Process for preparing triallyl isocyanurate from isocyanuric acid

Abstract

The invention relates to the technical field of preparation of triallyl isocyanurate, in particular to a process for preparing triallyl isocyanurate from isocyanuric acid. Comprising the following steps: S1, taking isocyanuric acid and chloropropene as reaction raw materials, taking an organic solvent as a reaction medium, taking composite alkali as an acid-binding agent, and taking tetrabutylammonium bromide as a catalyst; the mass ratio of the components is 10: 25: 60: 7: 1; s2, after the reaction is finished, conveying a liquid product of the reaction to a reduced pressure distillation kettle; by arranging the pressure stabilizing reaction kettle, the sliding plate in the pressure stabilizing reaction kettle slides in the kettle body, so that the size of the reaction space in the pressure stabilizing reaction kettle is adjusted to ensure that isocyanuric acid and chloropropene are subjected to stable reaction in a micro-positive pressure environment of 0.25-0.3 MPa, the reaction rate is increased, the yield of triallyl isocyanurate is increased, and the yield of triallyl isocyanurate is increased. And heat energy waste and solvent reduction caused by emission of hydrogen chloride gas are avoided, and energy consumption is reduced.

Description

Technical Field

[0001] This invention relates to the field of triallyl isocyanurate preparation technology, specifically a process for preparing triallyl isocyanurate using isocyanuric acid. Background Technology

[0002] Triallyl isocyanurate, also known as triallyl isocyanurate, crosslinking agent TAIC, etc., is an organic compound that appears as a colorless liquid or crystal. Triallyl isocyanurate is a multifunctional olefin monomer containing aromatic heterocycles. Industrially, it can be used in combination with organic peroxides such as DCP as a vulcanizing agent, crosslinking agent, and modifier for various thermoplastic plastics and ion exchange resins. It is highly efficient, non-toxic, easy to store and transport, and is a widely used polymeric additive. The main synthetic methods for triallyl isocyanurate include: isocyanate method, amination method, and multi-step synthesis method (including halogenation, substitution, and addition reactions). Among them, the isocyanate method involves reacting isocyanuric acid with allyl chloride to produce triallyl isocyanurate. Since isocyanuric acid reacts with allyl chloride to produce hydrogen chloride, in order to improve the conversion rate of isocyanuric acid, an acid-binding agent of equal amount to isocyanuric acid needs to be added to the reaction system to neutralize the hydrogen chloride produced in the reaction. However, the reaction of isocyanuric acid with allyl chloride to form triallyl isocyanurate, the addition of an acid-binding agent will significantly inhibit the generation of hydrogen chloride gas, but hydrogen chloride gas will still be generated. Since the reaction pressure environment is slightly positive, if the reaction vessel is not sealed, the hydrogen chloride gas can evaporate and escape, that is, the pressure is stable. However, the emission of hydrogen chloride gas will not only take away a lot of heat, but also carry away solvent vapor in the reaction system, resulting in waste of heat energy and reduction of solvent. However, if a sealed reaction vessel is used, it will lead to an increase in the reaction pressure environment, which will affect the reaction efficiency and reduce the yield of triallyl isocyanurate. In view of this, in order to overcome the above-mentioned technical problems, the present invention proposes a process for preparing triallyl isocyanurate using isocyanuric acid, which solves the above-mentioned technical problems. Summary of the Invention

[0003] To overcome the shortcomings of existing technologies, this invention proposes a process for preparing triallyl isocyanurate from isocyanuric acid. This invention utilizes a pressure-stabilized reactor, where a sliding plate within the reactor body adjusts the reaction space to ensure stable reaction of isocyanuric acid and allyl chloride under a slightly positive pressure of 0.25–0.3 MPa. This not only improves the reaction rate and increases the yield of triallyl isocyanurate but also avoids the waste of heat energy and solvent reduction caused by the emission of hydrogen chloride gas, thus reducing energy consumption.

[0004] The technical solution adopted by this invention to solve its technical problem is as follows: A process for preparing triallyl isocyanurate from isocyanuric acid, comprising the following steps: S1: Using isocyanuric acid and allyl chloride as reactants, organic solvent as reaction medium, tetrabutylammonium bromide as catalyst, and composite alkali as acid-binding agent, isocyanuric acid, allyl chloride, organic solvent, acid-binding agent, and catalyst are added to a pressure-stabilized reactor in a mass ratio of 10:25:60:7:1. The reaction temperature is controlled at 90-120℃, and the reaction time is 2-3 hours. S2: After the reaction is completed, the liquid product of the reaction is sent to a vacuum distillation kettle. The reaction temperature is 50-70℃. The gaseous product of the distillation is condensed by a condenser. The remaining liquid product is sent to centrifuge No. 1 for centrifugal separation. S3: The liquid separated by centrifugation in centrifuge No. 1 is transferred to centrifuge No. 2 and slowly cooled to 20-30℃. Then, centrifuge No. 2 is controlled to perform solid-liquid separation to obtain crude triallyl isocyanurate. S4: The mother liquor obtained from the separation by centrifuge No. 2 is transported to a vacuum distillation kettle, and the reaction temperature is controlled at 80-120℃ to achieve solvent recovery. The separated crude TAIC is washed 2-3 times with deionized water to finally obtain high-purity TAIC.

[0005] Preferably, in step S1, isocyanuric acid, organic solvent, acid binder and catalyst are first added to the pressure-stabilized reactor, and after the reaction temperature is controlled to rise to 90°C, allyl chloride is then added dropwise to the pressure-stabilized reactor.

[0006] Preferably, in step S1, the pressure inside the pressure-stabilized reactor is maintained at 0.25–0.3 MPa.

[0007] Preferably, the pressure-stabilized reactor includes a reactor body; a heater is embedded in the inner wall of the reactor body; a discharge port is opened at the lower end of the reactor body; a reactor cover is installed at the upper end of the reactor body; a feed port and a liquid addition tank are opened at the upper end of the reactor cover; an end cap is threadedly connected to the port of the liquid addition tank; an air inlet is opened on the surface of the end cap; a rotating rod is rotatably connected inside the reactor body; a blade is fixedly connected to the lower end of the rotating rod; a cylindrical rod is rotatably connected to the lower end of the reactor cover; a cylindrical groove is opened at the lower end of the cylindrical rod, and the rotating rod is slidably connected in the cylindrical groove; A drive motor is fixedly installed on the upper end of the vessel lid; the drive motor is used to drive the rotating rod to rotate; an air passage is opened inside the rotating rod; an annular groove communicating with the liquid addition tank is opened inside the vessel lid; a groove communicating with the annular groove is opened on the surface of the cylindrical rod; a spring hose is installed in the cylindrical groove; one end of the spring hose is connected to the air passage, and the other end is connected to the groove; an air hole communicating with the air passage is opened on the lower end face of the blade; a hydraulic pump is installed on the upper end of the vessel lid; the hydraulic pump is connected to the cylindrical groove through a pipe.

[0008] Preferably, the vessel body has a sliding seal connection to a slide plate; the rotating rod is in sliding seal contact with the slide plate; a connecting rod is provided between the rotating rod and the cylindrical rod; the connecting rod is slidably connected in the cylindrical groove; a circular groove communicating with a spring hose is opened at the lower end of the connecting rod; a sealing plug is slidably sealed in the circular groove; the sealing plug is connected to the bottom of the circular groove by a sealing spring; a through groove is opened on the surface of the slide plate; a pressure sensor is embedded at the lower end of the slide plate. The upper end of the rotating rod has a slot communicating with the air passage; a plug rod is slidably connected in the slot; the plug rod is connected to the bottom of the slot by a support spring; an L-shaped groove is formed on the surface of the plug rod; an arc-shaped groove is formed at the upper end of the rotating rod; and an L-shaped rod is fixedly connected to the lower end of the connecting rod. A clamping unit is installed on the side wall of the slide plate; the slide plate is connected to the inner wall of the vessel through the clamping unit.

[0009] Preferably, the bottom of the arc-shaped groove is provided with an installation groove; a blocking block is slidably connected in the installation groove; the blocking block is connected to the bottom of the installation groove by a blocking spring.

[0010] Preferably, the clamping unit includes a clamping block; the side wall of the slide plate is provided with a clamping groove; the clamping block is slidably and sealingly connected in the clamping groove; the clamping block and the bottom of the clamping groove are connected by a clamping spring; the lower end of the slide plate is provided with an oil groove communicating with the clamping groove; an arc-shaped plate is slidably and sealingly connected in the oil groove.

[0011] Preferably, a baffle is provided inside the through groove; a spherical rod is fixedly connected to the lower end of the baffle; a circular hole is opened on the surface of the baffle; and a one-way pressure regulating valve is installed in the circular hole.

[0012] The beneficial effects of this invention are as follows: This invention utilizes a pressure-stabilized reactor, where a sliding plate moves within the reactor body to adjust the reaction space. This ensures a stable reaction between isocyanuric acid and allyl chloride under a slightly positive pressure of 0.25–0.3 MPa. This not only increases the reaction rate and yield of triallyl isocyanurate but also avoids the waste of heat energy and solvent reduction caused by the emission of hydrogen chloride gas, thus reducing energy consumption.

[0013] This invention, by setting up a sliding plate, allows hydrogen chloride gas to directly contact and exchange heat with isocyanuric acid and organic solvents through the sliding plate, or indirectly through the sliding plate. This directly eliminates the purchase cost of heat exchangers, thereby reducing the overall preparation cost of triallyl isocyanurate (TAIC). At the same time, this design can effectively suppress the volatilization and escape of organic solvents, increase the subsequent solvent recovery, and further reduce material loss and environmental treatment pressure. Attached Figure Description

[0014] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0015] Figure 1 This is a process flow diagram of the present invention; Figure 2 This is a perspective view of the pressure-stabilized reactor used in this invention; Figure 3 This is a schematic diagram of the pressure-stabilized reactor used in this invention; Figure 4 yes Figure 3 Enlarged view of point A in the middle; Figure 5 yes Figure 3 Enlarged view of point B in the middle; Figure 6 This is a schematic diagram of the structure of the pot lid used in this invention; Figure 7 This is a schematic diagram of the connection between the rotating rod and the connecting rod used in this invention; In the diagram: 1. Kettle body; 11. Heater; 12. Discharge port; 13. Rotating rod; 131. Blade; 132. Air passage; 133. Air hole; 14. Slide plate; 141. Through groove; 142. Pressure sensor; 143. Clamping block; 144. Clamping groove; 145. Clamping spring; 146. Oil tank; 147. Arc plate; 15. Slot; 151. Insert rod; 152. Support spring; 153. L-shaped groove; 154. Arc groove; 155. Mounting groove; 156. Blocking block; 157. Blocking spring; 16. Baffle; 161. Ball rod; 162. Round hole; 163. One-way pressure regulating valve; 2. Kettle cover; 21. Feed inlet; 22. Liquid filling tank; 221. End cap; 222. Air inlet; 23. Cylindrical rod; 231. Cylindrical groove; 232. Groove; 233. Spring hose; 24. Drive motor; 25. Annular groove; 26. Hydraulic pump; 27. Connecting rod; 271. Round groove; 272. Sealing plug; 273. Sealing spring; 274. L-shaped rod. Detailed Implementation

[0016] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0017] like Figures 1 to 7 As shown, the process for preparing triallyl isocyanurate from isocyanuric acid according to the present invention includes the following steps: S1: Using isocyanuric acid and allyl chloride as reactants, organic solvent as reaction medium, tetrabutylammonium bromide as catalyst, and composite alkali as acid-binding agent, isocyanuric acid, allyl chloride, organic solvent, acid-binding agent, and catalyst are added to a pressure-stabilized reactor in a mass ratio of 10:25:60:7:1. The reaction temperature is controlled at 90-120℃, and the reaction time is 2-3 hours. S2: After the reaction is completed, the liquid product of the reaction is sent to a vacuum distillation kettle. The reaction temperature is 50-70℃. The gaseous product of the distillation is condensed by a condenser. The remaining liquid product is sent to centrifuge No. 1 for centrifugal separation. S3: The liquid separated by centrifugation in centrifuge No. 1 is transferred to centrifuge No. 2 and slowly cooled to 20-30℃. Then, centrifuge No. 2 is controlled to perform solid-liquid separation to obtain crude triallyl isocyanurate. S4: The mother liquor obtained from the separation by centrifuge No. 2 is transported to a vacuum distillation kettle, and the reaction temperature is controlled at 80-120℃ to achieve solvent recovery. The separated crude TAIC is washed 2-3 times with deionized water to finally obtain high-purity TAIC.

[0018] In one embodiment of the present invention, in step S1, isocyanuric acid, organic solvent, acid binder and catalyst are first added to the pressure-stabilized reactor, and after the reaction temperature is controlled to rise to 90°C, allyl chloride is added dropwise to the pressure-stabilized reactor.

[0019] In one embodiment of the present invention, in step S1, the pressure inside the pressure-stabilized reactor is maintained at 0.25 to 0.3 MPa.

[0020] During operation, isocyanuric acid reacts with allyl chloride to produce triallyl isocyanurate. Adding an acid-binding agent significantly inhibits the generation of hydrogen chloride gas, but some hydrogen chloride gas will still be generated. Since the reaction pressure environment is slightly positive, if the reactor is not sealed, the hydrogen chloride gas can evaporate and escape, i.e., the pressure is stable. However, the emission of hydrogen chloride gas will not only take away a lot of heat, but also carry away solvent vapors from the reaction system, resulting in wasted heat energy and reduced solvent. However, if a sealed reactor is used, the reaction pressure environment will increase, which will affect the reaction efficiency and reduce the yield of triallyl isocyanurate.

[0021] To address this issue, the present invention employs a pressure-stabilized reactor, in which a sliding plate 14 slides within the reactor body 1, thereby adjusting the size of the reaction space within the reactor. This ensures that isocyanuric acid and allyl chloride undergo a stable reaction under a slightly positive pressure environment of 0.25–0.3 MPa. This not only improves the reaction rate and increases the yield of triallyl isocyanurate, but also avoids the waste of heat energy and reduction of solvent caused by the emission of hydrogen chloride gas, thus reducing energy consumption.

[0022] In use, the user first weighs isocyanuric acid, allyl chloride, organic solvent (DMF), acid-binding agent (a mixture of calcium oxide, calcium carbonate, and calcium hydroxide), and catalyst; the mass ratio of each is 10:25:60:10:1. Then, isocyanuric acid, organic solvent, acid-binding agent, and catalyst are added sequentially to a pressure-stabilized reactor, and the reaction temperature is controlled to rise until it reaches 90°C. Then, allyl chloride is added dropwise to the pressure-stabilized reactor. This is because the reaction between isocyanuric acid and allyl chloride is an exothermic reaction (the hydroxyl group of isocyanuric acid undergoes nucleophilic substitution with the chlorine atom of allyl chloride, releasing the heat of reaction). Allyl chloride has high reactivity. If a large amount of allyl chloride is added rapidly at once, it will cause the reaction rate to surge within a unit time, releasing a large amount of heat in a short time, causing the local temperature of the reaction system to rise sharply, resulting in problems such as solvent evaporation and reactant decomposition. The dropwise addition of allyl chloride is used to control the feed rate of allyl chloride and ensure that the heat of reaction is released evenly.

[0023] After the addition of allyl chloride, the reaction temperature is maintained in the range of 90–120°C, and the reaction pressure is 0.25–0.3 MPa for 2 hours to ensure that isocyanuric acid and allyl chloride react fully to form triallyl isocyanurate. The reaction pressure is set at 0.25–0.3 MPa because the boiling point of allyl chloride is around 45°C, and it is easily volatile at room temperature. Since the reaction temperature is in the range of 90–120°C, a large amount of allyl chloride will volatilize under normal pressure, resulting in raw material loss. Therefore, by using a slightly positive reaction pressure, the boiling point of allyl chloride can be increased, keeping it in a liquid state at the reaction temperature, thereby improving utilization. That is, maintaining the reaction pressure at 0.25–0.3 MPa ensures that allyl chloride remains in a liquid state within the range of 90–120°C, thus promoting the stable reaction between isocyanuric acid and allyl chloride.

[0024] After the reaction is complete, the liquid product in vessel 1 is pumped through discharge port 12 to a vacuum distillation vessel using a discharge pump. The reaction temperature is 50-70℃. Unreacted allyl chloride is recovered through vacuum distillation, which heats and distills the liquid allyl chloride into a gaseous product under low pressure. The distilled gaseous product is then sent to a condenser for condensation, allowing the gaseous allyl chloride to condense back into a liquid state, thus recovering the unreacted allyl chloride. The remaining liquid product contains a complex alkali and a catalyst. This liquid product containing the complex alkali and catalyst is sent to centrifuge No. 1 for centrifugal separation, which separates the complex alkali and the catalyst. The resulting liquid contains... The solution consists of triallyl isocyanurate (TAIC) and a solvent. The separated liquid is cooled to 20–30°C to precipitate TAIC crystals. Solid-liquid separation is then performed again to obtain crude TAIC and a mother liquor. The cooling rate must be controlled (e.g., 0.2–0.4°C / min) to prevent excessive crystal precipitation and subsequent purity reduction. The separated mother liquor is transferred to a vacuum distillation vessel and distilled under reduced pressure at a vacuum of 0.09–0.095 MPa and a temperature of 80–120°C to recover the remaining solvent. The crude TAIC crystals are washed 2–3 times with deionized water to obtain high-purity TAIC.

[0025] In one embodiment of the present invention, the pressure-stabilized reactor includes a reactor body 1; a heater 11 is embedded in the inner wall of the reactor body 1; a discharge port 12 is opened at the lower end of the reactor body 1; a reactor cover 2 is installed at the upper end of the reactor body 1; a feed inlet 21 and a liquid addition tank 22 are opened at the upper end of the reactor cover 2; an end cap 221 is threadedly connected to the port of the liquid addition tank 22; an air inlet 222 is opened on the surface of the end cap 221; a rotating rod 13 is rotatably connected inside the reactor body 1; a blade 131 is fixedly connected to the lower end of the rotating rod 13; a cylindrical rod 23 is rotatably connected to the lower end of the reactor cover 2; a cylindrical groove 231 is opened at the lower end of the cylindrical rod 23; the rotating rod 13 is slidably connected in the cylindrical groove 231; the... A drive motor 24 is fixedly installed on the upper end of the vessel lid 2; the drive motor 24 is used to drive the rotating rod 13 to rotate; an air passage 132 is opened inside the rotating rod 13; an annular groove 25 communicating with the liquid filling tank 22 is opened inside the vessel lid 2; a groove 232 communicating with the annular groove 25 is opened on the surface of the cylindrical rod 23; a spring hose 233 is installed in the cylindrical groove 231; one end of the spring hose 233 is connected to the air passage 132, and the other end is connected to the groove 232; an air hole 133 communicating with the air passage 132 is opened on the lower end face of the blade 131; a hydraulic pump 26 is installed on the upper end of the vessel lid 2; the hydraulic pump 26 is connected to the cylindrical groove 231 through a pipe.

[0026] In one embodiment of the present invention, a sliding plate 14 is slidably and sealed inside the vessel body 1; the rotating rod 13 is in slidable and sealed contact with the sliding plate 14; a connecting rod 27 is provided between the rotating rod 13 and the cylindrical rod 23; the connecting rod 27 is slidably connected in the cylindrical groove 231; a circular groove 271 communicating with the spring hose 233 is opened at the lower end of the connecting rod 27; a sealing plug 272 is slidably and sealed in the circular groove 271; the sealing plug 272 is connected to the bottom of the circular groove 271 by a sealing spring 273; a through groove 141 is opened on the surface of the sliding plate 14; a pressure sensor 142 is embedded at the lower end of the sliding plate 14. The upper end of the rotating rod 13 has a slot 15 communicating with the air passage 132; a plug rod 151 is slidably connected in the slot 15; the plug rod 151 is connected to the bottom of the slot 15 by a support spring 152; an L-shaped groove 153 is formed on the surface of the plug rod 151; an arc-shaped groove 154 is formed at the upper end of the rotating rod 13; and an L-shaped rod 274 is fixedly connected to the lower end of the connecting rod 27. A clamping unit is installed on the side wall of the slide plate 14; the slide plate 14 is connected to the inner wall of the vessel body 1 through the clamping unit.

[0027] In one embodiment of the present invention, the bottom of the arc-shaped groove 154 is provided with an installation groove 155; a blocking block 156 is slidably connected in the installation groove 155; the blocking block 156 and the bottom of the installation groove 155 are connected by a blocking spring 157.

[0028] In one embodiment of the present invention, the clamping unit includes a clamping block 143; a clamping groove 144 is provided on the side wall of the slide plate 14; the clamping block 143 is slidably and sealingly connected in the clamping groove 144; the clamping block 143 and the bottom of the clamping groove 144 are connected by a clamping spring 145; an oil groove 146 communicating with the clamping groove 144 is provided at the lower end of the slide plate 14; an arc-shaped plate 147 is slidably and sealingly connected in the oil groove 146.

[0029] In one embodiment of the present invention, a baffle 16 is provided inside the through groove 141; a spherical rod 161 is fixedly connected to the lower end of the baffle 16; a circular hole 162 is opened on the surface of the baffle 16; a one-way pressure regulating valve 163 is installed in the circular hole 162.

[0030] During operation, initially, the vessel lid 2 and vessel body 1 are separated. The user uses a crane to lift the rotating rod 13. Due to the push of the clamping block 143 on the side wall of the sliding plate 14 by the clamping spring 145, it is in close contact with the inner wall of the vessel body 1. The clamping block 143 is made of fluororubber, which results in a high coefficient of friction. This allows the sliding plate 14 to be stably supported by the clamping block 143 and placed inside the vessel body 1. Therefore, when the crane lifts the rotating rod 13, the rotating rod 13 and the sliding plate 14 slide into contact. However, the rotating rod 13 drives the blade 131 to rise and approach the arc plate 147. When the blade 131 contacts the arc plate 147, it continues to rise under the pull of the rotating rod 13, causing the blade 131 to push the arc plate 147 into the oil tank 14. 6. The hydraulic oil in the oil tank 146 flows into the clamping groove 144, causing the clamping block 143 in the clamping groove 144 to be pushed by the hydraulic oil and squeeze the clamping spring 145 into the clamping groove 144, so that the clamping block 143 moves away from the inner wall of the vessel body 1 and separates from the inner wall of the vessel body 1. At this time, the crane lifts the slide plate 14 through the rotating rod 13 and the blade 131 until the slide plate 14 is separated from the vessel body 1. At this time, the user puts the acid binder and catalyst into the vessel body 1, and then controls the crane to lower the slide plate 14, so that the slide plate 14 falls into the vessel body 1 and continues to slide and connect with the vessel body 1 until the blade 131 contacts the bottom of the vessel body 1. At this time, the rotating rod 13 is separated from the crane, and the addition of the acid binder and catalyst is completed.

[0031] After adding the acid binder and catalyst, a crane is used to hoist the vessel lid 2 to the upper part of the vessel body 1, so that the connecting rod 27 below the vessel lid 2 is aligned with the rotating rod 13. The hydraulic pump 26 is then operated, causing it to deliver hydraulic oil through the pipeline into the cylindrical groove 231. The hydraulic oil entering the cylindrical groove 231 pushes the connecting rod 27 out of the cylindrical groove 231, causing the connecting rod 27 to push the lower L-shaped rod 274 closer to the rotating rod 13, until the L-shaped rod 274 aligns with the rotating rod 13. Upon contact at the upper end, the drive motor 24 is then controlled to operate. Since the output shaft of the drive motor 24 is connected to the cylindrical rod 23 via a belt drive, the drive motor 24 drives the cylindrical rod 23 to rotate. This causes the cylindrical rod 23 to rotate the connecting rod 27, which slides within the cylindrical groove 231. The connecting rod 27 then drives the L-shaped rod 274 to rotate, causing the L-shaped rod 274 to rotate at the upper end of the rotating rod 13 until the L-shaped rod 274 is aligned with the arc-shaped groove 154. At this point... Hydraulic oil pushes the connecting rod 27, causing the L-shaped rod 274 to enter the arc-shaped groove 154. Because the blocking block 156 in the mounting groove 155 is pushed by the blocking spring 157, it extends out of the mounting groove 155 and enters the arc-shaped groove 154, thus sealing the arc-shaped groove 154 to prevent external solid impurities from falling in and clogging it. Therefore, during the process of the L-shaped rod 274 entering the arc-shaped groove 154, the L-shaped rod 274 pushes the blocking block 156 to compress the blocking spring. Spring 157 enters the mounting groove 155 until L-shaped rod 274 is fully inserted into arc groove 154. Because the arc groove 154 is L-shaped, it forms a convex shape with the mounting groove 155. Therefore, the control drive motor 24 drives the connecting rod 27 to rotate L-shaped rod 274, so that L-shaped rod 274 rotates and slides along arc groove 154 until the rod wall of L-shaped rod 274 is blocked by the upper wall of arc groove 154. At this time, the lower end of L-shaped rod 274 is inserted into arc groove 154.

[0032] After the rotating rod 13 is connected to the connecting rod 27, the lid 2 is fixed to the body 1 with screws. Then, the feed port 21 is opened, and the isocyanuric acid and organic solvent are divided into two equal portions. One portion is poured into the body 1 from the feed port 21. At this time, the isocyanuric acid and organic solvent flow to the upper end of the slide plate 14. Since the channel 141 is blocked by the baffle 16, the isocyanuric acid and organic solvent located at the upper end of the slide plate 14 will not flow from the channel 141 to the lower end of the slide plate 14. At this time, the isocyanuric acid and organic solvent are located at the upper end of the slide plate 14.

[0033] To allow isocyanuric acid and organic solvent to react below the slide plate 14, the hydraulic pump 26 is controlled to draw back the hydraulic oil in the cylindrical groove 231. This causes the connecting rod 27 to enter the cylindrical groove 231 under hydraulic pressure. The connecting rod 27 then pulls the wall of the arc-shaped groove 154 via the L-shaped rod 274, causing the rotating rod 13 to rise. The rotating rod 13 then causes the slide plate 14 to rise. During the rise of the slide plate 14, the drive motor 24 is controlled to operate, enabling the drive motor 24 to drive the connecting rod 27 and the rotating rod 154. 3. Rotation causes the rotating rod 13 to drive the blade 131 to rotate on the lower end face of the slide plate 14, making the blade 131 slide into contact with the lower end face of the slide plate 14 until the blade 131 rotates to the ball rod 161. Since the lower end of the ball rod 161 is spherical, when the blade 131 contacts the ball rod 161, the curved surface of the lower end of the ball rod 161 is blocked by the blade 131 and rises, causing the ball rod 161 to push the upper connected baffle 16 to rise, causing the baffle 16 to extend out of the through groove 141, so that the through groove 141 is in a position where In the open state, isocyanuric acid and organic solvent located above slide plate 14 flow through channel 141 to below slide plate 14, allowing them to flow to the bottom of vessel 1. When slide plate 14 rises to a designated height, all isocyanuric acid and organic solvent above slide plate 14 flow below it. The drive motor 24 drives the rotating rod 13, causing the blade 131 to pass over baffle 16. At this point, baffle 16, under its own weight and the pressure of the isocyanuric acid and organic solvent above, falls into channel 141, causing... The passageway 141 is sealed. As the blade 131 continues to rotate and passes over the arc plate 147, the clamping block 143 is pushed out of the clamping groove 144 by the restoring force of the clamping spring 145. This causes the hydraulic oil in the clamping groove 144 to be squeezed by the clamping block 143 and enter the oil groove 146, pushing the arc plate 147 out of the oil groove 146. At this time, the slide plate 14 is fixed at a specified height under the support of the clamping block 143. Then, another portion of isocyanuric acid and organic solvent is poured into the upper end of the slide plate 14 through the feed port 21.

[0034] After the slide plate 14 is fixed at the specified height, the hydraulic pump 26 is controlled to deliver hydraulic oil to push the connecting rod 27 down, which in turn pushes the rotating rod 13 down. This causes the rotating rod 13 to drive the blade 131 below the liquid surface of the isocyanuric acid and organic solvent. At this time, the drive motor 24 is controlled to run, which drives the rotating rod 13 to rotate the blade 131. This causes the blade 131 to stir the isocyanuric acid and organic solvent below the slide plate 14, mixing them together. At the same time, the heater 11 is controlled to heat the mixture until it reaches 90°C. During the heating process, steam can be delivered into the vessel 1 through the discharge port 12. This accelerates the heating rate of the isocyanuric acid in the vessel 1 and increases the pressure inside the vessel 1. When the pressure sensor 142 detects that the pressure has increased to 0.25 MPa, room temperature allyl chloride solvent is added to the feeding tank. Then, the end cap 221 is used to cover the liquid tank 22, and the air inlet 222 is connected to the external nitrogen delivery equipment through a nitrogen delivery pipeline.

[0035] During the contact between the connecting rod 27 and the rotating rod 13, the insert rod 151 located in the slot 15 contacts the sealing plug 272, causing the insert rod 151 to push the sealing plug 272 to compress the sealing spring 273 into the circular groove 271. After the insert rod 151 enters the circular groove 271, the compression force of the sealing spring 273 is greater than that of the support spring 152. As the connecting rod 27 and the rotating rod 13 continue to approach each other, the insert rod 151 is blocked by the sealing plug 272 and compresses the support spring 152 into the slot 15. At this time, the circular groove 271 and the slot 15 are connected through the L-shaped groove 153 on the surface of the insert rod 151.

[0036] When adding allyl chloride solution, an external nitrogen delivery device supplies nitrogen gas through a nitrogen delivery pipe into the inlet 222, causing the nitrogen gas to enter the liquid addition tank 22. The nitrogen gas then pushes the allyl chloride solution in the liquid addition tank 22 into the annular groove 25. The allyl chloride solution in the annular groove 25 then flows through the groove 232 and the spring hose 233 into the circular groove 271. The allyl chloride solution in the circular groove 271 flows into the slot 15 through the L-shaped groove 153 on the surface of the insert rod 151. The allyl chloride solution in the slot 15 then enters the vent 133 through the air passage 132 connected to the slot 15, causing the allyl chloride solution to drip out through the vent 133. Since the drive motor 24 can drive the blade 131 to rotate... The rotating blade 131 causes the allyl chloride solution dripping from the lower vent 133 to mix evenly with the isocyanuric acid and organic solvent mixture. The hydraulic pump 26 is controlled to pump hydraulic oil into the cylindrical groove 231, so that the connecting rod 27 in the cylindrical groove 231 can drive the blade 131 to move up and down in the isocyanuric acid and organic solvent mixture through the rotating rod 13 connected to it. This allows the blade 131 to drip the allyl chloride solution at different heights in the isocyanuric acid and organic solvent mixture, so that the allyl chloride solution can fully and stably react with the isocyanuric acid and organic solvent mixture at different heights. Furthermore, by controlling the nitrogen delivery rate, the dripping rate of the allyl chloride solution can be directly controlled.

[0037] Because the reaction between allyl chloride solution and isocyanuric acid produces hydrogen chloride gas, although the acid-binding agent significantly inhibits the generation of hydrogen chloride gas, some hydrogen chloride gas still rises to the space between the slide plate 14 and the mixture. As the hydrogen chloride gas accumulates, the pressure in the area below the slide plate 14 increases. At this point, the pressure sensor 142 senses a pressure increase to 0.3 MPa, controlling the hydraulic pump 26 to draw back the hydraulic oil, causing the blade 131 to pull the slide plate 14 upwards. This increases the space below the slide plate 14 until the pressure sensor 142 senses a pressure increase to 0.25 MPa. When the isocyanuric acid and organic solvent levels above the slide plate 14 rise to the upper limit of the vessel body 1, the hydraulic pump 26 controls the hydraulic pump 26 to pull the blade 131 upward via the rotating rod 13 and squeeze the arc-shaped plate 147 into the oil tank 146. This causes the clamping block 143 to be pushed into the clamping groove 144 by the hydraulic oil. At this time, the hydraulic pump 26 controls the hydraulic pump 26 to deliver hydraulic oil and push the rotating rod 13 to descend rapidly. The rotating rod 13 can drive the slide plate 14 to descend rapidly and squeeze the hydrogen chloride gas, which increases the pressure of the hydrogen chloride gas and pushes the one-way pressure regulating valve 163 in the circular hole 162 to open, thus... Hydrogen chloride gas passes through the one-way pressure regulating valve 163 inside the circular orifice 162 to the area above the slide plate 14. This allows the hydrogen chloride gas to pass through the isocyanuric acid and organic solvent above the slide plate 14, transferring heat from the hydrogen chloride gas to the isocyanuric acid and organic solvent above the slide plate 14. Furthermore, the evaporating solvent mixed in the hydrogen chloride gas also absorbs heat from the isocyanuric acid and organic solvent above the slide plate 14. After the hydrogen chloride gas between the slide plate 14 and the material surface below is discharged above the slide plate 14, the control lever 13 pulls the slide plate 14 upwards, and the drive motor 24 drives the blades... As plate 131 passes over curved plate 147, the position of slide plate 14 is fixed. During the ascent of slide plate 14, the hydrogen chloride gas above slide plate 14 is compressed, causing the hydrogen chloride gas to release heat. The heat released by the hydrogen chloride gas is absorbed by isocyanuric acid and organic solvent above slide plate 14, thereby reducing heat waste. At the same time, the heat of the evaporated solvent is absorbed, causing the evaporated solvent to re-liquefy and fall into the isocyanuric acid and organic solvent above slide plate 14, allowing the solvent to be reused, reducing solvent waste, and increasing the amount of solvent recovered in the future.

[0038] Existing unsealed reactors use heat exchangers to exchange heat with emitted hydrogen chloride gas. This invention, by setting up a slide plate 14, allows hydrogen chloride gas to directly contact and exchange heat with isocyanuric acid and organic solvents through the slide plate 14, or indirectly contact and exchange heat through the slide plate 14. Compared with the traditional unsealed reactor method of using heat exchangers to treat hydrogen chloride gas, this directly eliminates the purchase cost of heat exchangers, thereby reducing the overall preparation cost of triallyl isocyanurate (TAIC). At the same time, this design can effectively suppress the volatilization and escape of organic solvents, increase the subsequent solvent recovery, and further reduce material loss and environmental treatment pressure.

[0039] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A process for preparing triallyl isocyanurate from isocyanuric acid, characterized in that: Includes the following steps: S1: Using isocyanuric acid and allyl chloride as reactants, organic solvent as reaction medium, tetrabutylammonium bromide as catalyst, and composite alkali as acid-binding agent, isocyanuric acid, allyl chloride, organic solvent, acid-binding agent, and catalyst are added to a pressure-stabilized reactor in a mass ratio of 10:25:60:7:

1. The reaction temperature is controlled at 90-120℃, and the reaction time is 2-3 hours. S2: After the reaction is completed, the liquid product of the reaction is sent to a vacuum distillation kettle. The reaction temperature is 50-70℃. The gaseous product of the distillation is condensed by a condenser. The remaining liquid product is sent to centrifuge No. 1 for centrifugal separation. S3: The liquid separated by centrifugation in centrifuge No. 1 is transferred to centrifuge No. 2 and slowly cooled to 20-30℃. Then, centrifuge No. 2 is controlled to perform solid-liquid separation to obtain crude triallyl isocyanurate. S4: The mother liquor obtained from the separation by centrifuge No. 2 is transported to a vacuum distillation kettle, and the reaction temperature is controlled at 80-120℃ to achieve solvent recovery. The separated crude TAIC is washed 2-3 times with deionized water to finally obtain high-purity TAIC.

2. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 1, characterized in that: In step S1, isocyanuric acid, organic solvent, acid binder and catalyst are first added to the pressure-stabilized reactor. After the reaction temperature is controlled to rise to 90°C, allyl chloride is added dropwise to the pressure-stabilized reactor.

3. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 1, characterized in that: In step S1, the pressure inside the pressure-stabilized reactor is maintained at 0.25–0.3 MPa.

4. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 1, characterized in that: The pressure-stabilized reactor includes a reactor body (1); a heater (11) is embedded in the inner wall of the reactor body (1); a discharge port (12) is opened at the lower end of the reactor body (1); a reactor cover (2) is installed at the upper end of the reactor body (1); a feed inlet (21) and a liquid addition tank (22) are opened at the upper end of the reactor cover (2); an end cap (221) is threaded to the port of the liquid addition tank (22); an air inlet (222) is opened on the surface of the end cap (221); a rotating rod (13) is rotatably connected inside the reactor body (1); a blade plate (131) is fixedly connected to the lower end of the rotating rod (13); a cylindrical rod (23) is rotatably connected to the lower end of the reactor cover (2); a cylindrical groove (231) is opened at the lower end of the cylindrical rod (23), and the rotating rod (13) is slidably connected in the cylindrical groove (231); the upper end of the reactor cover (2) A drive motor (24) is fixedly installed at the end; the drive motor (24) is used to drive the rotating rod (13) to rotate; the rotating rod (13) has an air passage (132) inside; the lid (2) has an annular groove (25) inside that communicates with the liquid filling tank (22); the cylindrical rod (23) has a groove (232) on its surface that communicates with the annular groove (25); a spring hose (233) is installed in the cylindrical groove (231); one end of the spring hose (233) communicates with the air passage (132), and the other end communicates with the groove (232); the lower end face of the blade (131) has an air hole (133) that communicates with the air passage (132); a hydraulic pump (26) is installed at the upper end of the lid (2); the hydraulic pump (26) is connected to the cylindrical groove (231) through a pipe.

5. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 4, characterized in that: The vessel body (1) is internally connected to a sliding plate (14) with a sliding seal; the rotating rod (13) is in sliding seal contact with the sliding plate (14); a connecting rod (27) is provided between the rotating rod (13) and the cylindrical rod (23); the connecting rod (27) is slidably connected in the cylindrical groove (231); the lower end of the connecting rod (27) is provided with a circular groove (271) communicating with the spring hose (233); a sealing plug (272) is slidably sealed in the circular groove (271); the sealing plug (272) is connected to the bottom of the circular groove (271) by a sealing spring (273); a through groove (141) is provided on the surface of the sliding plate (14); a pressure sensor (142) is embedded in the lower end of the sliding plate (14); The upper end of the rotating rod (13) is provided with a slot (15) communicating with the air passage (132); a plug rod (151) is slidably connected in the slot (15); the plug rod (151) and the bottom of the slot (15) are connected by a support spring (152); an L-shaped groove (153) is provided on the surface of the plug rod (151); an arc-shaped groove (154) is provided at the upper end of the rotating rod (13); an L-shaped rod (274) is fixedly connected to the lower end of the connecting rod (27); A clamping unit is installed on the side wall of the slide plate (14); the slide plate (14) is connected to the inner wall of the vessel body (1) through the clamping unit.

6. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 5, characterized in that: The bottom of the arc-shaped groove (154) is provided with an installation groove (155); a blocking block (156) is slidably connected in the installation groove (155); the blocking block (156) is connected to the bottom of the installation groove (155) by a blocking spring (157).

7. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 6, characterized in that: The clamping unit includes a clamping block (143); the side wall of the slide plate (14) is provided with a clamping groove (144); the clamping block (143) is slidably and sealed in the clamping groove (144); the clamping block (143) and the bottom of the clamping groove (144) are connected by a clamping spring (145); the lower end of the slide plate (14) is provided with an oil groove (146) communicating with the clamping groove (144); an arc plate (147) is slidably and sealed in the oil groove (146).

8. The process for preparing triallyl isocyanurate from isocyanuric acid according to claim 7, characterized in that: A baffle (16) is provided inside the through groove (141); a ball rod (161) is fixedly connected to the lower end of the baffle (16); a round hole (162) is opened on the surface of the baffle (16); a one-way pressure regulating valve (163) is installed in the round hole (162).

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