A production process and distillation apparatus for benzophenone-based ultraviolet absorbers

Abstract

This invention discloses a production process and distillation apparatus for benzoyl ketone-based ultraviolet absorbers, comprising a distillation shell, a rotary distillation assembly, a benzoyl chloride distillation assembly, a benzene distillation assembly, a petroleum ether distillation assembly, and a base plate. The rotary distillation assembly is disposed on top of the distillation shell and includes a disc, a rotary motor, an L-shaped fixing plate, a first guide plate, a distillation plate, an automatic turntable, and a distillation tray. The disc is rotatably mounted on top of the distillation shell, the L-shaped fixing plate is fixedly mounted on top of the base plate, and the rotary motor is fixedly mounted on the bottom of the L-shaped fixing plate. The disc is fixedly connected to the output end of the rotary motor. This invention, through its rotary distillation assembly, enables rapid distillation of benzoyl chloride, benzene, and petroleum ether according to their different boiling points, thereby increasing the distillation efficiency of the distillation apparatus for benzoyl chloride, benzene, and petroleum ether, and thus allowing for the recycling of benzoyl chloride, benzene, and petroleum ether.

Description

Technical Field

[0001] This invention relates to the field of benzophenone-based ultraviolet absorbers, specifically to a production process and distillation apparatus for benzophenone-based ultraviolet absorbers. Background Technology

[0002] Benzophenone compounds are widely used additives that strongly absorb ultraviolet light and are extensively used in daily chemical products, pharmaceuticals, pesticides, plastics, and coatings. Due to the increasing damage to the Earth's ozone layer and the intensifying solar ultraviolet radiation, ultraviolet absorbers are essential additives in various polymer materials and skin protection products. In recent years, the demand for high-quality ultraviolet absorbers has been continuously increasing abroad, especially in Southeast Asian countries. Foreign countries have successively developed sulfonate esters, amino-based benzophenone-based bis(azo)oxanes as UV absorbers, and benzophenone-based benzophenones as UV stabilizers. In comparison, there are fewer reports on this type of compound in China, indicating a significant market potential for the research and development of benzophenone-based ultraviolet absorbers.

[0003] For example, the patent application with application number CN201310603285.3 includes the following steps: adding liquid benzene to a condensation reactor, adding benzoyl chloride to a dropwise storage tank, heating the liquid benzene to 65-70°C under stirring and maintaining the temperature, adding ferric chloride to the reactor, and simultaneously adding benzoyl chloride dropwise to the reactor, using a vacuum device to remove the HCl gas generated during the reaction during the dropwise addition; after the dropwise addition is completed, heating to 80°C, distilling to recover excess benzene, opening the jacket water to allow the material in the reactor to cool to room temperature, centrifuging and filtering to obtain the product; this invention solves the problem that the current production process of benzophenone is cumbersome and cannot achieve large-scale industrial production. By using ferric chloride as a reaction catalyst, the yield of benzophenone is greatly improved, the waste of raw materials is reduced, and the production cost is greatly reduced, resulting in significant social and economic benefits.

[0004] The aforementioned and existing production methods use ferric chloride as a catalyst. Ferric chloride is an inorganic acid, which means the catalyst cannot be recovered and reused, remaining in the reaction products. Post-processing requires neutralization and washing, resulting in a long process route, significant product loss, and the generation of large amounts of waste liquid, causing environmental pollution and posing safety hazards. Therefore, there is an urgent need to design a production process and distillation apparatus for benzophenone-based ultraviolet absorbers to solve these problems. Summary of the Invention

[0005] The purpose of this invention is to provide a production process and distillation apparatus for benzophenone-based ultraviolet absorbers to overcome the aforementioned shortcomings in the prior art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] The device includes a distillation shell, a rotary distillation assembly, a benzoyl chloride distillation assembly, a benzene distillation assembly, a petroleum ether distillation assembly, and a base plate. The rotary distillation assembly is located on top of the distillation shell and includes a disc, a rotary motor, an L-shaped fixing plate, a first guide plate, a distillation plate, an automatic turntable, and a distillation tray. The disc is rotatably mounted on top of the distillation shell, the L-shaped fixing plate is fixedly mounted on top of the base plate, and the rotary motor is fixedly mounted on the bottom of the L-shaped fixing plate. The disc is fixedly connected to the output end of the rotary motor.

[0008] The rotary distillation unit can rapidly distill benzoyl chloride, benzene, and petroleum ether according to their different boiling points, thereby increasing the distillation efficiency of the distillation unit for benzoyl chloride, benzene, and petroleum ether, and thus enabling the recycling of benzoyl chloride, benzene, and petroleum ether.

[0009] The L-shaped fixing plate can support and fix the rotary motor, thereby increasing the stability of the distillation device during use.

[0010] The automatic turntable can drive the distillation tray to rotate, thereby ensuring that benzoyl chloride, benzene and petroleum ether in the distillation tray are heated evenly, thus increasing the distillation efficiency of the distillation device for benzoyl chloride, benzene and petroleum ether.

[0011] A slot is provided between the disc and the distillation shell, the first guide plate is fixedly installed on the top of the inner wall of the distillation shell, and the distillation plate is fixedly installed inside the distillation shell.

[0012] The automatic turntable is fixedly installed at the bottom of the inner wall of the distillation shell, and the distillation tray is locked at the top of the automatic turntable.

[0013] A door panel is rotatably mounted on the front side of the distillation shell. A groove is opened on the front side of the door panel, and a glass plate is fixedly installed in the groove. A controller is fixedly installed on the front side of the door panel, a thermometer is fixedly installed on the front side of the door panel, a handle is fixedly installed on the front side of the door panel, and a buckle is fixedly installed on the front side of the door panel.

[0014] The benzoyl chloride distillation assembly includes a first ring plate, a benzoyl chloride condenser plate, a benzoyl chloride condenser, a first funnel, a one-way valve, a first support plate, and a benzoyl chloride collection cup. The first ring plate is fixedly installed on the top of the disc, and the benzoyl chloride condenser plate is fixedly installed on one side of the first ring plate. A benzoyl chloride trough is formed between the benzoyl chloride condenser plate and the first ring plate.

[0015] The benzoyl chloride condenser is fixedly installed inside the benzoyl chloride condensing plate, the first funnel is fixedly installed at the bottom of the benzoyl chloride condensing plate, the one-way gas valve is fixedly installed inside the benzoyl chloride tank, the first support plate is fixedly installed on the outer surface of the disc, and the benzoyl chloride collection cup is clamped on the top of the first support plate.

[0016] The benzene distillation assembly includes a second ring plate, a benzene condenser plate, a benzene condenser, a second funnel, a second guide plate, a second support plate, and a benzene collection cup. The second ring plate is fixedly installed on the top of the disc, and the benzene condenser plate is fixedly installed on one side of the second ring plate. A benzene groove is formed between the benzene condenser plate and the second ring plate.

[0017] The benzene condenser is fixedly installed inside the benzene condensing plate, the second funnel is fixedly installed at the bottom of the benzene condensing plate, the second guide plate is fixedly installed inside the benzene tank, the second support plate is fixedly installed on the outer surface of the disc, and the benzene collecting cup is secured to the top of the second support plate.

[0018] The petroleum ether distillation assembly includes a third ring plate, a petroleum ether condenser plate, a petroleum ether condenser, a third funnel, a guide plate, a third support plate, and a petroleum ether collection cup. The third ring plate is fixedly installed on the top of the disc, the petroleum ether condenser plate is fixedly installed on one side of the third ring plate, a petroleum ether groove is formed between the petroleum ether condenser plate and the third ring plate, the petroleum ether condenser is fixedly installed inside the petroleum ether condenser plate, the third funnel is fixedly installed at the bottom of the petroleum ether condenser plate, the guide plate is fixedly installed at the bottom of the third funnel, the third support plate is fixedly installed on the outer surface of the disc, and the petroleum ether collection cup is secured on the top of the third support plate.

[0019] A distillation apparatus for a benzophenone-based ultraviolet absorber includes the following steps:

[0020] S1: Concentrated hydrochloric acid (37.0%) was slowly added dropwise to an equimolar amount of triethylamine under constant stirring. The reaction was vigorous and released a large amount of heat. After the reaction was complete, the mixture was subjected to rotary evaporation under reduced pressure at 60°C for 8 hours to remove water from the reaction mixture. The resulting white solid was triethylamine hydrochloride. Place it in a desiccator for later use;

[0021] S2: Before each catalytic synthesis of benzophenone experiment, a certain amount of... and waterless The ionic liquid is obtained by grinding the mixture thoroughly in a mortar.

[0022] S3: Synthesis of benzophenone: A certain amount of benzoyl chloride (0.043 mol), benzene, and... were added to a 50 mL three-necked flask. Using an ionic liquid catalyst, the mixture was magnetically stirred and refluxed for a certain period while maintaining the reaction temperature at 80°C. After the reaction was complete, it was cooled to room temperature. Then, the reaction solution and 5-6 times its volume of petroleum ether (30-60°C) were added to a separatory funnel. Since the dielectric constant of petroleum ether is much smaller than that of petroleum ether... As an ionic liquid catalyst, the catalyst can be separated from the reaction system relatively well. Most of the catalyst is separated into the lower layer of the separatory funnel, while unreacted benzoyl chloride, benzene, the product benzophenone and petroleum ether are in the upper layer. Then, the upper layer mixture is taken out for qualitative (GC-MS) and quantitative (GC) analysis.

[0023] S4: Place the upper mixture in the distillation tray and place the distillation tray on the automatic turntable. Close the door and start the distillation plate to distill the upper mixture using the controller and thermometer. Start the automatic turntable to rotate the upper mixture via the distillation tray. When the temperature reaches 30°C... ~60 At that time, the petroleum ether in the upper mixture evaporates, and the petroleum ether vapor enters the petroleum ether condenser through the first guide plate, the third ring plate and the petroleum ether condensing plate for condensation. The petroleum ether condensate flows into the petroleum ether collection cup through the third funnel and the guide plate.

[0024] S5: After the petroleum ether has condensed, start the rotary motor to drive the disc to rotate. The disc drives the benzoyl chloride distillation assembly, benzene distillation assembly, and petroleum ether distillation assembly to rotate, connecting the slot to the second ring plate. The controller heats the distillation plate until the temperature reaches 80.1℃. ~196 At this time, the benzene in the upper mixture evaporates, and the benzene vapor flows along the first guide plate through the second ring plate and the benzene condenser plate, and is guided by the second guide plate into the benzene condenser for condensation. The benzene condensate flows into the benzene collection cup through the second funnel. Referring to the above steps, the rotary motor is started to drive the disc to rotate, so that the first ring plate is connected to the groove opening. The controller heats the distillation plate. When the temperature reaches 197°C... ~304 At that time, the benzoyl chloride in the upper mixture evaporates. The benzoyl chloride vapor flows along the first guide plate, through the first ring plate and the benzoyl chloride condenser plate, and enters the benzoyl chloride condenser through the one-way valve for condensation. The benzoyl chloride condensate flows along the first funnel into the benzoyl chloride collection cup. After the benzoyl chloride distillation is completed, the upper mixture in the distillation pan is left with benzophenone.

[0025] In the above technical solution, the production process and distillation apparatus for benzophenone-based ultraviolet absorbers provided by the present invention have the following advantages:

[0026] 1. The rotary distillation unit can rapidly distill benzoyl chloride, benzene, and petroleum ether according to their different boiling points, thereby increasing the distillation efficiency of the distillation unit for benzoyl chloride, benzene, and petroleum ether, and thus enabling the recycling of benzoyl chloride, benzene, and petroleum ether.

[0027] 2. The L-shaped fixing plate can support and fix the rotary motor, thereby increasing the stability of the distillation device during use.

[0028] 3. The automatic turntable can drive the distillation tray to rotate, thereby ensuring that the benzoyl chloride, benzene and petroleum ether in the distillation tray are heated evenly, thus increasing the distillation effect of the distillation device on benzoyl chloride, benzene and petroleum ether. Attached Figure Description

[0029] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.

[0030] Figure 1 This is a schematic diagram of the distillation apparatus provided in an embodiment of the production process and distillation apparatus for a benzophenone-based ultraviolet absorber according to the present invention.

[0031] Figure 2 This is a schematic diagram of the rotary distillation assembly structure provided in an embodiment of the production process and distillation apparatus for a benzophenone-based ultraviolet absorber according to the present invention.

[0032] Figure 3 This is a schematic diagram of the benzoyl chloride distillation assembly structure provided in an embodiment of the production process and distillation apparatus for a benzophenone-based ultraviolet absorber according to the present invention.

[0033] Figure 4 This is a schematic diagram of the benzene distillation component structure provided in an embodiment of the production process and distillation apparatus for a benzophenone-based ultraviolet absorber according to the present invention.

[0034] Figure 5 This is a schematic diagram of the petroleum ether distillation assembly structure provided in an embodiment of the production process and distillation apparatus for a benzophenone-based ultraviolet absorber according to the present invention.

[0035] Explanation of reference numerals in the attached figures:

[0036] 1. Distillation shell; 2. Rotary distillation assembly; 3. Benzoyl chloride distillation assembly; 4. Benzene distillation assembly; 5. Petroleum ether distillation assembly; 6. Base plate; 7. Disc; 8. Rotary motor; 9. L-shaped fixing plate; 10. First guide plate; 11. Distillation plate; 12. Automatic turntable; 13. Distillation tray; 14. Groove; 15. Door panel; 16. Recess; 17. Glass plate; 18. Controller; 19. Thermometer; 20. Handle; 21. Buckle; 22. First ring plate; 23. Benzoyl chloride condenser plate; 24. Benzoyl chloride condenser plate. 25. First funnel; 26. One-way valve; 27. First support plate; 28. Benzoyl chloride collection cup; 29. ​​Benzoyl chloride tank; 30. Second ring plate; 31. Benzene condenser plate; 32. Benzene condenser; 33. Second funnel; 34. Second guide plate; 35. Second support plate; 36. Benzene collection cup; 37. Benzene tank; 38. Third ring plate; 39. Petroleum ether condenser plate; 40. Petroleum ether condenser; 41. Third funnel; 42. Drain plate; 43. Third support plate; 44. Petroleum ether collection cup; 45. Petroleum ether tank. Detailed Implementation

[0037] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0038] like Figure 1-5 As shown in the figure, an embodiment of the present invention provides a production process and distillation apparatus for a benzophenone-based ultraviolet absorber.

[0039] The assembly includes a distillation shell 1, a rotary distillation component 2, a benzoyl chloride distillation component 3, a benzene distillation component 4, a petroleum ether distillation component 5, and a base plate 6. The rotary distillation component 2 is located on top of the distillation shell 1. The rotary distillation component 2 includes a disc 7, a rotary motor 8, an L-shaped fixing plate 9, a first guide plate 10, a distillation plate 11, an automatic turntable 12, and a distillation tray 13. The disc 7 is rotatably mounted on top of the distillation shell 1, the L-shaped fixing plate 9 is fixedly mounted on top of the base plate 6, and the rotary motor 8 is fixedly mounted on the bottom of the L-shaped fixing plate 9. The disc 7 is fixedly connected to the output end of the rotary motor 8.

[0040] The rotary distillation unit 2 can rapidly distill benzoyl chloride, benzene, and petroleum ether according to their different boiling points, thereby increasing the distillation efficiency of the distillation unit for benzoyl chloride, benzene, and petroleum ether, and thus enabling the recycling of benzoyl chloride, benzene, and petroleum ether.

[0041] The L-shaped fixing plate 9 can support and fix the rotary motor 8, thereby increasing the stability of the distillation device during use.

[0042] The automatic turntable 12 can drive the distillation plate 13 to rotate, thereby making the benzoyl chloride, benzene and petroleum ether in the distillation plate 13 heat evenly, thus increasing the distillation effect of the distillation device on benzoyl chloride, benzene and petroleum ether.

[0043] Reference Figure 2 In this embodiment, a slot 14 is provided between the disc 7 and the distillation shell 1, the first guide plate 10 is fixedly installed on the top of the inner wall of the distillation shell 1, and the distillation plate 11 is fixedly installed inside the distillation shell 1.

[0044] The automatic turntable 12 is fixedly installed at the bottom of the inner wall of the distillation shell 1, and the distillation tray 13 is locked on the top of the automatic turntable 12.

[0045] Reference Figure 1 In this embodiment, a door panel 15 is rotatably mounted on the front side of the distillation shell 1. A groove 16 is provided on the front side of the door panel 15. A glass plate 17 is fixedly mounted in the groove 16. A controller 18 is fixedly mounted on the front side of the door panel 15. A thermometer 19 is fixedly mounted on the front side of the door panel 15. A handle 20 is fixedly mounted on the front side of the door panel 15. A buckle 21 is fixedly mounted on the front side of the door panel 15.

[0046] Reference Figure 3 The benzoyl chloride distillation assembly 3 in this embodiment includes a first ring plate 22, a benzoyl chloride condenser plate 23, a benzoyl chloride condenser 24, a first funnel 25, a one-way valve 26, a first support plate 27, and a benzoyl chloride collection cup 28. The first ring plate 22 is fixedly installed on the top of the disc 7, and the benzoyl chloride condenser plate 23 is fixedly installed on one side of the first ring plate 22. A benzoyl chloride trough 29 is provided between the benzoyl chloride condenser plate 23 and the first ring plate 22.

[0047] The benzoyl chloride condenser 24 is fixedly installed inside the benzoyl chloride condensing plate 23, the first funnel 25 is fixedly installed at the bottom of the benzoyl chloride condensing plate 23, the one-way valve 26 is fixedly installed inside the benzoyl chloride tank 29, the first support plate 27 is fixedly installed on the outer surface of the disc 7, and the benzoyl chloride collection cup 28 is clamped on the top of the first support plate 27.

[0048] Reference Figure 4 The benzene distillation assembly 4 in this embodiment includes a second ring plate 30, a benzene condenser plate 31, a benzene condenser 32, a second funnel 33, a second guide plate 34, a second support plate 35, and a benzene collection cup 36. The second ring plate 30 is fixedly installed on the top of the disc 7, and the benzene condenser plate 31 is fixedly installed on one side of the second ring plate 30. A benzene groove 37 is provided between the benzene condenser plate 31 and the second ring plate 30.

[0049] The benzene condenser 32 is fixedly installed inside the benzene condensing plate 31, the second funnel 33 is fixedly installed at the bottom of the benzene condensing plate 31, the second guide plate 34 is fixedly installed inside the benzene tank 37, the second support plate 35 is fixedly installed on the outer surface of the disc 7, and the benzene collection cup 36 is clamped at the top of the second support plate 35.

[0050] Reference Figure 5 The petroleum ether distillation assembly 5 of this embodiment includes a third ring plate 38, a petroleum ether condenser plate 39, a petroleum ether condenser 40, a third funnel 41, a guide plate 42, a third support plate 43, and a petroleum ether collection cup 44. The third ring plate 38 is fixedly installed on the top of the disc 7, the petroleum ether condenser plate 39 is fixedly installed on one side of the third ring plate 38, a petroleum ether trough 45 is provided between the petroleum ether condenser plate 39 and the third ring plate 38, the petroleum ether condenser 40 is fixedly installed inside the petroleum ether condenser plate 39, the third funnel 41 is fixedly installed at the bottom of the petroleum ether condenser plate 39, the guide plate 42 is fixedly installed at the bottom of the third funnel 41, the third support plate 43 is fixedly installed on the outer surface of the disc 7, and the petroleum ether collection cup 44 is secured to the top of the third support plate 43.

[0051] A distillation apparatus for a benzophenone-based ultraviolet absorber includes the following steps:

[0052] S1: Concentrated hydrochloric acid (37.0%) was slowly added dropwise to an equimolar amount of triethylamine under constant stirring. The reaction was vigorous and released a large amount of heat. After the reaction was complete, the mixture was subjected to rotary evaporation under reduced pressure at 60°C for 8 hours to remove water from the reaction mixture. The resulting white solid was triethylamine hydrochloride. Place it in a desiccator for later use;

[0053] S2: Before each catalytic synthesis of benzophenone experiment, a certain amount of... and waterless The ionic liquid is obtained by grinding the mixture thoroughly in a mortar.

[0054] S3: Synthesis of benzophenone: A certain amount of benzoyl chloride (0.043 mol), benzene, and... were added to a 50 mL three-necked flask. Using an ionic liquid catalyst, the mixture was magnetically stirred and refluxed for a certain period while maintaining the reaction temperature at 80°C. After the reaction was complete, it was cooled to room temperature. Then, the reaction solution and 5-6 times its volume of petroleum ether (30-60°C) were added to a separatory funnel. Since the dielectric constant of petroleum ether is much smaller than that of petroleum ether... As an ionic liquid catalyst, the catalyst can be separated from the reaction system relatively well. Most of the catalyst is separated into the lower layer of the separatory funnel, while unreacted benzoyl chloride, benzene, the product benzophenone and petroleum ether are in the upper layer. Then, the upper layer mixture is taken out for qualitative (GC-MS) and quantitative (GC) analysis.

[0055] S4: Place the upper mixture in the distillation tray 13 and place the distillation tray 13 on the automatic turntable 12. Close the door panel 15 and start the distillation plate 11 to distill the upper mixture using the controller 18 and thermometer 19. Start the automatic turntable 12 to rotate the upper mixture via the distillation tray 13. When the temperature reaches 30°C... ~60 At that time, the petroleum ether in the upper mixture evaporates, and the petroleum ether vapor enters the petroleum ether condenser 40 through the third ring plate 38 and the petroleum ether condensing plate 39 along the first guide plate 10 for condensation. The petroleum ether condensate flows into the petroleum ether collection cup 44 along the third funnel 41 and the guide plate 42.

[0056] S5: After the petroleum ether has condensed, start the rotary motor 8 to drive the disc 7 to rotate. The disc 7 drives the benzoyl chloride distillation assembly 3, the benzene distillation assembly 4, and the petroleum ether distillation assembly 5 to rotate, so that the slot 14 is connected to the second ring plate 30. The controller 18 heats the distillation plate 11 until the temperature reaches 80.1℃. ~196 At this time, the benzene in the upper mixture evaporates, and the benzene vapor is guided by the second guide plate 34 through the second ring plate 30 and the benzene condensing plate 31 to the benzene condenser 32 for condensation. The benzene condensate flows into the benzene collection cup 36 through the second funnel 33. Referring to the above steps, the rotary motor 8 is started to drive the disc 7 to rotate, so that the first ring plate 22 is connected to the slot 14. The controller 18 heats the distillation plate 11. When the temperature reaches 197°C... ~304 At that time, the benzoyl chloride in the upper mixture evaporates, and the benzoyl chloride vapor flows along the first guide plate 10, through the first ring plate 22 and the benzoyl chloride condenser plate 23, and enters the benzoyl chloride condenser 24 through the one-way gas valve 26 for condensation. The benzoyl chloride condensate flows along the first funnel 25 into the benzoyl chloride collection cup 28. After the benzoyl chloride distillation is completed, the upper mixture in the distillation pan 13 is left with benzophenone.

[0057] Working principle: Concentrated hydrochloric acid (37.0%) was slowly added dropwise to an equimolar amount of triethylamine under constant stirring. The reaction was vigorous and released a large amount of heat. After the reaction was complete, the mixture was subjected to rotary evaporation under reduced pressure at 60°C for 8 hours to remove water from the reaction mixture. The resulting white solid was triethylamine hydrochloride. Place it in a desiccator for later use; Before each catalytic synthesis of benzophenone experiment, a certain amount of... and waterless The ionic liquid is obtained by thoroughly grinding the ingredients in a mortar; Synthesis of benzophenone: A certain amount of benzoyl chloride (0.043 mol), benzene, and... are added to a 50 mL three-necked flask. Using an ionic liquid catalyst, the mixture was magnetically stirred and refluxed for a certain period while maintaining the reaction temperature at 80°C. After the reaction was complete, it was cooled to room temperature. Then, the reaction solution and 5-6 times its volume of petroleum ether (30-60°C) were added to a separatory funnel. Since the dielectric constant of petroleum ether is much smaller than that of petroleum ether... The ionic liquid catalyst allows for relatively good separation from the reaction system. Most of the catalyst is separated into the lower layer of the separatory funnel, while unreacted benzoyl chloride, benzene, the product benzophenone, and petroleum ether remain in the upper layer. The upper layer mixture is then removed for qualitative (GC-MS) and quantitative (GC) analysis. The upper layer mixture is placed in distillation tray 13, which is then placed on an automatic turntable 12. The door 15 is closed, and the distillation plate 11 is activated via controller 18 and thermometer 19 to distill the upper layer mixture. The automatic turntable 12 rotates the upper layer mixture via distillation tray 13. When the temperature reaches 30°C... ~60 During this process, the petroleum ether in the upper mixture evaporates. The petroleum ether vapor flows along the first guide plate 10, through the third ring plate 38 and the petroleum ether condensing plate 39, into the petroleum ether condenser 40 for condensation. The petroleum ether condensate flows along the third funnel 41 and the guide plate 42 into the petroleum ether collection cup 44. After the petroleum ether has condensed, the rotary motor 8 is started to drive the disc 7 to rotate. The disc 7 drives the benzoyl chloride distillation assembly 3, the benzene distillation assembly 4, and the petroleum ether distillation assembly 5 to rotate, so that the slot 14 is connected to the second ring plate 30. The controller 18 heats the distillation plate 11 until the temperature reaches 80.1°C. ~196 At this time, the benzene in the upper mixture evaporates, and the benzene vapor is guided by the second guide plate 34 through the second ring plate 30 and the benzene condensing plate 31 to the benzene condenser 32 for condensation. The benzene condensate flows into the benzene collection cup 36 through the second funnel 33. Referring to the above steps, the rotary motor 8 is started to drive the disc 7 to rotate, so that the first ring plate 22 is connected to the slot 14. The controller 18 heats the distillation plate 11. When the temperature reaches 197°C... ~304 At that time, the benzoyl chloride in the upper mixture evaporates, and the benzoyl chloride vapor flows along the first guide plate 10, through the first ring plate 22 and the benzoyl chloride condenser plate 23, and enters the benzoyl chloride condenser 24 through the one-way gas valve 26 for condensation. The benzoyl chloride condensate flows along the first funnel 25 into the benzoyl chloride collection cup 28. After the benzoyl chloride distillation is completed, the upper mixture in the distillation pan 13 is left with benzophenone.

[0058] The foregoing has only described certain exemplary embodiments of the present invention by way of illustration. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the foregoing drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A distillation apparatus for a benzophenone-based ultraviolet absorber, comprising a distillation shell (1), a rotary distillation assembly (2), a benzoyl chloride distillation assembly (3), a benzene distillation assembly (4), a petroleum ether distillation assembly (5), and a base plate (6), characterized in that, The rotary distillation assembly (2) is disposed on the top of the distillation shell (1). The rotary distillation assembly (2) includes a disc (7), a rotary motor (8), an L-shaped fixing plate (9), a first guide plate (10), a distillation plate (11), an automatic turntable (12), and a distillation tray (13). The disc (7) is rotatably mounted on the top of the distillation shell (1). The L-shaped fixing plate (9) is fixedly mounted on the top of the base plate (6). The rotary motor (8) is fixedly mounted on the bottom of the L-shaped fixing plate (9). The disc (7) is fixedly connected to the output end of the rotary motor (8). A slot (14) is provided between the disc (7) and the distillation shell (1). The first guide plate (10) is fixedly mounted on the top of the inner wall of the distillation shell (1). The distillation plate (11) is fixedly mounted inside the distillation shell (1).

2. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 1, characterized in that, The automatic turntable (12) is fixedly installed at the bottom of the inner wall of the distillation shell (1), and the distillation plate (13) is clamped at the top of the automatic turntable (12).

3. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 2, characterized in that, A door panel (15) is rotatably mounted on the front side of the distillation shell (1). A groove (16) is provided on the front side of the door panel (15). A glass plate (17) is fixedly installed in the groove (16). A controller (18) is fixedly installed on the front side of the door panel (15). A thermometer (19) is fixedly installed on the front side of the door panel (15). A handle (20) is fixedly installed on the front side of the door panel (15). A buckle (21) is fixedly installed on the front side of the door panel (15).

4. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 3, characterized in that, The benzoyl chloride distillation assembly (3) includes a first ring plate (22), a benzoyl chloride condenser plate (23), a benzoyl chloride condenser (24), a first funnel (25), a one-way valve (26), a first support plate (27), and a benzoyl chloride collection cup (28). The first ring plate (22) is fixedly installed on the top of the disc (7), and the benzoyl chloride condenser plate (23) is fixedly installed on one side of the first ring plate (22). A benzoyl chloride trough (29) is provided between the benzoyl chloride condenser plate (23) and the first ring plate (22).

5. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 4, characterized in that, The benzoyl chloride condenser (24) is fixedly installed inside the benzoyl chloride condensing plate (23), the first funnel (25) is fixedly installed at the bottom of the benzoyl chloride condensing plate (23), the one-way gas valve (26) is fixedly installed inside the benzoyl chloride tank (29), the first support plate (27) is fixedly installed on the outer surface of the disc (7), and the benzoyl chloride collection cup (28) is clamped on the top of the first support plate (27).

6. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 5, characterized in that, The benzene distillation assembly (4) includes a second ring plate (30), a benzene condenser plate (31), a benzene condenser (32), a second funnel (33), a second guide plate (34), a second support plate (35), and a benzene collection cup (36). The second ring plate (30) is fixedly installed on the top of the disc (7), and the benzene condenser plate (31) is fixedly installed on one side of the second ring plate (30). A benzene groove (37) is provided between the benzene condenser plate (31) and the second ring plate (30).

7. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 6, characterized in that, The benzene condenser (32) is fixedly installed inside the benzene condensing plate (31), the second funnel (33) is fixedly installed at the bottom of the benzene condensing plate (31), the second guide plate (34) is fixedly installed inside the benzene tank (37), the second support plate (35) is fixedly installed on the outer surface of the disc (7), and the benzene collection cup (36) is clamped on the top of the second support plate (35).

8. The distillation apparatus for a benzophenone-based ultraviolet absorber according to claim 7, characterized in that, The petroleum ether distillation assembly (5) includes a third ring plate (38), a petroleum ether condenser plate (39), a petroleum ether condenser (40), a third funnel (41), a flow guide plate (42), a third support plate (43), and a petroleum ether collection cup (44). The third ring plate (38) is fixedly installed on the top of the disc (7). The petroleum ether condenser plate (39) is fixedly installed on one side of the third ring plate (38). A petroleum ether groove (45) is provided between the petroleum ether condenser plate (39) and the third ring plate (38). The petroleum ether condenser (40) is fixedly installed inside the petroleum ether condenser plate (39). The third funnel (41) is fixedly installed at the bottom of the petroleum ether condenser plate (39). The flow guide plate (42) is fixedly installed at the bottom of the third funnel (41). The third support plate (43) is fixedly installed on the outer surface of the disc (7). The petroleum ether collection cup (44) is clamped on the top of the third support plate (43).

9. A production process for a benzophenone-based ultraviolet absorber, comprising using the distillation apparatus for a benzophenone-based ultraviolet absorber as described in claim 8, characterized in that, Includes the following steps: S1: Concentrated hydrochloric acid was slowly added dropwise to an equimolar amount of triethylamine under constant stirring. The reaction was vigorous and released a large amount of heat. After the reaction was completed, the mixture was subjected to rotary evaporation under reduced pressure at 60°C for 8 hours to remove water from the reaction mixture. The resulting white solid was triethylamine hydrochloride. Place it in a desiccator for later use; S2: Before each catalytic synthesis of benzophenone experiment, a certain amount of... and waterless The ionic liquid is obtained by grinding the mixture thoroughly in a mortar. S3: Synthesis of benzophenone: A certain amount of benzoyl chloride, benzene, and... were added to a 50 mL three-necked flask. An ionic liquid catalyst was used. The magnetic stirring was started, and the reaction temperature was maintained at 80°C. The mixture was refluxed for a certain period of time. After the reaction was completed, it was cooled to room temperature. Then, the reaction solution and 5-6 times its volume of petroleum ether were added to a separatory funnel. The catalyst was separated from the reaction system. Unreacted benzoyl chloride, benzene, the product benzophenone and petroleum ether were in the upper layer. The upper mixture was then taken out for qualitative and quantitative analysis. S4: Place the upper mixture in the distillation tray (13) and place the distillation tray (13) on the automatic turntable (12). Close the door (15) and start the distillation plate (11) to distill the upper mixture through the controller (18) and thermometer (19). Start the automatic turntable (12) to drive the upper mixture to rotate through the distillation tray (13). When the temperature reaches 30°C... ~60 At that time, the petroleum ether in the upper mixture evaporates, and the petroleum ether vapor enters the petroleum ether condenser (40) through the third ring plate (38) and the petroleum ether condensing plate (39) along the first guide plate (10) for condensation. The petroleum ether condensate flows into the petroleum ether collection cup (44) along the third funnel (41) and the guide plate (42). S5: After the petroleum ether has condensed, start the rotary motor (8) to drive the disc (7) to rotate. The disc (7) drives the benzoyl chloride distillation assembly (3), the benzene distillation assembly (4), and the petroleum ether distillation assembly (5) to rotate, so that the slot (14) is connected to the second ring plate (30). The controller (18) heats the distillation plate (11). When the temperature reaches 80.1℃... ~196 At this time, the benzene in the upper mixture evaporates, and the benzene vapor is guided by the second guide plate (34) through the second ring plate (30) and the benzene condensing plate (31) to the benzene condenser (32) for condensation. The benzene condensate flows into the benzene collection cup (36) through the second funnel (33). Referring to the above steps, the rotary motor (8) is started to drive the disc (7) to rotate, so that the first ring plate (22) is connected to the slot (14). The controller (18) heats the distillation plate (11). When the temperature reaches 197°C, the distillation plate (11) is heated. ~304 At that time, the benzoyl chloride in the upper mixture evaporates. The benzoyl chloride vapor passes through the first guide plate (10), the first ring plate (22), and the benzoyl chloride condenser plate (23) and enters the benzoyl chloride condenser (24) through the one-way valve (26) for condensation. The benzoyl chloride condensate flows into the benzoyl chloride collection cup (28) through the first funnel (25). After the benzoyl chloride distillation is completed, the upper mixture in the distillation pan (13) is left with benzophenone.

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