Electronic-grade ultraviolet light absorber UV-1577 production control device and control method thereof

Abstract

The invention discloses a production control device for an electronic-grade ultraviolet light absorber UV-1577 and a control method of the production control device. Cyanuric chloride and benzene are used as starting raw materials, and UV-1577 is generated through multi-step reaction under the catalysis of aluminum chloride. The production control device comprises a first reaction kettle and a second reaction kettle, a stirring shaft, stirring blades and a storage bin are arranged in the first reaction kettle, granular aluminum chloride is stored in the storage bin, micropores are formed in the outer wall of the storage bin, and the micropores are controlled to be opened and closed through an adjusting device, so that the aluminum chloride is in contact with or separated from reaction liquid. The synthesis of the UV-1577 is performed through step-by-step reaction, rectification is performed after the first-step reaction, then the subsequent reaction is performed, regular sampling detection is performed in the reaction process of each step, and the reaction endpoint is judged according to the change of the product content. According to the method, side reactions in the rectification process can be reduced, the purity and yield of an intermediate product and a final product are improved, the reaction endpoint control is accurate, the product quality is stable, and the production efficiency is high.

Description

Technical Field

[0001] The present invention relates to the technical field of carrier for catalyst use, and particularly to an electronic grade ultraviolet absorber UV-1577 production control device and its control method. Background Art

[0002] Due to its excellent ultraviolet absorption performance, the demand for electronic grade ultraviolet absorber UV-1577 is increasing in the fields of electronic materials, plastics, coatings, etc. It has been found through research that trichlorocyanuric acid and benzene can be used as starting materials and undergo multiple reactions under the catalysis of aluminum chloride to obtain UV-1577.

[0003] After the first reaction is completed, if the second reaction is carried out directly without rectification, since the solution contains a certain amount of trichlorocyanuric acid and benzene, a large number of side reactions will occur, seriously affecting the purity and yield of the product. If the rectification operation is carried out directly, due to the change in the temperature of the solution and the presence of the aluminum chloride catalyst, the reaction conditions change, and the unreacted trichlorocyanuric acid and benzene will undergo side reactions during the rectification process, resulting in the generation of a large number of side reaction products, which is also not conducive to obtaining a high-purity product.

[0004] Therefore, developing a production control device and control method that can effectively reduce side reactions during the rectification process has become an important issue that needs to be solved urgently. Summary of the Invention

[0005] The object of the present invention is to propose an electronic grade ultraviolet absorber UV-1577 production control device and control method, which improve the carrier for the use of aluminum chloride catalyst during the reaction process, so that the aluminum chloride catalyst is separated from the solution during the rectification process of the solution, thereby reducing the generation of side reactions in the solution during the rectification process; at the same time, after the rectification is completed, the aluminum chloride catalyst can quickly contact the external solution, and then the next reaction can be carried out, thereby effectively improving the production efficiency.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] An electronic grade ultraviolet absorber UV-1577 production control device includes a first reaction kettle and a second reaction kettle. A stirring shaft and stirring blades are arranged in the first reaction kettle. A storage bin is arranged in the first reaction kettle, and granular aluminum chloride is stored inside the storage bin. A plurality of micropores are opened on the outer wall of the storage bin, and the aperture of the micropores is smaller than the diameter of the granular aluminum chloride.

[0008] An adjusting device is also arranged in the storage bin. When the stirring blades are stationary, the adjusting device closes the micropores; when the stirring blades rotate at high speed, the adjusting device controls the micropores to open, and the granular aluminum chloride comes into contact with the reaction liquid in the first reaction kettle, thereby catalyzing the reaction of the solution in the first reaction kettle.

[0009] In the production process, the first-step reaction starts with cyanuric chloride and benzene. It contacts the reaction solution of cyanuric chloride and benzene in the first reaction kettle, thereby catalyzing the reaction to produce 2-chloro-4,6-diphenyl-1,3,5-triazine. After the first-step reaction is completed, rectification is required before the second-step reaction. The second-step reaction also requires an aluminum chloride catalyst. During the rectification process, stirring needs to be stopped. At this time, the regulating device controls the micropores to close, so that the aluminum chloride particles are separated from the reaction solution. At this time, the temperature of the solution in the reaction kettle is adjusted for rectification. Since the aluminum chloride particles are separated from the reaction solution, the generation of side reaction products during the rectification process can be effectively reduced. After the rectification is completed, resorcinol is added and stirring is started. At this time, the aluminum chloride comes into contact with the external solution again, thereby continuing to catalyze the reaction.

[0010] By the rotation state of the stirring blades, the start and stop of the first-step and second-step reactions are accurately controlled respectively, ensuring that after the first-step reaction is completed, the contact between the aluminum chloride and the reaction solution can be stopped in time, avoiding the continuous reaction of the remaining cyanuric chloride and benzene to produce by-products, and effectively improving the purity and yield of the intermediate product and the final product.

[0011] Preferably, the storage bin is fixed on the side wall of the stirring blade, and the micropores are arranged on the side wall of the storage bin away from the stirring blade. It also includes a sealing plate, and communication holes corresponding to the micropores one by one are arranged on the sealing plate. When the stirring blade is stationary, the communication holes on the sealing plate are misaligned with the micropores, and the sealing plate closes the micropores. When the stirring blade rotates at a high speed, the sealing plate moves accordingly, and the communication holes are connected to the micropores.

[0012] In this device, the storage bin is fixed on the side wall of the stirring blade, and the micropores are arranged on the side wall away from the stirring blade. When the stirring blade is stationary, the communication holes on the sealing plate are misaligned with the micropores, and the sealing plate blocks in front of the micropores, thereby closing the micropores. When the stirring blade rotates at a high speed, due to the action of centrifugal force, the sealing plate moves accordingly, so that the communication holes are aligned with the micropores and connected, realizing the opening of the micropores. The aluminum chloride particles in the storage bin can pass through the micropores and the communication holes to contact the reaction solution and play a catalytic role. By controlling the rotation speed of the stirring blade to control the movement of the sealing plate, the opening and closing of the micropores are realized, so that the aluminum chloride can participate in the reaction timely according to the reaction process, reducing the occurrence of side reactions. This control method based on mechanical movement does not require a complex electronic control system, is relatively simple to operate, and reduces the complexity and maintenance cost of the equipment.

[0013] Preferably, guide plates are provided on the side wall of the storage bin far from the stirring blades. There are two guide plates, which are respectively arranged on the upper and lower sides of the sealing plate. The guide plates are provided with tracks for the sealing plate to insert. The length of the track is greater than the length of the sealing plate. Limit plates for limiting the sealing plate are provided on both sides of the track. When the stirring blades are stationary, the sealing plate is located on the side of the track close to the stirring shaft. When the stirring blades rotate at high speed, the sealing plate moves away from the stirring shaft under the action of centrifugal force and then abuts against the limit plates. At this time, the communication holes are connected to the micropores.

[0014] When the stirring blades are stationary, the sealing plate is located on the side of the track close to the stirring shaft, and at this time the sealing plate closes the micropores. When the stirring blades rotate at high speed, the centrifugal force causes the sealing plate to move along the track away from the stirring shaft. Since there are limit plates on both sides of the track, the sealing plate will abut against the limit plates when it moves to a certain position. At this time, the communication holes are connected to the micropores, and the aluminum chloride particles in the storage bin can contact the reaction solution through the micropores and the communication holes. The setting of the guide plates and the tracks provides a stable path for the movement of the sealing plate, ensuring that the sealing plate remains straight during the movement; the existence of the limit plates can accurately control the moving end point of the sealing plate, ensuring the accurate connection between the communication holes and the micropores every time the micropores are opened, and improving the reliability and repeatability of the device.

[0015] Preferably, a return spring is provided in the track. When the stirring blades change from high-speed rotation to stationary, the sealing plate moves towards the direction of the stirring shaft under the action of the return spring, and then the communication holes and the micropores are misaligned.

[0016] When the stirring blades rotate at high speed, the centrifugal force causes the sealing plate to overcome the elastic force of the return spring and move along the track away from the stirring shaft, and the communication holes are connected to the micropores, enabling the aluminum chloride particles to participate in the reaction. When the stirring blades change from high-speed rotation to stationary, the centrifugal force disappears, and the elastic force of the return spring comes into play, pushing the sealing plate towards the direction of the stirring shaft, misaligning the communication holes and the micropores, and re-closing the micropores to prevent the aluminum chloride particles from continuing to contact the reaction solution. The return spring can make the sealing plate move along the track when the stirring blades stop rotating, thus automatically resetting the sealing plate and quickly closing the micropores without additional operations.

[0017] Preferably, the storage bin is arranged on the side where the stirring blades rotate.

[0018] By arranging the storage bin on the side where the stirring blades rotate, during the stirring process of the stirring blades, the solution can more efficiently contact the aluminum chloride particles in the micropores during the stirring process, accelerating the reaction start-up speed.

[0019] Preferably, a detachable inner liner is provided in the storage bin. The aluminum chloride catalyst is arranged in the inner liner. Exchange holes are provided on the inner liner. When the inner liner is installed in the storage bin, the exchange holes are aligned with the micropores one by one. A hatch for taking out the inner liner is provided on the upper end face of the storage bin.

[0020] A detachable inner tank is arranged in the storage bin, and the aluminum chloride catalyst is placed in the inner tank. When the stirring blade rotates at a high speed to move the sealing plate and the micropores are communicated with the communicating holes, the exchange holes on the inner tank are aligned with the micropores of the storage bin one by one, and the aluminum chloride catalyst can contact the reaction solution through the exchange holes, micropores and communicating holes, so as to play a catalytic role. When it is necessary to replace or supplement the aluminum chloride catalyst, the operation can be carried out by opening the door on the upper end face of the storage bin and taking out the inner tank; the detachable inner tank design makes it simple and fast to replace and supplement the aluminum chloride catalyst, without complex operations on the whole storage bin, reducing the maintenance time and cost. When the door is closed, the door presses tightly against the inner tank.

[0021] Preferably, positioning rods are arranged in the storage bin, positioning holes for the positioning rods to extend into are arranged on the outer wall of the inner tank, and a charging door is arranged on the side wall of the inner tank.

[0022] The cooperation of the positioning rods and the positioning holes ensures that the inner tank can be accurately installed at the designated position in the storage bin, ensuring the accurate alignment of the exchange holes and the micropores, so that the aluminum chloride catalyst can be normally released and play a role; on the other hand, the cooperation of the positioning rods and the positioning holes realizes the limit of the inner tank, ensuring that the position of the inner tank does not move during the rotation of the stirring blade.

[0023] A production control method for electronic grade ultraviolet absorber UV-1577, which comprises the following production steps:

[0024] Step 1: Add cyanuric chloride and benzene into the first reaction kettle, close the first reaction kettle and heat it to 130°C - 160°C, start stirring, and carry out the Friedel-Crafts arylation reaction of cyanuric chloride and benzene under the catalysis of aluminum chloride to obtain 2-chloro-4,6-diphenyl-1,3,5-triazine; after the reaction is completed, stop stirring and heat for rectification to distill out benzene and cyanuric chloride.

[0025] Step 2: Add resorcinol and chlorobenzene into the first reaction kettle, heat and start stirring at the same time, and carry out the Friedel-Crafts reaction of 2-chloro-4,6-diphenyl-1,3,5-triazine and resorcinol under the catalysis of aluminum chloride to obtain 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine. After the reaction is completed, stop stirring.

[0026] Step 3: Transfer 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine from the first reaction kettle to the second reaction kettle, add bromohexane and sodium carbonate, heat and start stirring to obtain the product UV-1577.

[0027] The addition of distillation operation between the first reaction and the second reaction can effectively improve the purity of the intermediate product. The agitator needs to stop running during the distillation process. At this time, the aluminum chloride catalyst is also out of contact with the external solvent, which effectively reduces the generation of side reactions during the distillation process, thereby reducing the generation of side reaction products during the distillation process. Strict step-by-step reaction and control conditions help to obtain the final product UV-1577 with stable quality to meet the needs of different application fields. Chlorobenzene as a solvent can promote the reaction.

[0028] Preferably, during the reaction of step 1, the solution in the first reaction kettle 110 is sampled and tested every hour to monitor the content of the product 2-chloro-4,6-diphenyl-1,3,5-triazine in the solution, and the mass content of 2-chloro-4,6-diphenyl-1,3,5-triazine is calculated as a percentage of the total mass of the solution. When the change in the data of two consecutive tests is less than 2%, the reaction is considered to be completed and the stirring is turned off.

[0029] During the reaction of step 2, the solution in the first reaction kettle 110 is sampled and tested every hour to monitor the content of the product 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine in the solution, and the mass content of 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine is calculated as a percentage of the total mass of the solution. When the change in the data of two adjacent tests is less than 2%, the reaction is considered to be completed and the stirring is turned off.

[0030] During the reaction process of step 3, the solution in the second reactor is sampled and tested every hour to monitor the content of the product UV-1577 in the solution, and the percentage of the mass content of UV-1577 to the total mass of the solution is calculated. When the change in the data of two adjacent tests is less than 2%, the reaction is considered to be completed and the stirring is turned off.

[0031] During the entire reaction process, the solution in the first reactor and the second reactor is sampled and tested every hour in steps one, two, and three, and the content change of the reaction product in each step in the solution is monitored in real time. When the percentage change of the mass content of the product in the total mass of the solution in two adjacent detection data is less than the set 2%, the reaction step is judged to be completed, and then the stirring is turned off. This judgment method is based on the fact that when the chemical reaction is close to completion, the speed of product generation will gradually slow down, and the endpoint of the reaction is determined by monitoring the slight change in the product content. Through strict control of the reaction endpoint, the quality of the product produced each time is more stable and the difference between batches is reduced. At the same time, it avoids unnecessary extension of reaction time, saves energy, raw materials and production time, and improves production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1Schematic diagram of the overall structure of the stirring blade and the storage bin in the embodiment;

[0033] Figure 2 Schematic diagram of the structure of the storage bin and the sealing plate in the embodiment;

[0034] Figure 3 Schematic diagram of the structure of the storage bin in the embodiment;

[0035] Figure 4 Exploded view of the storage bin in the embodiment;

[0036] Figure 5 Schematic diagram of the structure of the inner tank in the direction of the exchange hole in the embodiment;

[0037] Figure 6 Schematic diagram of the internal structure of the storage bin in the embodiment;

[0038] Figure 7 Schematic diagram of the structure of the inner tank in the direction of the material changing door in the embodiment;

[0039] Figure 8 Structural formula reaction formula for the first step of synthesizing UV-1577 of the present invention;

[0040] Figure 9 Structural formula reaction formula for the first step of synthesizing UV-1577 of the present invention;

[0041] Figure 10 Structural formula reaction formula for the first step of synthesizing UV-1577 of the present invention.

[0042] In the figure: 120, stirring shaft; 1201, stirring blade; 130, storage bin; 1301, micropores; 1302, guide plate; 1303, track; 1304, limiting plate; 1305, bin door; 1306, positioning rod; 140, sealing plate; 1401, communication hole; 150, spring; 160, inner tank; 1601, exchange hole; 1602, positioning hole; 1604, material changing door. Detailed implementation manners

[0043] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0044] Refer to the attached Figure 1 - attached Figure 7 , the production control device for electronic grade ultraviolet absorber UV-1577 includes:

[0045] The first reaction kettle and the second reaction kettle are provided with a stirring shaft 120 and stirring blades 1201 inside the first reaction kettle. A storage bin 130 is arranged inside the first reaction kettle. In this embodiment, the storage bin 130 is fixed on the side wall of the stirring blade 1201, and the storage bin 130 is arranged on the side where the rotation direction of the stirring blade 1201 is located.

[0046] The storage bin 130 stores granular aluminum chloride inside. A plurality of micropores 1301 are formed on the side wall of the storage bin 130 away from the stirring blade 1201, and the aperture of the micropores 1301 is smaller than the diameter of the granular aluminum chloride.

[0047] The storage bin 130 is provided with an adjusting device for controlling the opening and closing of the micropores 1301. The adjusting device includes a sealing plate 140. Communication holes 1401 corresponding to the micropores 1301 one by one are arranged on the sealing plate 140. Guide plates 1302 are arranged on the side wall away from the stirring blade 1201. There are two guide plates 1302 and they are respectively arranged on the upper and lower sides of the sealing plate 140. Tracks 1303 for inserting the sealing plate 140 are arranged on the guide plates 1302. The length of the tracks 1303 is greater than the length of the sealing plate 140. Limit plates 1304 for limiting the sealing plate 140 are arranged on both sides of the tracks 1303.

[0048] A return spring 150 is arranged inside the track 1303. When the stirring blade 1201 is stationary, the sealing plate 140 is located on the side of the track 1303 close to the stirring shaft 120. The communication holes 1401 on the sealing plate 140 are misaligned with the micropores 1301, and the sealing plate 140 closes the micropores 1301. When the stirring blade 1201 rotates at a high speed, the sealing plate 140 moves in the direction away from the stirring shaft 120 under the action of centrifugal force, and then abuts against the limit plate 1304. At this time, the communication holes 1401 are connected with the micropores 1301, and the granular aluminum chloride comes into contact with the reaction liquid phase in the first reaction kettle, thereby catalyzing the reaction of the solution in the first reaction kettle. When the stirring blade 1201 changes from high-speed rotation to stationary, the sealing plate 140 moves in the direction of the stirring shaft 120 under the action of the return spring 150, so that the communication holes 1401 and the micropores 1301 are misaligned.

[0049] In order to facilitate the replacement of the aluminum chloride catalyst in the storage bin 130, a detachable inner liner 160 is arranged inside the storage bin 130 in this embodiment. The aluminum chloride catalyst is arranged inside the inner liner 160. Exchange holes 1601 are formed on the inner liner 160. When the inner liner 160 is installed inside the storage bin 130, the exchange holes 1601 are aligned with the micropores 1301 one by one. A hatch 1305 for taking out the inner liner 160 is arranged on the upper end face of the storage bin 130. In this embodiment, the hatch 1305 is fixed on the storage bin 130 with bolts.

[0050] A positioning rod 1306 is provided inside the storage bin 130, and a positioning hole 1602 for the positioning rod 1306 to extend into is provided on the outer wall of the inner tank 160. A material-changing door 1604 is provided on the side wall of the inner tank 160; in this embodiment, the material-changing door 1604 is provided on the side wall of the inner tank 160 away from the exchange hole 1601.

[0051] The working principle of the production control device for electronic grade ultraviolet absorber UV-1577 is as follows: When the solution reacts in the first reaction kettle, stirring needs to be started to accelerate the reaction process. At this time, the stirring blade 1201 rotates, and the sealing plate 140 moves away from the stirring shaft 120 under the action of centrifugal force, so that the communication hole 1401 on the sealing plate 140 is connected to the micropore 1301, so as to ensure that when the stirring blade 1201 stirs, the aluminum chloride catalyst in the storage bin 130 contacts the external solution, and then the catalytic reaction proceeds.

[0052] When the first-step reaction is completed, impurities need to be removed by rectification to make the intermediate product in the solution in the first reaction kettle purer and improve the production efficiency of the next-step reaction; heating is required during the rectification process, which in turn causes the temperature of the solution in the first reaction kettle to change. Due to the characteristics of organic reactions, there is still a certain amount of reaction raw materials remaining in the first reaction kettle at this time. Under the action of the catalyst, due to the change in the temperature of the solution in the first reaction kettle, a large number of side reactions will occur in the first reaction kettle, which in turn affects the rectification effect.

[0053] During the rectification process, stirring needs to be turned off. At this time, the sealing plate 140 moves towards the direction close to the stirring shaft 120 under the action of the spring 150, so that the communication hole 1401 is misaligned with the micropore 1301, and the aluminum chloride catalyst is disconnected from the external solvent, which can effectively reduce the generation of side reactions and improve the rectification effect.

[0054] Among them, the aluminum chloride catalyst is arranged in the storage bin 130. When the solution in the first reaction kettle reaches the specified temperature, stirring is started again. At this time, the aluminum chloride catalyst contacts the external solution, which can effectively avoid the occurrence of side reactions caused by the aluminum chloride catalyst during the heating process.

[0055] Process flow description of the production control method for electronic grade ultraviolet absorber UV-1577:

[0056] As Figures 8 - 10 shown, the chemical synthesis steps for synthesizing electronic grade ultraviolet absorber UV-1577 in the present invention are as follows:

[0057] 1. Cyanuric chloride and benzene react under the catalysis of aluminum chloride to generate 2-chloro-4,6-diphenyl-1,3,5-triazine;

[0058] 2. 2-chloro-4,6-diphenyl-1,3,5-triazine and resorcinol react under the catalysis of aluminum chloride to form 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine;

[0059] 3. 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine, bromohexane and sodium carbonate react to form UV-1577.

[0060] The structural formula of UV-1577 is as follows:

[0061]

[0062] The specific production process is as follows: Among them, cyanuric chloride, benzene and resorcinol are dehydrated before adding.

[0063] 1. Add cyanuric chloride and benzene into the first reaction kettle, where the molar ratio of benzene to cyanuric chloride is ten to one. Seal the first reaction kettle, heat up to 130°C - 160°C, and start stirring; make them react under the action of granular aluminum chloride catalyst to form 2-chloro-4,6-diphenyl-1,3,5-triazine; during the reaction, sample and detect every hour, calculate the percentage of the mass content of 2-chloro-4,6-diphenyl-1,3,5-triazine in the total mass of the solution. When the percentage calculated from the detection data of two adjacent times is subtracted and the change is less than 2%, the reaction is regarded as completed, and the stirring is turned off.

[0064] 2. After the stirring stops, start to cool down. When the temperature drops to 80°C, open the pipeline from the first reaction kettle to the No. 1 recovery tank and keep the temperature constant; distill out benzene to the No. 1 recovery tank; when there is no obvious distillate in the pipeline, close the pipeline from the first reaction kettle to the No. 1 recovery tank;

[0065] While step one reacts to form 2-chloro-4,6-diphenyl-1,3,5-triazine, two by-products, 2,4-dichloro-6-phenyl-1,3,5-triazine and 2,4,6-triphenyl-1,3,5-triazine, will also be generated.

[0066] Add silylated molecular sieve (pore diameter 0.65nm) into the first reaction kettle, stir at 60°C for 1.5 hours to adsorb the by-product 2,4,6-triphenyl-1,3,5-triazine, and then take out the silylated molecular sieve.

[0067] Then add ZSM-5 molecular sieve (pore diameter 0.45nm) to adsorb 2,4-dichloro-6-phenyl-1,3,5-triazine, and then take out the ZSM-5 molecular sieve.

[0068] 3. Under normal pressure, continue to heat the first reactor to 190°C, open the pipeline from the first reactor to the No. 2 recovery tank, distill cyanuric chloride into the No. 2 recovery tank. When there is no obvious distillate in the pipeline, close the pipeline from the first reactor to the No. 2 recovery tank, slowly cool the reaction solution to -10°C, and keep it for 4 hours to preferentially crystallize 2-chloro-4,6-diphenyl-1,3,5-triazine (solubility 0.12 g / mL, 25°C). Filter to remove low-substituted by-products in the residual liquid phase; wash the crystals twice with cold ethanol (-20°C) to further remove entrapped impurities.

[0069] 4. Add resorcinol and chlorobenzene into the first reactor, heat to 90°C - 95°C, start stirring. During the reaction, take samples for detection every hour, calculate the percentage of the mass content of 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine in the total mass of the solution. When the difference between the percentages calculated from two adjacent detection data is less than 2%, consider the reaction completed and stop stirring.

[0070] 5. Remove chlorobenzene, resorcinol and 2-chloro-4,6-diphenyl-1,3,5-triazine from the solution; transfer the purified 2-chloro-4,6-diphenyl-1,3,5-triazine to the second reactor.

[0071] 6. Add 1-bromohexane and sodium carbonate into the second reactor; heat and start stirring for the reaction. During the reaction, take samples for detection every hour, calculate the percentage of the mass content of UV-1577 in the total mass of the solution. When the difference between the percentages calculated from two adjacent detection data is less than 2%, consider the reaction completed and stop stirring.

[0072] 7. Add an appropriate amount of water into the second reactor, let it stand for liquid separation and then stop stirring. Open the pipeline from the second reactor to the No. 5 recovery tank to separate the aqueous phase into the No. 3 recovery tank to remove NaBr, sodium carbonate and water-soluble impurities.

[0073] 8. Add saturated brine into the organic phase of the second reactor, start stirring and wash for 10 minutes; let it stand for liquid separation and then stop stirring. Open the pipeline from the second reactor to the No. 4 recovery tank to separate the aqueous phase into the No. 4 recovery tank to remove residual NaBr and resorcinol.

[0074] 9. Heat the second reactor to 80°C - 85°C, start the vacuum distillation device; distill 1-bromohexane and recover it to the No. 5 recovery tank to remove 1-bromohexane and low-boiling impurities. When there is no liquid drop falling from the condenser, close the vacuum device.

[0075] 10. Add ethanol to the remaining crude product in the second reactor, heat to 60°C - 65°C to dissolve; start stirring and slowly cool to 0°C - 5°C for crystallization, keep it for 2 hours; stop stirring, and obtain electronic-grade UV-1577 crystals by crystallization method.

[0076] As described above, it is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, making equivalent substitutions or changes, shall be covered by the protection scope of the present invention.

Claims

1. Electronic grade ultraviolet absorber UV-1577 production control device, including a first reaction kettle and a second reaction kettle, wherein a stirring shaft (120) and stirring blades (1201) are arranged in the first reaction kettle, and it is characterized in that: There is a storage bin (130) arranged inside the first reaction kettle. Granular aluminum chloride is stored inside the storage bin (130). A plurality of micropores (1301) are formed on the outer wall of the storage bin (130), and the aperture of the micropores (1301) is smaller than the diameter of the granular aluminum chloride. An adjusting device is also provided inside the storage bin (130). When the stirring blade (1201) is stationary, the adjusting device closes the micropores (1301). When the stirring blade (1201) rotates at a high speed, the adjusting device controls the opening of the micropores (1301), and the granular aluminum chloride comes into contact with the reaction liquid phase inside the first reaction kettle, thereby catalyzing the reaction of the solution inside the first reaction kettle.

2. The production control device for electronic grade ultraviolet absorber UV-1577 according to claim 1, wherein: The storage bin (130) is fixed on the side wall of the stirring blade (1201), and the micropores (1301) are arranged on the side wall of the storage bin (130) away from the stirring blade (1201). A sealing plate (140) is further included. Communication holes (1401) corresponding to the micropores (1301) one by one are arranged on the sealing plate (140). When the stirring blade (1201) is stationary, the communication holes (1401) on the sealing plate (140) are misaligned with the micropores (1301), and the sealing plate (140) closes the micropores (1301). When the stirring blade (1201) rotates at a high speed, the sealing plate (140) moves accordingly, and the communication holes (1401) are connected to the micropores (1301).

3. The production control device for electronic-grade ultraviolet absorber UV-1577 according to claim 2, wherein: Guide plates (1302) are arranged on the side wall of the storage bin (130) away from the stirring blade (1201). There are two guide plates (1302) and they are respectively arranged on the upper and lower sides of the sealing plate (140). Tracks (1303) for inserting the sealing plate (140) are arranged on the guide plates (1302). The length of the tracks (1303) is greater than the length of the sealing plate (140). Limit plates (1304) for limiting the sealing plate (140) are arranged on both sides of the tracks (1303). When the stirring blade (1201) is stationary, the sealing plate (140) is located on the side of the tracks (1303) close to the stirring shaft (120). When the stirring blade (1201) rotates at a high speed, the sealing plate (140) moves in the direction away from the stirring shaft (120) under the action of centrifugal force, and then abuts against the limit plates (1304). At this time, the communication holes (1401) are connected to the micropores (1301).

4. The production control device for the electronic grade ultraviolet absorber UV-1577 according to claim 3, characterized in that: A return spring (150) is arranged inside the tracks (1303). When the stirring blade (1201) changes from high-speed rotation to stationary, the sealing plate (140) moves in the direction of the stirring shaft (120) under the action of the return spring (150), thereby misaligning the communication holes (1401) and the micropores (1301).

5. The production control device of the electronic-grade ultraviolet absorber UV-1577 according to claim 4, wherein: The storage bin (130) is arranged on the side where the stirring blade (1201) rotates.

6. The production control device for the electronic grade ultraviolet absorber UV-1577 according to claim 2, wherein: A detachable inner container (160) is arranged inside the storage bin (130). The aluminum chloride catalyst is arranged inside the inner container (160). Exchange holes (1601) are formed on the inner container (160). When the inner container (160) is installed inside the storage bin (130), the exchange holes (1601) are aligned with the micropores (1301) one by one. A bin door (1305) for taking out the inner container (160) is arranged on the upper end face of the storage bin (130).

7. The production control device for electronic grade ultraviolet absorber UV-1577 according to claim 6, characterized in that: A positioning rod (1306) is provided inside the storage bin (130), a positioning hole (1602) for the positioning rod (1306) to extend into is provided on the outer wall of the inner tank (160), and a material changing door (1604) is provided on the side wall of the inner tank (160).

8. Production control method for electronic grade ultraviolet absorber UV-1577, characterized in that: It includes the following production steps Step 1: Add cyanuric chloride and benzene into the first reaction kettle, seal the first reaction kettle and heat it to 130°C - 160°C, turn on the stirring, and enable cyanuric chloride and benzene to carry out Friedel-Crafts arylation reaction under the catalysis of aluminum chloride to obtain 2-chloro-4,6-diphenyl-1,3,5-triazine; after the reaction is completed, turn off the stirring, and heat for rectification to distill out benzene and cyanuric chloride; Step 2: Add resorcinol and chlorobenzene into the first reaction kettle, heat it, turn on the stirring, and enable 2-chloro-4,6-diphenyl-1,3,5-triazine and resorcinol to carry out Friedel-Crafts reaction under the catalysis of aluminum chloride to obtain 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine. After the reaction is completed, turn off the stirring; Step 3: Transfer 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine from the first reaction kettle to the second reaction kettle, add bromohexane and sodium carbonate, heat and turn on the stirring to obtain the UV-1577 product.

9. According to the production control method of the electronic grade ultraviolet absorber UV-1577 in claim 8, it is characterized in that: During the reaction process of Step 1, sample and detect the solution in the first reaction kettle every hour to monitor the content of the product 2-chloro-4,6-diphenyl-1,3,5-triazine in the solution, calculate the percentage of the mass content of 2-chloro-4,6-diphenyl-1,3,5-triazine in the total mass of the solution. When the change in the detection data of two adjacent times is less than 2%, it is regarded that the reaction is completed and the stirring is turned off; During the reaction process of Step 2, sample and detect the solution in the first reaction kettle every hour to monitor the content of the product 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine in the solution, calculate the percentage of the mass content of 2-(2,4-dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine in the total mass of the solution. When the change in the detection data of two adjacent times is less than 2%, it is regarded that the reaction is completed and the stirring is turned off; During the reaction process of Step 3, sample and detect the solution in the second reaction kettle every hour to monitor the content of the product UV-1577 in the solution, calculate the percentage of the mass content of UV-1577 in the total mass of the solution. When the change in the detection data of two adjacent times is less than 2%, it is regarded that the reaction is completed and the stirring is turned off.

Images