A preparation process and equipment for high-purity benzophenone

Abstract

The present invention relates to the technical field of preparation process and equipment of high-purity benzophenone, specifically, to a preparation process and equipment of high-purity benzophenone, wherein a preparation equipment of high-purity benzophenone includes a first shell, the outer side of the first shell is rotatably connected to a second shell for crystallization, the outer ring of the second shell is fixedly connected to a heating ring, the upper side of the first shell is connected to a cover, the upper side of the cover is fixedly connected to a pressure gauge, one side of the pressure gauge is fixedly connected to several delivery pipelines, the inner annular array of the first shell is provided with several drainage holes, the inner wall of the first shell is slidably connected to a water retaining ring, the water retaining ring is used to block several drainage holes, and the first shell is connected to a stirring assembly for quickly mixing the solution in the first shell. Through the above technical scheme, the reaction efficiency, crystallization quality and cleaning efficiency of the benzophenone solution are improved.

Description

Technical Field

[0001] The invention relates to the technical field of a preparation process and equipment for high-purity benzophenone, and specifically to a preparation process and equipment for high-purity benzophenone. Background Art

[0002] Benzophenone (chemical formula is C 13 H 10 Benzophenone (BPA) is an organic compound belonging to the aromatic ketone family. It usually appears as a colorless to light yellow crystalline solid with a unique aromatic odor. It is synthesized from benzene and benzoyl through the Friedel-Crafts acylation reaction. The structure of benzophenone contains two benzene rings and a ketone group. Its molecular structure makes it exhibit unique properties in terms of ultraviolet absorption, photostability and chemical reactivity. Benzophenone is widely used in industrial production, especially in light stabilizers, ultraviolet absorbers and plasticizers. It is widely used in cosmetics, plastics and coatings as a UV absorber. It can effectively absorb ultraviolet rays, prevent ultraviolet rays from damaging products, and extend the service life of materials. In addition, benzophenone is also an important photocatalyst and has important applications in photochemical reactions and organic synthesis. In the laboratory, benzophenone is often used as an intermediate in organic synthesis and participates in the synthesis of other organic compounds. It has strong reactivity and can react with different chemical reagents to carry out a variety of reactions such as acylation and reduction. In short, benzophenone plays an important role in the chemical industry and daily life with its unique chemical properties and wide range of applications.

[0003] In the prior art, there is a benzophenone purification device with a publication number of "CN220424587U", which includes a device body, a mounting seat is installed inside the device body through a bearing, and a driving motor is installed on the mounting seat through a rotating shaft, a circular sleeve is connected to the mounting seat through a spring sheet, a stirring paddle is arranged inside the circular sleeve, a scraper is arranged on the side surface of the stirring paddle, and a damping spring is arranged on one side of the scraper, a first gear is arranged on the surface of the stirring paddle, and the first gear is meshed with a second gear, the second gear is installed on the surface of a rotating rod, and a striking rod is arranged on the surface of the rotating rod.

[0004] The above technology uses a stirring rod to stir the mixed solution, and at the same time, the benzophenone crystals solidified on the inner wall of the cleaning device are removed by a scraper. The upper end of the scraper is equipped with a beating rod, which shakes off the excess crystals accumulated on the scraper through the hammering action, thereby completing the crystallization cleaning of the stirring paddle and the scraper surface, and improving the convenience of cleaning. However, this technology still has the following problems: First, the mixed solution of benzophenone only needs slight stirring to complete the mixing in practical applications. If the stirring is too violent, it may cause the solvent to evaporate too quickly or the solution to be violently disturbed, which will affect the crystallization process and reduce the purification effect of benzophenone. Secondly, when benzophenone crystals are solidified, there are still some residual solutions in the crystals, and the scraper rotates synchronously with the stirring rod. While scraping off the crystals, the stirring rod will break some of the crystals again, causing some of the crystals to dissolve back into the mixed solution again, further reducing the purification effect. In addition, the side of the scraper is parallel to the axis of the device body, which will cause the crystals to be squeezed along the side of the scraper when scraping off the crystals, and part of the crystals will be pushed to the upper space of the inner wall of the device, thereby reducing the crystal output effect. Summary of the invention

[0005] The invention provides a preparation device for high-purity benzophenone, which improves the reaction efficiency and crystallization quality of a benzophenone solution and the cleaning efficiency of the device.

[0006] The technical solution of the present invention is as follows: A high-purity benzophenone preparation device comprises a first shell; The outer side of the first shell is rotatably connected to a second shell for crystallization, the outer ring of the second shell is fixedly connected to a heating ring, the upper side of the first shell is connected to a cover, the upper side of the cover is fixedly connected to a pressure gauge, and one side of the pressure gauge is fixedly connected to a plurality of conveying pipes; A plurality of drainage holes are provided in an annular array in the first shell, and a water retaining ring is slidably connected to the inner wall of the first shell, and the water retaining ring is used to block the plurality of drainage holes; The first shell is connected to a stirring component for quickly mixing the solution in the first shell; A blocking block is fixedly connected to the outside of the first shell, and a discharge pipe is fixedly connected to the lower side of the second shell, wherein the blocking block is used to block the outlet of the discharge pipe; The first shell outer wall and the second shell inner wall are respectively fixedly connected with a first scraper and a second scraper, and the first scraper and the second scraper are tightly abutted against the second shell inner wall and the first shell outer wall; A first motor is fixedly connected to the lower side of the second shell, and a driving shaft of the first motor is fixedly connected to the bottom of the first shell.

[0007] Furthermore, the stirring assembly includes a lifting plate, the lifting plate is slidably abutted against the inner wall of the first shell, a limiting sleeve is fixedly connected to the lower side of the lifting plate, a limiting column is slidably connected inside the limiting sleeve, and an isolation plate is fixedly connected to the lower end of the limiting column; A transmission sleeve is fixedly connected to the lower side of the lifting plate, a magnetic rotor is rotatably connected inside the transmission sleeve, a stirring rod is magnetically connected to the upper side of the magnetic rotor, a transmission column is threadedly connected inside the transmission sleeve, and a driving column is rotatably connected inside the transmission column; A second motor is fixedly connected to the lower side of the isolation plate, and a driving shaft of the second motor is fixedly connected to the driving column; The driving column is slidably engaged with the magnetic attraction rotary machine; A locking assembly is connected between the transmission column and the second motor.

[0008] Further, the positioning assembly includes a positioning plate, a plurality of reset columns are fixedly connected to the lower side of the positioning plate, each of the reset columns is slidably connected to the isolation plate, each reset column is sleeved with a reset spring, and the two ends of the reset spring are respectively in contact with the lower side of the isolation plate and the reset column; The first clamping cylinder is rotatably connected to the clamping plate, the first clamping cylinder is clamped with the driving shaft of the second motor, the lower side of the transmission column is fixedly connected with the second clamping cylinder, and the first clamping cylinder and the second clamping cylinder are mutually engaged and clamped; A locking cylinder is fixedly connected to the isolation plate, a locking block is fixedly connected to the telescopic shaft of the locking cylinder, and an upper inclined surface of the locking block abuts against a side edge of the locking plate.

[0009] Furthermore, the first scraper and the second scraper are both arranged in a spiral manner.

[0010] Furthermore, the upper side surface of the lifting plate is an arc-shaped surface which is high in the middle and low around.

[0011] Furthermore, a partition cover plate with a filter screen is detachably fixedly connected to the lower side of the discharge pipe.

[0012] The beneficial effects of the present invention are: The stirring component has two working modes (fast stirring mode and excessive stirring to prevent crystal dissolution mode). Combined with the solution level control and automatic cleaning function, it significantly improves the reaction efficiency, crystal quality and cleaning efficiency of the benzophenone solution. Through fine control of the stirring and crystallization process, it not only optimizes the production process, but also reduces the labor intensity of workers, improves the versatility and automation level of the equipment, and improves the purification effect of benzophenone crystals. The first motor drives the first shell and the second shell to rotate relative to each other. Through the relative rotation of the first shell and the second shell combined with the spiral scraping action of the scraper and the scraper, this design effectively enhances the removal effect of the crystals and improves the cleaning efficiency of the inner and outer walls of the equipment. It not only ensures the timely removal of the crystals and avoids the impact of accumulation on the operation of the equipment, but also improves the stability of the crystallization reaction and the product quality. In addition, this removal mechanism greatly reduces the workload of equipment maintenance and manual cleaning, improves the automation level and production efficiency of the equipment, and enhances the long-term stability and sustainability of the equipment.

[0013] Another object of the present invention is to provide a preparation process of high-purity benzophenone, thereby improving the purity of benzophenone crystals and optimizing the quality and yield of the crystals.

[0014] The following steps are involved: S100: Raw material preparation: prepare benzene, benzoyl chloride, a suitable catalyst, and a solvent for use; S200: Mixing preparation: clean the inside of the first shell and the second shell, dry them, add benzene and benzoyl chloride into the first shell, add the catalyst, mix the solution, and finally transfer the mixed solution to the second shell for heat treatment and crystallization; S300: scraping operation: start the first motor to drive the first shell and the second shell to rotate relative to each other, so that the crystals and the remaining mixed liquid in the second shell are collected by the first scraper and the second scraper, and finally discharged through the discharge pipe, and the solid-liquid separation is performed, and then the relative positions of the first shell and the second shell are reset; S400: Purification: The initially obtained crystals and a mixed solvent of dichloromethane and ethanol are added to the first shell for mixing, and then the mixed solution is transferred to the second shell. After setting the temperature, a secondary crystallization operation is performed, and then a secondary scraping operation is performed: a more purified benzophenone is collected and dried; S500: Purity test: Use high performance liquid chromatography (HPLC) or gas chromatography (GC) to test the purity of benzophenone to ensure that it meets product requirements; S600: Finished Product Packaging and Storage: Package the purified benzophenone in airtight containers and store them in a dry, cool place.

[0015] Further, the step S200 of mixing preparation includes: S210: Benzene and benzoyl chloride are quantitatively input into the first shell through each delivery pipeline according to the molar ratio, and then a catalyst of 10%-20% of the used amount of benzoyl chloride is dripped into it, and then a stirring component is started to quickly mix the mixed solution; S220: The mixed solution being mixed is transferred to the second shell through the drainage hole, and then the stirring assembly is reset to make the first shell and the second shell become separate chambers, and the heating ring is started to heat the mixed solution, so that the mixed solution is placed in the sealed chamber for crystallization.

[0016] Another beneficial effect of the present invention is: The quality and yield of crystallization are optimized, and the impurities in the crystals can be further purified and removed to improve the purity of the raw materials, which helps to improve the selectivity and conversion rate of subsequent reactions. When high-purity benzophenone is used as a reactant, it can play a better role in the subsequent synthesis process, avoiding the interference of impurities on the reaction, and through real-time detection of crystals precipitated twice or multiple times, it is used to test the purity of the crystals, and then classify crystals of different purities, summarize experimental data, and use raw materials of different purities in different usage scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0018] Figure 1 It is an enlarged schematic diagram of the present invention; Figure 2 This is a partial half-section enlarged schematic diagram of the present invention. Figure 1 ; Figure 3 for Figure 2 A is an enlarged schematic diagram; Figure 4 This is a partial half-section enlarged schematic diagram of the present invention. Figure 2 ; Figure 5 for Figure 4 A magnified schematic diagram of B; Figure 6 This is a partial enlarged explosion diagram of the present invention. Figure 1 ; Figure 7 This is a partial enlarged explosion diagram of the present invention. Figure 2 .

[0019] In the figure: 11, the first shell; 12, the second shell; 13, the heating ring; 14, the sealing cover; 15, the pressure gauge; 16, the water retaining ring; 17, the blocking block; 18, the discharge pipe; 181, the partition cover; 19, the first scraper; 110, the second scraper; 111, the drainage hole; 112, the first motor; 113, the conveying pipeline; 21, the lifting plate; 22, the limiting sleeve; 23, the limiting column; 24, the isolation plate; 25, the transmission sleeve; 26, the magnetic rotor; 27, the stirring rod; 28, the transmission column; 29, the driving column; 210, the second motor; 31, the locking plate; 32, the reset column; 33, the reset spring; 34, the first locking cylinder; 35, the second locking cylinder; 36, the locking cylinder; 37, the locking block. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. 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 creative work are within the scope of protection of the present invention. Example

[0021] like Figure 1 to Figure 7 As shown, this embodiment provides a preparation device for high-purity benzophenone, including a first shell 11; The outer side of the first shell 11 is rotatably connected to a second shell 12 for crystallization, the outer ring of the second shell 12 is fixedly connected to a heating ring 13, the upper side of the first shell 11 is connected to a cover 14, the upper side of the cover 14 is fixedly connected to a pressure gauge 15, and one side of the pressure gauge 15 is fixedly connected to a plurality of delivery pipes 113; A plurality of drainage holes 111 are provided in an annular array in the first shell 11, and a water retaining ring 16 is slidably connected to the inner wall of the first shell 11, and the water retaining ring 16 is used to block the plurality of drainage holes 111; The water retaining ring 16 moves downward under the action of gravity, and then when the water retaining ring 16 slides to the lowest position under the limit of the inner wall feature of the first shell 11, it can just block the plurality of drainage holes 111, so that the first shell 11 and the second shell 12 can form two separate chambers, thereby improving the sealing and independence of different chambers during operation; The first shell 11 is connected to a stirring component for quickly mixing the solution in the first shell 11; The stirring component provides two working modes (fast stirring mode and excessive stirring to prevent crystal dissolution mode). Combined with the solution level control and automatic cleaning functions, it significantly improves the reaction efficiency, crystallization quality and cleaning efficiency of the benzophenone solution. By finely controlling the stirring and crystallization process, it not only optimizes the production process, but also reduces the labor intensity of workers, improves the versatility and automation level of the equipment, and improves the purification effect of benzophenone crystals.

[0022] A blocking block 17 is fixedly connected to the outside of the first housing 11, and a discharge pipe 18 is fixedly connected to the bottom of the second housing 12. The blocking block 17 is used to block the outlet of the discharge pipe 18. The first scraper 19 and the second scraper 110 are fixedly connected to the outer wall of the first shell 11 and the second shell 12. The first scraper 19 and the second scraper 110 are tightly abutted against the inner wall of the second shell 12 and the outer wall of the first shell 11. A first motor 112 is fixedly connected to the lower side of the second housing 12, and a driving shaft of the first motor 112 is fixedly connected to the bottom of the first housing 11; The first motor 112 drives the first shell 11 and the second shell 12 to rotate relative to each other. The relative rotation of the first shell 11 and the second shell 12 combined with the spiral scraping action of the first scraper 19 and the second scraper 110 effectively enhances the crystal removal effect and improves the cleaning efficiency of the inner and outer walls of the equipment. It not only ensures the timely removal of crystals and avoids the impact of accumulation on equipment operation, but also improves the stability of the crystallization reaction and product quality. In addition, this cleaning mechanism greatly reduces the workload of equipment maintenance and manual cleaning, improves the automation level and production efficiency of the equipment, and enhances the long-term stability and sustainability of the equipment. In summary, through multiple innovative technologies such as relative rotation, scraping by the first scraper 19 and the second scraper 110, sealing by the water retaining ring 16, and regulation of the stirring component, the efficiency of the crystallization reaction process and the automation level of the equipment are improved. The equipment can not only effectively remove crystals and optimize the production process, but also reduce maintenance workload, improve equipment stability and long-term operation capabilities. Through refined control of the crystallization process, the crystallization quality and purification effect of benzophenone are significantly improved, meeting the needs of high-purity benzophenone production, while reducing the labor intensity of workers and promoting the intelligence and automation of the production process.

[0023] like Figure 2 and Figure 4~Figure 7 As shown, the stirring assembly includes a lifting plate 21, the lifting plate 21 is slidably abutted against the inner wall of the first shell 11, the lower side of the lifting plate 21 is fixedly connected to a limiting sleeve 22, the limiting sleeve 22 is slidably connected to a limiting column 23, and the lower end of the limiting column 23 is fixedly connected to an isolation plate 24; A transmission sleeve 25 is fixedly connected to the lower side of the lifting plate 21, a magnetic rotor 26 is rotatably connected inside the transmission sleeve 25, a stirring rod 27 is magnetically connected to the upper side of the magnetic rotor 26, a transmission column 28 is threadedly connected to the transmission sleeve 25, and a driving column 29 is rotatably connected inside the transmission column 28; A second motor 210 is fixedly connected to the lower side of the isolation plate 24, and a driving shaft of the second motor 210 is fixedly connected to the driving column 29; The driving column 29 is slidably engaged with the magnetic rotor 26; A latching assembly is connected between the transmission column 28 and the second motor 210; The stirring assembly is equipped with a locking assembly so that the stirring assembly has two working modes. When in the stirring mode, the driving shaft of the second motor 210 drives the magnetic rotor 26 to rotate, thereby causing the stirring rod 27 in the magnetic state of the magnetic rotor 26 to rotate rapidly. However, the benzophenone solution may crystallize during the mixing process. Excessive stirring may cause the crystals to dissolve in the solution again. Therefore, the upward movement of the transmission sleeve 25 will gradually separate the magnetic rotor 26 from the driving column 29, thereby causing the stirring rod 27 to lose its rotational driving force, thereby causing the vortex of the stirred mixed solution to gradually and slowly stop, and only a preliminary stirring effect is exerted on the mixed solution, that is, through the stirring effect, the solution is quickly The mixing reaction reduces the impact of the vortex on the benzophenone solution, so that the benzophenone solution can better react and crystallize, and then as the transmission sleeve 25 moves upward, the horizontal plane of the benzophenone solution will gradually move upward. After the lifting plate 21 opens the water retaining ring 16, the benzophenone solution is also mixed, and then it is sent to the second shell 12 for heating and static reaction. When the equipment needs to be cleaned internally, the lifting plate 21 will not move, and the stirring rod 27 can continue to stir for a long time, so that the clean water input into the first shell 11 can better clean the inner wall of the first shell 11, reducing the labor intensity of workers and improving the practicability of the equipment.

[0024] like Figure 4~Figure 6 As shown, the positioning assembly includes a positioning plate 31, and a plurality of reset posts 32 are fixedly connected to the lower side of the positioning plate 31, and each reset post 32 is slidably connected to the isolation plate 24, and each reset post 32 is sleeved with a reset spring 33, and the two ends of the reset spring 33 are respectively in contact with the lower side of the isolation plate 24 and the reset post 32; The first clamping cylinder 34 is rotatably connected to the clamping plate 31, and the first clamping cylinder 34 is slidably clamped with the driving shaft of the second motor 210. The second clamping cylinder 35 is fixedly connected to the lower side of the transmission column 28, and the first clamping cylinder 34 and the second clamping cylinder 35 are mutually engaged and clamped. The connection relationship between the first clamping cylinder 34 and the driving shaft of the second motor 210 ensures that the first clamping cylinder 34 can rotate synchronously with the driving shaft of the second motor 210 and can move up and down along the axis direction of the driving shaft of the second motor 210. A locking cylinder 36 is fixedly connected to the isolation plate 24, and a locking block 37 is fixedly connected to the telescopic shaft of the locking cylinder 36. The upper inclined surface of the locking block 37 abuts against the side edge of the locking plate 31; The movement of the telescopic shaft of the locking cylinder 36 drives the locking block 37 to move. When the locking block 37 moves in the direction of the locking plate 31, the locking block 37 will push the locking plate 31 upward, so that the first locking cylinder 34 and the second locking cylinder 35 are locked with each other, so that the second motor 210 can indirectly drive the limiting column 23 to rotate, thereby causing the limiting sleeve 22 threadedly connected to the limiting column 23 to move upward, thereby separating the magnetic suction rotor 26 from the driving column 29. After the magnetic suction rotor 26 has no rotational force, the stirring rod 27 gradually stops stirring the mixed solution. When the locking block 37 moves away from the locking plate 31, the stirring rod 27 stops stirring the mixed solution. When the first shell 11 is moved, the locking plate 31 moves downward under the action of the reset spring 33, and the first locking cylinder 34 and the second locking cylinder 35 are separated from each other. Then the rotation of the drive shaft of the second motor 210 will only drive the drive column 29 to rotate, thereby causing the magnetic rotor 26 to rotate continuously, that is, the stirring rod 27 to rotate continuously. The rotation serves as a cleaning function inside the first shell 11. When the inside of the first shell 11 needs to be cleaned, clean water is injected into the first shell 11. The first shell 11 can be cleaned through the locking assembly, which is convenient for the next use of the equipment, increases the practicability of the equipment, and reduces the labor intensity of workers.

[0025] like Figure 7 As shown, the first scraper 19 and the second scraper 110 are both arranged in a spiral manner; When the first shell 11 and the second shell 12 are rotated relative to each other, the crystals scraped off by the first scraper 19 and the second scraper 110 will move downward along the spiral downward sides of the first scraper 19 and the second scraper 110, thereby improving the scraping effect on the inner wall of the second shell 12 and the outer wall of the first shell 11.

[0026] like Figure 2~Figure 4 As shown, the upper side surface of the lifting plate 21 is an arc-shaped surface that is high in the middle and low around; When the mixed solution on the upper side of the lifting plate 21 moves to the vicinity of the plurality of drainage holes 111 along with the lifting plate 21, the mixed solution can completely flow into the second shell 12 through the drainage holes 111 according to its own weight, that is, the residue of the mixed solution is reduced and the crystallization effect of the mixed solution is improved.

[0027] like Figure 1~Figure 2 As shown, the partition cover 181 with the filter screen is detachably fixedly connected to the lower side of the discharge pipe 18; The partition cover 181 can be used to quickly separate the solid and liquid of the preliminary crystals or the purified crystals that have been crystallized, so that the crystals can be dried in the second shell 12. The dried crystals are in powder form, and their adhesion to the second shell 12 is reduced, so that the first scraper 19 and the second scraper 110 can scrape the dried crystals better, so that the crystals can be collected completely, thereby improving the material output effect.

[0028] Working principle: Through the structural design of the first shell 11 and the second shell 12, a plurality of drainage holes 111 are provided in the first shell 11, and a water retaining ring 16 is provided. The water retaining ring 16 moves downward by gravity, blocking the drainage holes 111, and separating the first shell 11 and the second shell 12 into two independent chambers. This ensures the sealing and independence of the two chambers during the crystallization and heating process, preventing the mixed liquid from leaking or the crystals from affecting the reaction. A heating ring 13 is provided on the outer ring of the second shell 12 for heating and standing reaction, so that benzophenone can crystallize at a suitable temperature; Operation of the stirring assembly: The stirring assembly provides two stirring modes (stirring and cleaning mode and mixing mode) to accurately control the stirring intensity of the solution. The mixing mode is used to quickly mix the solution and reduce the impact on the mixed solution. When crystallization begins, to ensure the quality of the crystallization, the stirring rod 27 is connected to the magnetic rotor 26 and rotated by magnetic attraction. The drive of the stirring rod 27 is directly controlled by the magnetic rotor 26. During the stirring process, the transmission sleeve 25 moves up to separate the magnetic rotor 26 from the driving column 29, thereby driving the stirring rod 27 to gradually stop rotating, which is used to reduce the disturbance of the benzophenone solution and promote better crystallization; With the cooperation of the locking assembly, the stirring mode can be adjusted by controlling the locking cylinder 36 and the return spring 33 during the stirring process. When internal cleaning is required, the stirring rod 27 can continue to rotate, and the inner wall of the first shell 11 can be cleaned with clean water to reduce the residual crystals, improve the practicality of the equipment and reduce the labor intensity of the workers. The equipment uses the structure of the transmission sleeve 25 and the magnetic rotor 26 to enable the inner wall of the first shell 11 to be efficiently cleaned, avoiding the complicated manual cleaning process. Spiral scrapers (first scraper 19 and second scraper 110) are provided on the outer walls of the first shell 11 and the second shell 12. The first shell 11 and the second shell 12 are driven by the first motor 112 to rotate relative to each other, so that the scrapers can effectively scrape off the crystals. The crystals move downward along the spiral surface of the scrapers, thereby improving the removal effect of the crystals and the cleaning efficiency of the equipment. Example

[0029] like Figure 1 to Figure 7As shown, this embodiment, based on Example 1, proposes a preparation process of high-purity benzophenone, comprising the following steps: S100: Raw material preparation: prepare benzene, benzoyl chloride, a suitable catalyst, and a solvent for use; Prepare the raw materials to facilitate subsequent operations; S200: Mixing preparation: clean the inside of the first shell 11 and the second shell 12, dry them, add benzene and benzoyl chloride into the first shell 11, then continue to add the catalyst, mix the solution, and finally transfer the mixed solution to the second shell 12 for heat treatment and crystallization; In the initial stage of stirring, rapid stirring allows the benzophenone solution to be quickly and evenly mixed, and the reactants can fully contact each other, ensuring the efficient progress of the reaction. As the stirring gradually slows down, the cyclonic effect in the solution weakens, which helps the stable formation of crystals in the benzophenone solution. Through this controlled stirring mode, excessive stirring that causes dissolution of crystallized substances is avoided, and the quality and yield of crystals are optimized; S300: scraping operation: start the first motor 112 to drive the first shell 11 and the second shell 12 to rotate relative to each other, so that the crystals and the remaining mixed liquid in the second shell 12 are collected by the first scraper 19 and the second scraper 110, and finally discharged through the discharge pipe 18, and the solid-liquid separation is performed, and then the relative positions of the first shell 11 and the second shell 12 are reset; Through the scraping operation, the relative rotation of the first shell 11 and the second shell 12 combined with the spiral scraping action of the first scraper 19 and the second scraper 110 can more effectively scrape the solidified crystals from the inner wall, effectively preventing the accumulation of crystals on the inner wall of the shell. This design ensures that the crystals can be scraped off in time, avoiding interference of crystalline materials with the operation of the equipment.

[0030] S400: Purification: The initially obtained crystals and a mixed solvent of dichloromethane and ethanol are added to the first housing 11 for mixing, and then the mixed solution is transferred to the second housing 12. After the temperature is set, a secondary crystallization operation is performed, and then a secondary scraping operation is performed: a more purified benzophenone is collected and dried; Through purification, the crystals processed initially are crystallized for a second time, which can further purify and remove impurities in the crystals and improve the purity of the raw materials, which helps to improve the selectivity and conversion rate of subsequent reactions. When high-purity benzophenone is used as a reactant, it can play a better role in the subsequent synthesis process and avoid the interference of impurities on the reaction; S500: Purity test: Use high performance liquid chromatography (HPLC) or gas chromatography (GC) to test the purity of benzophenone to ensure that it meets product requirements; By testing the crystals precipitated twice or multiple times, the purity of the crystals can be checked and the crystals of different purities can be classified so that they can be better applied. S600: Finished Product Packaging and Storage: Package the purified benzophenone in airtight containers and store them in a dry, cool place.

[0031] like Figure 1 to Figure 7 As shown, step S200 mixing preparation includes the following steps: S210: Benzene and benzoyl chloride are quantitatively fed into the first housing 11 through the delivery pipes 113 according to the molar ratio, and then a catalyst of 10%-20% of the amount of benzoyl chloride used is dripped into the first housing 11, and then a stirring component is started to quickly mix the mixed solution; S220: The mixed solution being mixed is transferred to the second shell 12 through the drainage hole 111, and then the stirring assembly is reset to make the first shell 11 and the second shell 12 become separate chambers, and the heating ring 13 is started to heat the mixed solution so that the mixed solution is allowed to stand and crystallize in the sealed chamber.

[0032] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A high-purity benzophenone preparation device, comprising a first housing (11), characterized in that ； The first shell (11) is rotatably connected to the outside of a second shell (12) for crystallization, the outer ring of the second shell (12) is fixedly connected to a heating ring (13), the upper side of the first shell (11) is connected to a cover (14), the upper side of the cover (14) is fixedly connected to a pressure gauge (15), and one side of the pressure gauge (15) is fixedly connected to a plurality of conveying pipes (113); A plurality of drainage holes (111) are provided in an annular array in the first shell (11), and a water retaining ring (16) is slidably connected to the inner wall of the first shell (11), wherein the water retaining ring (16) is used to block the plurality of drainage holes (111); A stirring component for quickly mixing the solution in the first shell (11) is connected to the first shell (11); A blocking block (17) is fixedly connected to the outside of the first shell (11), and a discharge pipe (18) is fixedly connected to the bottom of the second shell (12), wherein the blocking block (17) is used to block the outlet of the discharge pipe (18); The outer wall of the first shell (11) and the inner wall of the second shell (12) are respectively fixedly connected with a first scraper (19) and a second scraper (110), and the first scraper (19) and the second scraper (110) are both in tight contact with the inner wall of the second shell (12) and the outer wall of the first shell (11); A first motor (112) is fixedly connected to the lower side of the second housing (12), and a drive shaft of the first motor (112) is fixedly connected to the bottom of the first housing (11).

2. The preparation equipment of high-purity benzophenone according to claim 1, characterized in that: The stirring assembly comprises a lifting plate (21), the lifting plate (21) is in sliding contact with the inner wall of the first shell (11), a limiting sleeve (22) is fixedly connected to the lower side of the lifting plate (21), a limiting column (23) is slidably connected inside the limiting sleeve (22), and an isolation plate (24) is fixedly connected to the lower end of the limiting column (23); A transmission sleeve (25) is fixedly connected to the lower side of the lifting plate (21), a magnetic rotor (26) is rotatably connected inside the transmission sleeve (25), a stirring rod (27) is magnetically connected to the upper side of the magnetic rotor (26), a transmission column (28) is internally threadedly connected to the transmission sleeve (25), and a driving column (29) is rotatably connected inside the transmission column (28); A second motor (210) is fixedly connected to the lower side of the isolation plate (24), and a drive shaft of the second motor (210) is fixedly connected to a drive column (29); The driving column (29) is slidably engaged with the magnetic rotor (26); A locking assembly is connected between the transmission column (28) and the second motor (210).

3. The preparation equipment of high-purity benzophenone according to claim 2, characterized in that, The positioning assembly comprises a positioning plate (31), a plurality of reset columns (32) being fixedly connected to the lower side of the positioning plate (31), each of the reset columns (32) being slidably connected to the isolation plate (24), each of the reset columns (32) being sleeved with a reset spring (33), and two ends of the reset spring (33) respectively abutting against the lower side of the isolation plate (24) and the reset column (32); A first locking cylinder (34) is rotatably connected to the locking plate (31), the first locking cylinder (34) is locked with the drive shaft of the second motor (210), a second locking cylinder (35) is fixedly connected to the lower side of the transmission column (28), and the first locking cylinder (34) and the second locking cylinder (35) are engaged with each other; A locking cylinder (36) is fixedly connected to the isolation plate (24), a telescopic shaft of the locking cylinder (36) is fixedly connected to a locking block (37), and an upper inclined surface of the locking block (37) abuts against a side edge of the locking plate (31).

4. The preparation equipment of high-purity benzophenone according to claim 1, characterized in that: The first scraper (19) and the second scraper (110) are both arranged in a spiral arrangement.

5. The preparation equipment of high-purity benzophenone according to claim 2, characterized in that: The upper side surface of the lifting plate (21) is an arc-shaped surface that is high in the middle and low around.

6. The preparation equipment of high-purity benzophenone according to claim 1, characterized in that: A partition cover plate (181) with a filter screen is detachably fixedly connected to the lower side of the discharge pipe (18).

7. A process for preparing high-purity benzophenone, characterized in that: A preparation device comprising the high-purity benzophenone according to claims 1 to 6, characterized in that it comprises the following steps: S100: Raw material preparation: prepare benzene, benzoyl chloride, a suitable catalyst, and a solvent for use; S200: Mixing preparation: clean the inside of the first shell (11) and the second shell (12), dry them, add benzene and benzoyl chloride into the first shell (11), add the catalyst, mix the solution, and finally transfer the mixed solution to the second shell (12) for heat treatment and crystallization; S300: scraping operation: starting the first motor (112) to drive the first shell (11) and the second shell (12) to rotate relative to each other, so that the crystals and the remaining mixed liquid in the second shell (12) are collected by the first scraper (19) and the second scraper (110), and finally discharged through the discharge pipe (18), and the solid-liquid separation is performed, and then the relative position of the first shell (11) and the second shell (12) is reset; S400: Purification: the initially obtained crystals and a mixed solvent of dichloromethane and ethanol are added to the first shell (11) for mixing, and then the mixed solution is transferred to the second shell (12). After setting the temperature, a secondary crystallization operation is performed, and then a secondary scraping operation is performed: a more purified benzophenone is collected and dried; S500: Purity test: Use high performance liquid chromatography or gas chromatography to test the purity of benzophenone to ensure that it meets product requirements; S600: Finished Product Packaging and Storage: Package the purified benzophenone in airtight containers and store them in a dry, cool place.

8. The process for preparing high-purity benzophenone according to claim 7, characterized in that: The step S200 mixing preparation includes the following steps: S210: quantitatively inputting benzene and benzoyl chloride into the first shell (11) through the respective delivery pipes (113) according to the molar ratio, then dripping a catalyst of 10% to 20% of the amount of benzoyl chloride used, and then starting a stirring component to rapidly mix the mixed solution; S220: The mixed solution being mixed is transferred to the second shell (12) through the drainage hole (111), and then the stirring assembly is reset, so that the first shell (11) and the second shell (12) become separate chambers, and the heating ring (13) is started to heat the mixed solution, so that the mixed solution is placed in the sealed chamber for crystallization.

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