes a connecting pipe 1, the two sides of the connecting pipe 1 are respectively fixedly connected with a liquid feed pipe 2 and a solid feed port 3, the top of the connecting pipe 1 is provided with a condenser 11, the bottom end of the connecting pipe 1 is fixedly connected with a reaction bin 4, the bottom end of the reaction bin 4 is fixedly connected with a discharge pipe 5, the bottom end of the discharge pipe 5 is fixedly connected with a centrifugal bin 6, a spiral tapered pipe 7 is installed inside the centrifugal bin 6, the bottom end of the centrifugal bin 6 is fixedly connected with a mounting seat 25, the bottom end of the mounting seat 25 is provided with a collecting bucket 26, the inner cavity of the collecting bucket 26 is provided with a filter basket 10, the outer wall of the reaction bin 4 is provided with a heating jacket 12, the outer wall of the centrifugal bin 6 is provided with an insulation jacket 13, one side outer wall of the mounting seat 25 is fixedly connected with a leaching pipe 14, and one side outer wall of the reaction bin 4 is fixedly connected with an air inlet pipe 15.

[0028] The bottom end of the inner wall of the reaction bin 4 is provided with a baffle 16, and the bottom end of the inner wall of the reaction bin 4 is symmetrically provided with a limit rod 17 and a screw rod 18 that pass through the baffle 16. The limit rod 17 is fixedly connected to the reaction bin 4, and the outer bottom end of the reaction bin 4 is installed with a first motor 19. The screw rod 18 is connected to the output end of the first motor 19 and is rotatably connected to the reaction bin 4. A filter plate 20 is installed in the inner cavity of the discharge pipe 5. The inner cavity of the centrifugal bin 6 is rotatably connected to a rotating plate 21 with an upper surface having an inwardly concave arc shape. The rotating plate 21 is fixedly connected to The top of the spiral tapered pipe 7 is hollow and the upper end opening is located at the top of the rotating plate 21. The lower outer wall of the spiral tapered pipe 7 is fixedly connected to the first bevel gear 22. The outer wall of the mounting seat 25 is installed with a second motor 24. The output end of the second motor 24 is connected to the second bevel gear 23. The second bevel gear 23 is in contact with the first bevel gear 22. The collecting bucket 26 is installed on the bottom end of the mounting seat 25 through the mounting mechanism 8. The inner wall of the filter basket 10 is scraped by the scraping mechanism 9.

[0029] In this embodiment, alkylcyclohexylphenol is added through the solid feed port 3, and the solvent is added through the liquid feed pipe 2. The temperature is increased and dissolved in the reaction chamber 4 to form a supersaturated solution. The first motor 19 is started, and the first motor 19 drives the screw 18 to rotate. The rotation of the screw 18 drives the baffle 16 to move and open the discharge pipe 5. At the same time, the air inlet pipe 15 injects nitrogen into the reaction chamber 4 to pressurize it to 0.2 MPa. The solution flows into the spiral tapered pipe 7 through the discharge pipe 5. At this time, the second motor 24 is started and the second motor 24 is driven. The rotation drives the second bevel gear 23 to rotate, and the rotation of the second bevel gear 23 drives the first bevel gear 22 to rotate. The rotation of the first bevel gear 22 drives the spiral tapered pipe 7 to rotate, so that the solution moves along the pipe wall, forming a vortex crystallization environment in the pipe, and then easily enters the filter basket 10. Through the cooperation of the parts in the scraping mechanism 9, the liquid passes through the filter basket 10 and flows into the collection barrel 26. The crystals remain in the filter basket 10. After that, the elution liquid can be injected into the filter basket 10 through the elution pipe 14, so that the crystals in the filter basket 10 are cleaner.

[0030] Please refer to Figures 4 to 7The mounting mechanism 8 includes a first docking plate 801, which is symmetrically fixedly connected to both sides of the bottom end of the mounting seat 25, and a second docking plate 802 is symmetrically fixedly connected to both sides of the top of the collecting barrel 26. The top of the second docking plate 802 is fixedly connected to a connecting rod 803, and a fixing groove 804 is provided on the outer wall of the connecting rod 803. A connecting groove 805 is provided on the outer wall of the first docking plate 801. The interior of the first docking plate 801 is slidably connected to a fixing block 806 extending to the inner cavity of the connecting groove 805. A first spring 807 is connected between the fixing block 806 and the first docking plate 801. The first docking plate The interior of 801 is located below the fixed block 806 and is slidably connected to a push plate 808 on the side away from the first spring 807. The outer wall of the first docking plate 801 is rotatably connected to a rotating column 810. One end of the rotating column 810 is fixedly connected to a threaded rod 809. The threaded rod 809 passes through the push plate 808. The top of the filter basket 10 is fixedly connected to an annular plate 811. The top of the annular plate 811 is symmetrically provided with a slot 812. The top of the collecting barrel 26 is provided with a placement groove 813. The inner wall of the placement groove 813 is symmetrically fixedly connected with an insertion rod 814. The bottom end of the inner wall of the collecting barrel 26 is fixedly connected to a support seat 815.

[0031] In this embodiment: when installing the collection barrel 26 and the filter basket 10, the filter basket 10 is placed in the collection barrel 26 until the bottom end of the filter basket 10 contacts the support seat 815, the annular plate 811 is displaced into the placement groove 813, and the insertion rod 814 is inserted into the slot 812 to position the filter basket 10. Then, the collection barrel 26 is moved so that the first docking plate 801 and the second docking plate 802 are aligned, the connecting rod 803 is inserted into the connecting groove 805, and the fixing block 806 is engaged into the fixing groove 804 by the elastic force of the first spring 807, and the collection barrel 26 and the filter basket 10 are installed.

[0032] When removing the collection barrel 26, rotate the rotating column 810, and the rotating column 810 drives the threaded rod 809 to rotate, and the threaded rod 809 drives the push plate 808 to move. The push plate 808 moves and contacts the fixed block 806, pushing the fixed block 806 to move. The fixed block 806 moves out of the fixed groove 804, canceling the fixation of the connecting rod 803. At this time, the connecting rod 803 is moved out of the connecting groove 805, thereby performing the removal operation of the collection barrel 26.

[0033] Please refer to Figures 7 to 9The scraping mechanism 9 includes a third motor 901, which is installed at the bottom end of the collecting barrel 26. The output end of the third motor 901 is connected to a connecting shaft 902. The top of the connecting shaft 902 is fixedly connected to a square rod 903. The square rod 903 is rotatably connected to the top of the support seat 815. The bottom of the filter basket 10 is rotatably connected to a rotating disk 904. The bottom end of the rotating disk 904 is provided with a square groove 905. The top of the rotating disk 904 is fixedly connected to a vertical rod 906. The outer wall of the vertical rod 906 is opposite to the bottom of the filter basket 10. It is fixedly connected with a cross bar 907, and the outer wall of the cross bar 907 is slidably connected with a scraper 908. The outer wall of the scraper 908 is obliquely fixedly connected with a guide frame 909 with a strip guide groove. The interior of the vertical bar 906 is slidably connected with a cross 910 extending from the vertical bar 906. The horizontal arms on both sides of the cross 910 extend from the two ends of the vertical bar 906 and are symmetrically fixedly connected with sliding bars 911. The sliding bars 911 are slidably connected to the inner wall of the strip guide groove, and the top of the cross 910 is fixedly connected with a downward pressure cylinder 912.

[0034] In this embodiment, during the installation of the collection barrel 26 and the filter basket 10, the filter basket 10 moves to the top of the support seat 815. At this time, the square rod 903 is inserted into the square groove 905, and the square rod 903 is displaced to contact the cross 910, pushing the cross 910 to move. The displacement of the cross 910 drives the sliding rod 911 to move. The sliding rod 911 slides in the guide frame 909 to push the scraper 908 to move. The scraper 908 moves along the cross bar 907, and the scraper 908 is separated from the inner wall of the filter basket 10. When the collection barrel 26 and the filter basket 10 are installed, the third motor 901 can be started. The operation of the third motor 901 drives the connecting shaft 902 to rotate. The rotation of the connecting shaft 902 drives the square rod 903 to rotate. The rotation of the square rod 903 drives the vertical rod 906 to rotate through the rotating disk 904. The rotation of the vertical rod 906 drives the scraper 908 to rotate, stirring the solution in the filter basket 10, thereby performing a centrifugal separation operation on the solution in the filter basket 10.

[0035] After the collection barrel 26 and the filter basket 10 are removed, the filter basket 10 is removed from the collection barrel 26 and the pressure cylinder 912 is pushed downward. The displacement of the pressure cylinder 912 drives the cross 910 to move, and the displacement of the cross 910 drives the sliding rod 911 to move. The sliding rod 911 slides along the inner wall of the guide frame 909 and drives the scraper 908 to move. The scraper 908 moves and contacts the inner wall of the filter basket 10. The pressure cylinder 912 can then be rotated. The rotation of the pressure cylinder 912 drives the vertical rod 906 to rotate. The rotation of the vertical rod 906 drives the scraper 908 to rotate, scraping off the crystals on the inner wall of the filter basket 10. This design facilitates the rapid installation and removal of the filter basket 10. When the filter basket 10 is installed, the solution in the filter basket 10 is centrifuged by the rotation of the scraper 908. After the filter basket 10 is removed, the crystals on the inner wall of the filter basket 10 are scraped off by the rotation of the scraper 908.

[0036] Please refer to Figures 4 to 7 The outer wall of the annular plate 811 fits with the inner wall of the placement groove 813, the inner wall of the slot 812 fits with the outer wall of the insertion rod 814, the inner wall of the connecting groove 805 fits with the outer wall of the connecting rod 803, and the protruding end of the fixing block 806 is provided with a bevel and the outer wall of the protruding end fits with the inner wall of the fixing groove 804.

[0037] In this embodiment: the filter basket 10 is placed in the collection barrel 26 until the bottom end of the filter basket 10 contacts the support seat 815, the annular plate 811 is displaced into the placement groove 813, and the insertion rod 814 is inserted into the slot 812 to position the filter basket 10. Then, the collection barrel 26 is moved so that the first docking plate 801 and the second docking plate 802 are aligned, the connecting rod 803 is inserted into the connecting groove 805, and the fixing block 806 is engaged into the fixing groove 804 by the elastic force of the first spring 807, and the collection barrel 26 and the filter basket 10 are installed.

[0038] Please refer to Figures 4 to 7 The fixing block 806 is L-shaped, and a threaded hole is provided on the outer wall of the push plate 808, which matches the threaded rod 809.

[0039] In this embodiment: the rotating column 810 is rotated, and the rotating column 810 drives the threaded rod 809 to rotate, and the threaded rod 809 drives the push plate 808 to move. The push plate 808 moves and contacts the fixed block 806, pushing the fixed block 806 to move. The fixed block 806 moves out of the fixed groove 804, and the fixation of the connecting rod 803 is cancelled.

[0040] Please refer to Figures 7 to 9 The outer wall of the square rod 903 fits with the inner wall of the square groove 905 , and the inner wall of the strip guide groove fits with the outer wall of the slide rod 911 .

[0041] In this embodiment: during the installation of the collection barrel 26 and the filter basket 10, the filter basket 10 moves to the top of the support seat 815. At this time, the square rod 903 is inserted into the square groove 905. The square rod 903 moves and contacts the cross 910, pushing the cross 910 to move. The displacement of the cross 910 drives the sliding rod 911 to move. The sliding rod 911 slides in the guide frame 909 and pushes the scraper 908 to move. The scraper 908 moves along the cross bar 907 so that the scraper 908 is separated from the inner wall of the filter basket 10.

[0042] The strip-shaped flaky crystalline alkylcyclohexylphenol prepared in Example 1 was subjected to product performance testing. The test methods and test results are shown in Table 1 below: Table 1 Product performance data verification of Example 1

[0043] The results show that this embodiment achieves a dimensional coefficient of variation (CV) of only 6% under standard process parameters, far below the industry standard threshold of 20%. The lattice defect rate of 0.03% breaks the existing technological limit (conventional processes are >0.1%). Synchrotron radiation diffraction shows that lattice distortion is mainly concentrated in the edge region (<5μm), while the core region perfectly matches the single crystal model. After accelerated aging at 80°C, the defect rate only increases to 0.035%, demonstrating that the eddy current field-induced (001) crystal plane directional growth significantly improves thermal stability, solving the core pain point of high-temperature applications of liquid crystal materials.

[0044] Example 2

[0045] A method for preparing alkylcyclohexylphenol strip-shaped flake crystals, the steps being the same as those in Example 1 except for the following differences: S1: adding 0.2 wt % of alkylcyclohexylphenol microcrystals (particle size 50 μm ± 5 μm) as seed crystals after dissolution; S3: Pulse addition of a supersaturated solution containing 0.1 wt% microcrystals. The strip-shaped flaky alkylcyclohexylphenol prepared in Example 1 was subjected to product performance testing. The test methods and test results are shown in Table 2 below: Table 2 Product performance data verification of Example 2 (seed crystal optimization type)

[0046] The addition of microseeds increased the nucleation density by 3 times, but the size distribution CV value dropped to 5%, demonstrating that the seeds effectively inhibited secondary nucleation. EBSD data showed that the (001) plane orientation reached 98.3% ± 0.5%, with an orientation deviation angle of ≤ 2°, far superior to the 92.5% ± 3.2% of the unseeded group. XRD refinement revealed that lattice distortion could be reduced to 0.005 eV / atom. The addition of microseeds provided directional growth sites, transforming the Ostwald ripening process from random nucleation to controlled growth. Although the initial nucleation density increased by 3 times, the crystal coalescence rate increased by 5 times, and the final CV value dropped to 5%.

[0047] The results of Example 3 show A method for preparing alkylcyclohexylphenol strip-shaped flaky crystals, with the following differences: S1: the mass ratio of alkylcyclohexylphenol to ethanol is 1:1.6; S2: centrifugal speed 120 rpm, pipe temperature 65 °C; S3: Rehydration rate 2.0 mL / min. The strip-shaped flaky crystalline alkylcyclohexylphenol prepared in Example 3 was subjected to product performance testing. The test method and test results are shown in Table 3 below: Table 3 Product performance data verification of Example 3 (large size customized type)

[0048] Results showed that even under the extreme conditions of a 4:1 pipe contraction ratio, the crystal width was precisely controlled to 5.5±0.2mm (RSD=3.6%), exceeding the ±1mm fluctuation limit of conventional processes. Scanning electron microscopy (SEM) revealed that the thickness of the deposited layer on the pipe wall was less than 10μm after 120 hours of continuous operation, far below the critical scaling threshold of 200μm. Energy consumption data revealed key innovations: vortex flow field replacing mechanical agitation reduced mass transfer energy consumption by 62%, and pulse rehydration technology reduced solvent evaporation losses by 41%. The resulting unit energy consumption of 1.7 kW·h / kg was a 43% decrease compared to the industry benchmark (3.0 kW·h / kg).

[0049] Example 4 The same batch of raw materials was processed using the patented method of CN103553878B: multi-reactor series gradient cooling crystallization (without eddy current field and pulse rehydration), with a mechanical stirring speed of 200 rpm and a cooling rate of 0.5°C / min. The strip-shaped, flake-shaped alkylcyclohexylphenol prepared in Example 4 was subjected to product performance testing. The test methods and test results are shown in Table 4 below: Table 4 Product performance data verification of Example 4

[0050] The results show that the 28% CV value of the size is due to the difference in nucleation position caused by the temperature gradient (infrared thermal imaging shows ±8℃ fluctuation). The grain boundary melting phenomenon was confirmed by SEM-EDS: impurity elements (Na +, Cl - ) is enriched at the grain boundaries (concentrations reach 1200 ppm), lowering the local melting point to 75°C. The underlying reason for the LCI value of 0.75 is the (001) plane orientation disorder (EBSD shows a maximum deviation angle of 42°), which leads to a failure in liquid crystal cell gap control. This data quantitatively explains the display color shift problem described in the background art.

[0051] The above is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with this technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solutions and inventive concepts of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A method for preparing strip-shaped flaky crystal alkylcyclohexylphenol, characterized in that: The following steps are involved: S1: dissolving alkylcyclohexylphenol and solvent at a mass ratio of 1:(1.2-1.6) at elevated temperature to form a supersaturated solution; S2: introducing the solution prepared in step S1 into a spiral tapered pipe (7) with a centrifugal function, maintaining the pipe temperature and starting the centrifugal rotation, so that the solution moves along the pipe wall, forming a vortex crystallization environment in the pipe; S3: Pulse-feed a supersaturated solution of alkylcyclohexylphenol into the pipeline at a rate of 0.5-2 mL / min, controlling the supersaturation of the solution S = 1.2-1.5 to induce Ostwald ripening; S4: Repeat steps S2 and S3 to perform multi-stage dynamic crystallization, so that the crystallization solution circulates in the spiral tapered pipe (7) 3 to 5 times until the crystal length reaches 9 to 17 mm and the width reaches 2 to 5.5 mm; S5: Start the scraping mechanism (9) to peel off the crystals, centrifuge and then dry to obtain strip-shaped alkylcyclohexylphenol crystals.

2. The method for preparing a strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 1, wherein: The heating and dissolving in step S1 is carried out at a temperature within the range of 65 to 80° C.; the added solvent is ethanol.

3. The method for preparing a strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 1, wherein: The diameter contraction ratio of the spiral tapered pipe (7) in step S2 is 2:1 to 4:1, the pipe temperature is maintained at 45 to 65°C, and the centrifugal speed is started at 80 to 120 rpm.

4. The equipment used in the method for preparing a strip-shaped flaky crystal type alkylcyclohexylphenol according to any one of claims 1 to 3, characterized in that: Steps S1 to S4 are completed in an integrated device, which includes a connecting pipe (1), wherein both sides of the connecting pipe (1) are fixedly connected to a liquid feed pipe (2) and a solid feed port (3), a condenser (11) is installed at the top of the connecting pipe (1), a reaction chamber (4) is fixedly connected to the bottom end of the connecting pipe (1), a discharge pipe (5) is fixedly connected to the bottom end of the reaction chamber (4), a centrifugal chamber (6) is fixedly connected to the bottom end of the discharge pipe (5), and a spiral is installed inside the centrifugal chamber (6). A tapered pipe (7), the bottom end of the centrifugal chamber (6) is fixedly connected to a mounting seat (25), the bottom end of the mounting seat (25) is installed with a collecting bucket (26), the inner cavity of the collecting bucket (26) is provided with a filter basket (10), the outer wall of the reaction chamber (4) is installed with a heating jacket (12), the outer wall of the centrifugal chamber (6) is installed with a heat-insulating jacket (13), one side outer wall of the mounting seat (25) is fixedly connected to a leaching pipe (14), and one side outer wall of the reaction chamber (4) is fixedly connected to an air inlet pipe (15).

5. The preparation equipment for a strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 4, characterized in that: The bottom end of the inner wall of the reaction bin (4) is provided with a baffle (16), and the bottom end of the inner wall of the reaction bin (4) is symmetrically provided with a limit rod (17) and a screw rod (18) penetrating the baffle (16), the limit rod (17) is fixedly connected to the reaction bin (4), the outer bottom end of the reaction bin (4) is provided with a first motor (19), the screw rod (18) is connected to the output end of the first motor (19) and is rotatably connected to the reaction bin (4), the inner cavity of the discharge pipe (5) is provided with a filter plate (20), and the inner cavity of the centrifugal bin (6) is rotatably connected with a rotating plate (21) whose upper surface is in the shape of an inner concave arc surface, and the rotating plate (21) is fixed. The spiral converging pipe (7) is connected to the top end thereof. The spiral converging pipe (7) is hollow and has an upper opening located at the top end of the rotating plate (21). The lower outer wall of the spiral converging pipe (7) is fixedly connected to a first bevel gear (22). The outer wall of the mounting seat (25) is mounted with a second motor (24). The output end of the second motor (24) is connected to a second bevel gear (23). The second bevel gear (23) is in contact with the first bevel gear (22). The collecting barrel (26) is mounted on the bottom end of the mounting seat (25) via a mounting mechanism (8). The inner wall of the filter basket (10) is scraped by a scraping mechanism (9).

6. The preparation equipment for strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 5, characterized in that: The mounting mechanism (8) includes a first docking plate (801), the first docking plate (801) is symmetrically fixedly connected to both sides of the bottom end of the mounting seat (25), the second docking plates (802) are symmetrically fixedly connected to both sides of the top end of the collecting barrel (26), the top end of the second docking plate (802) is fixedly connected to a connecting rod (803), the outer wall of the connecting rod (803) is provided with a fixing groove (804), the outer wall of the first docking plate (801) is provided with a connecting groove (805), the interior of the first docking plate (801) is slidably connected to a fixing block (806) extending to the inner cavity of the connecting groove (805), a first spring (807) is connected between the fixing block (806) and the first docking plate (801), and the first docking plate The interior of (801) is located below the fixed block (806) and is slidably connected to a push plate (808) on one side away from the first spring (807). The outer wall of the first docking plate (801) is rotatably connected to a rotating column (810). One end of the rotating column (810) is fixedly connected to a threaded rod (809). The threaded rod (809) passes through the push plate (808). The top of the filter basket (10) is fixedly connected to an annular plate (811). The top of the annular plate (811) is symmetrically provided with a slot (812). The top of the collection barrel (26) is provided with a placement groove (813). The inner wall of the placement groove (813) is symmetrically fixedly connected to an insertion rod (814). The bottom end of the inner wall of the collection barrel (26) is fixedly connected to a support seat (815).

7. The preparation equipment for strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 6, characterized in that: The scraping mechanism (9) includes a third motor (901), the third motor (901) is installed at the bottom end of the collecting barrel (26), the output end of the third motor (901) is connected to a connecting shaft (902), the top end of the connecting shaft (902) is fixedly connected to a square rod (903), the square rod (903) is rotatably connected to the top end of the support seat (815), the bottom of the filter basket (10) is rotatably connected to a rotating disk (904), the bottom end of the rotating disk (904) is provided with a square groove (905), the top end of the rotating disk (904) is fixedly connected to a vertical rod (906), the vertical rod (906) 06) is symmetrically fixedly connected to the outer wall of the cross bar (907), the outer wall of the cross bar (907) is slidably connected to the scraper (908), the outer wall of the scraper (908) is obliquely fixedly connected to the guide frame (909) with a strip guide groove, the interior of the vertical bar (906) is slidably connected to a cross (910) extending from the vertical bar (906), the two side horizontal arms of the cross (910) extend from the two ends of the vertical bar (906) and are symmetrically fixedly connected to the sliding rods (911), the sliding rods (911) are slidably connected to the inner wall of the strip guide groove, and the top of the cross (910) is fixedly connected to the lower pressure cylinder (912).

8. The preparation equipment for strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 7, characterized in that: The outer wall of the annular plate (811) fits with the inner wall of the placement groove (813), the inner wall of the slot (812) fits with the outer wall of the insertion rod (814), the inner wall of the connecting groove (805) fits with the outer wall of the connecting rod (803), and the extended end of the fixing block (806) is provided with an inclined surface and the outer wall of the extended end fits with the inner wall of the fixing groove (804).

9. The preparation equipment for strip-shaped flaky crystal type alkylcyclohexylphenol according to claim 8, characterized in that: The fixing block (806) is L-shaped, and a threaded hole is provided on the outer wall of the push plate (808), and the threaded hole matches the threaded rod (809); the outer wall of the square rod (903) fits with the inner wall of the square groove (905), and the inner wall of the strip guide groove fits with the outer wall of the slide rod (911).

10. The strip-shaped flaky crystal alkylcyclohexylphenol prepared by the method for preparing strip-shaped flaky crystal alkylcyclohexylphenol according to any one of claims 1 to 3, characterized in that: The strip-shaped sheet single crystal obtained by the process described in steps S1-S5 has a thickness of 0.1 to 0.3 mm, an aspect ratio of 3:1 to 5:1, and a lattice defect rate of ≤0.05%.

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