A cyanate ester synthesis reaction device and method for adaptively adding organic solvent

Abstract

The invention discloses a cyanate synthesis reaction device and method for adaptively adding an organic solvent, belonging to the field of cyanate synthesis. The device comprises a reactor, wherein a lower cylinder is fixedly connected in the reactor, an upper cylinder is slidably connected in the lower cylinder, the outer wall of the upper cylinder is fitted with the inner wall of the lower cylinder, the lower cylinder has a conical bottom surface, the cone angle of the conical bottom surface opens toward the upper part of the lower cylinder, and a conical hole is opened in the middle of the conical bottom surface; a hydraulic rod is connected to the top of the reactor, the middle part of the hydraulic rod is hung on the upper cylinder, a cone plate is hung on the bottom end of the hydraulic rod, and a solvent adsorption block is placed on the cone plate; the device can separate part of the dichloromethane solvent in the initial stage of the reaction, thereby increasing the concentration of phenolic compounds in the remaining solvent and accelerating the reaction speed, and in the subsequent reaction, if the reaction is too intense, the previously separated dichloromethane can be re-injected into the reactor to maintain a suitable concentration of the reaction solution, thereby ensuring that the reaction is continuously and efficiently carried out.

Description

Technical Field

[0001] The invention relates to the technical field of cyanate synthesis, and in particular to a cyanate synthesis reaction device and method capable of adaptively adding an organic solvent. Background Art

[0002] In the synthesis process of cyanate esters, cyanogen chloride reacts with phenolic compounds in a dichloromethane solvent. Usually, when preparing the reaction solution, due to various factors, the phenolic compounds are not dissolved in the dichloromethane solvent in a saturated state. In the early stage of the reaction, when cyanogen chloride is slowly and uniformly added to the reactor through the cyanogen chloride supply pipe, the concentration of the phenolic compound does not reach the optimal reaction concentration, and the gap between the molecules is large, so that the effective collision frequency between the reactant molecules is relatively low, resulting in a slow reaction rate.

[0003] The traditional reaction device and method are difficult to effectively solve the problem of insufficient concentration of phenolic compounds in the initial stage of the reaction, and cannot quickly increase the reaction speed to achieve the purpose of efficiently synthesizing cyanate esters. Moreover, as the reaction proceeds, the consumption of reactants causes the concentration of the reaction system to gradually change. If the concentration of the reaction solution cannot be adjusted in time, the temperature in the reactor will rise, the reaction may be inhibited, and it cannot be carried out continuously and efficiently. Summary of the invention

[0004] The object of the present invention is to provide a cyanate synthesis reaction device and method for adaptively adding an organic solvent, which solves the problem that the concentration of phenolic compounds is low at the initial stage of the reaction, resulting in a slow reaction rate, and as the reaction proceeds, the concentration of reactants increases, causing the temperature in the reactor to rise.

[0005] To achieve the above object, the present invention provides the following technical solution: a cyanate ester synthesis reaction device with adaptive addition of organic solvent, comprising a reactor, a lower cylinder is fixedly connected in the reactor, an upper cylinder is slidably connected in the lower cylinder, the outer wall of the upper cylinder is in contact with the inner wall of the lower cylinder, the lower cylinder has a conical bottom surface, the cone angle of the conical bottom surface is open toward the upper part of the lower cylinder, and a conical hole is opened in the middle of the conical bottom surface;

[0006] The top of the reactor is connected with a hydraulic rod, the middle part of the hydraulic rod is hung on the upper cylinder, the bottom end of the hydraulic rod is hung with a cone plate, and a solvent adsorption block is placed on the cone plate;

[0007] When the hydraulic rod is extended, it can move downward on the upper cylinder, and the solvent adsorption block moves downward and is immersed in the reaction solution in the reactor to adsorb the organic solvent, thereby increasing the concentration of the reaction solution. In addition, when the hydraulic rod is shortened, the cone plate is clamped on the conical bottom surface, so that after the hydraulic rod continues to shorten, the hydraulic rod can move upward on the cone plate to form a negative pressure in the inner cavities of the upper cylinder and the lower cylinder.

[0008] Preferably, a conical column is connected to the middle part of the cylinder rod of the hydraulic rod, and a conical hole matching with the conical column is opened on the top wall of the upper cylinder. When the hydraulic rod is extended, the conical column moves away from the upper cylinder, and when the hydraulic rod is shortened, the conical column is inserted into the conical hole on the top wall of the upper cylinder, thereby driving the upper cylinder to move upward to the lower cylinder.

[0009] Preferably, the bottom end of the cylinder rod of the hydraulic rod is connected to a limit plate, and the cylinder rod is slidably connected with a sleeve located at the lower part of the cone column, the limit plate is located in the sleeve, the cone plate is connected to the bottom of the sleeve, the solvent adsorption block is sleeved on the sleeve, and a first spring is connected between the limit plate and the top wall of the sleeve. After the cone plate is clamped on the conical bottom surface, the hydraulic rod continues to shorten so that the limit plate moves up to the sleeve and compresses the first spring.

[0010] Preferably, the diameter of the cone column is smaller than that of the cone plate.

[0011] Preferably, a hose is connected between the top wall of the upper cylinder and the conical bottom surface of the lower cylinder, and the hose is connected to the upper part of the upper cylinder and the lower space of the lower cylinder in the reactor. When the upper cylinder moves up to the lower cylinder, the pressure in the space outside the inner cavities of the upper cylinder and the lower cylinder in the reactor increases.

[0012] Preferably, the lower part of the lower tube is connected to an L-shaped frame, the L-shaped frame is connected to a cylinder, the output end of the cylinder is connected to a ring, the upper surface of the ring is connected to a plug, and the conical bottom surface of the lower tube is provided with a plug hole that cooperates with the plug;

[0013] The inner wall of the reactor is provided with a time delay switch for controlling the shortening of the cylinder. When the hydraulic rod is shortened, the upper cylinder abuts against the time delay switch, so that the cylinder is shortened to discharge the solvent in the lower cylinder into the reaction solution.

[0014] Preferably, the lower space of the lower cylinder in the reactor is connected to a solvent supply pipe, the solvent supply pipe is connected to an external dichloromethane solvent supply, an external water pump is connected to the solvent supply pipe, and a pressure-sensitive switch for controlling the start of the external water pump is provided on the top of the reactor. When the hydraulic rod is shortened to the shortest state, the upper cylinder presses the pressure-sensitive switch to start the external water pump.

[0015] Preferably, the lower space of the lower cylinder in the reactor is connected to a cyanogen chloride supply pipe, and a solenoid valve is provided on the cyanogen chloride supply pipe. When the hydraulic rod is extended to allow the solvent adsorption block to be immersed in the reaction solution, the solenoid valve is closed.

[0016] Preferably, a motor is connected to the bottom of the reactor, a turntable is connected to the output end of the motor, the turntable rotates at the bottom of the reactor, a first stirring blade is connected to the upper surface of the turntable, a rotating plate is rotatably connected to the middle of the turntable, and a second stirring blade is connected to the rotating plate;

[0017] The cam is provided with a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the slide bar and a second spring which is arranged on a side wall of the second spring ... which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is arranged on a side wall of the second spring which is

[0018] A cyanate ester synthesis reaction method with adaptive addition of an organic solvent comprises the following steps:

[0019] Adding a dichloromethane reaction solution in which a phenolic compound is dissolved into the reactor, and then slowly and evenly adding cyanogen chloride into the reactor through a cyanogen chloride supply pipe;

[0020] The temperature sensor detects the temperature in the reactor. When the temperature is low, it means that the reaction speed is slow. At this time, the control system controls the hydraulic rod to extend so that the solvent adsorption block is immersed in the reaction solution, so that the dichloromethane solvent is adsorbed by the solvent adsorption block, thereby increasing the concentration of phenolic compounds in dichloromethane and reducing the gap between molecules, thereby increasing the reaction speed of phenolic compounds and cyanogen chloride;

[0021] Then the hydraulic rod is shortened, and after the cone plate is clamped on the bottom wall of the lower cylinder to seal the bottom of the lower cylinder, the hydraulic rod continues to shorten, so that the cone column is hung on the upper cylinder, so that the space between the upper cylinder and the lower cylinder is sealed, and then the hydraulic rod drives the upper cylinder to move upward, so that the space between the upper cylinder and the lower cylinder increases and negative pressure is generated. Under the action of negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block is desorbed into the lower cylinder;

[0022] The control system continues to obtain the temperature in the reactor detected by the temperature sensor. If the temperature in the reactor does not rise or rises slowly after the hydraulic rod is extended and shortened, the hydraulic rod continues to extend and retract, repeating the above solvent adsorption and desorption process until the temperature in the reactor rises.

[0023] After the temperature in the reactor rises, the hydraulic rod stops moving, and the temperature sensor continues to monitor the temperature in the reactor. When the temperature in the reactor continues to rise, the hydraulic rod continues to shorten in the current shortened state, so that the upper cylinder is separated from the lower cylinder, and the negative pressure environment between the two disappears. At the same time, the upper cylinder touches the delay switch, and the delay switch controls the cylinder to shorten immediately, so that the plug column pulls out the lower cylinder, so that the reverse stripping solvent is discharged into the reaction solution, so that the reaction solution is diluted, thereby slowing down the reaction speed;

[0024] When the hydraulic rod is shortened to the length where the upper cylinder is separated from the lower cylinder and the upper cylinder touches the delay switch, the temperature sensor continues to monitor the temperature in the reactor. If the reaction temperature does not drop, the hydraulic rod is shortened again and the top of the upper cylinder abuts against the pressure-sensitive switch, and then extends until the upper cylinder is just away from the pressure-sensitive switch, so that the external water pump runs and quantitatively replenishes the dichloromethane solvent into the reactor through the solvent supply pipe;

[0025] As the reaction continues, when it reaches the end, the temperature sensor detects that the temperature in the reactor is no longer rising. At this time, the hydraulic rod shortens again and presses the pressure-sensitive switch on the top of the upper cylinder, so that the solvent is supplied to the reactor again, so that the solution in the reactor is diluted again, increasing the chance of collision between the remaining cyanogen chloride and phenolic compounds that have not reacted completely, thereby promoting the completion of the reaction.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1. In the present invention, when synthesizing cyanate ester, a dichloromethane reaction solution in which phenolic compounds are dissolved is added into a reactor, and then cyanogen chloride is slowly and uniformly added into the reactor through a cyanogen chloride supply pipe. A temperature sensor is arranged in the reactor. After cyanogen chloride is injected into the reactor, as the reaction proceeds, if the temperature in the reactor does not increase significantly, it indicates that the reaction speed is slow. At this time, the control system controls the hydraulic rod to extend so that the solvent adsorption block is immersed in the reaction solution, so that the dichloromethane solvent is adsorbed by the solvent adsorption block, thereby increasing the concentration of phenolic compounds in dichloromethane and reducing the intermolecular The gap is increased, thereby increasing the reaction rate of the phenolic compound and cyanogen chloride. Subsequently, the hydraulic rod is shortened. After the cone plate is clamped on the bottom wall of the lower cylinder to seal the bottom of the lower cylinder, the hydraulic rod continues to shorten, so that the cone column is hung on the upper cylinder, so that the space between the upper cylinder and the lower cylinder is sealed. Subsequently, the hydraulic rod drives the upper cylinder to move upward, thereby increasing the space between the upper cylinder and the lower cylinder and generating negative pressure. Under the action of negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block is desorbed into the lower cylinder, so that a large amount of solvent and a small amount of phenolic compounds in the reaction solution are transferred to the lower cylinder, thereby increasing the concentration of the reaction solution and promoting the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the external structure of the present invention;

[0029] Figure 2 is a cross-sectional view of the present invention;

[0030] Figure 3 It is a structural schematic diagram of the state where the upper cylinder is close to the lower cylinder of the present invention;

[0031] Figure 4 It is a structural schematic diagram of the state in which the upper cylinder of the present invention is away from the lower cylinder;

[0032] Figure 5 It is a structural schematic diagram of the contact state between the first stirring blade and the second stirring blade of the present invention;

[0033] Figure 6 It is a structural schematic diagram of the first stirring blade and the second stirring blade of the present invention in a separated state;

[0034] Figure 7 It is a structural schematic diagram of the transfer plate of the present invention;

[0035] Figure 8 It is a structural schematic diagram of the vertical rod of the present invention.

[0036] In the figure: 100, reactor; 110, solvent supply pipe; 120, cyanogen chloride supply pipe; 121, solenoid valve; 122, pressure-sensitive switch; 200, lower cylinder; 210, upper cylinder; 220, cone plate; 230, sleeve; 240, solvent adsorption block; 250, hydraulic rod; 251, cone column; 252, limit plate; 253, first spring; 260, ring; 261, plug column; 262, cylinder; 263, L-shaped frame; 270, hose; 280, delay switch; 300, motor; 310, turntable; 320, first stirring blade; 330, turntable; 331, bump; 340, second stirring blade; 350, slide rod; 351, spiral groove; 360, vertical rod; 370, second spring. DETAILED DESCRIPTION

[0037] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] Reference Figure 1-Figure 8The present embodiment provides a technical solution: a cyanate synthesis reaction device with adaptive addition of organic solvent, comprising a reactor 100, a lower cylinder 200 is fixedly connected in the reactor 100, an upper cylinder 210 is slidably connected in the lower cylinder 200, the outer wall of the upper cylinder 210 is in contact with the inner wall of the lower cylinder 200, the lower cylinder 200 has a conical bottom surface, the conical angle of the conical bottom surface is open toward the upper part of the lower cylinder 200, and a conical hole is opened in the middle of the conical bottom surface; a hydraulic rod 250 is connected to the top of the reactor 100, and the middle part of the hydraulic rod 250 is hung on the upper cylinder 210. 0, a cone plate 220 is hung at the bottom end of the hydraulic rod 250, and a solvent adsorption block 240 is placed on the cone plate 220; when the hydraulic rod 250 is extended, it can move down to the upper cylinder 210, and the solvent adsorption block 240 moves down and is immersed in the reaction solution in the reactor 100 to adsorb the organic solvent, thereby increasing the concentration of the reaction solution; and, when the hydraulic rod 250 is shortened, the cone plate 220 is clamped on the conical bottom surface, so that after the hydraulic rod 250 continues to shorten, the hydraulic rod 250 can move up to the cone plate 220, so that a negative pressure is formed in the inner cavity of the upper cylinder 210 and the lower cylinder 200.

[0039] During the synthesis of cyanate ester, a dichloromethane reaction solution in which phenolic compounds are dissolved is added to the reactor 100, and then cyanogen chloride is slowly and evenly added to the reactor 100 through the cyanogen chloride supply pipe 120. A temperature sensor is provided in the reactor 100. After cyanogen chloride is injected into the reactor 100, as the reaction proceeds, if the temperature in the reactor 100 does not increase significantly, it means that the reaction speed is slow. At this time, the control system controls the hydraulic rod 250 to extend so that the solvent adsorption block 240 is immersed in the reaction solution, so that the dichloromethane solvent is adsorbed by the solvent adsorption block 240, thereby increasing the concentration of phenolic compounds in dichloromethane, reducing the gap between molecules, and thus increasing the temperature of the phenolic compounds and the solvent adsorption block 240. The reaction speed of cyanogen chloride is increased, and then the hydraulic rod 250 is shortened. After the cone plate 220 is clamped on the bottom wall of the lower cylinder 200 to seal the bottom of the lower cylinder 200, the hydraulic rod 250 continues to shorten, so that the cone column 251 is hung on the upper cylinder 210, so that the space between the upper cylinder 210 and the lower cylinder 200 is sealed. Then the hydraulic rod 250 drives the upper cylinder 210 to move upward, so that the space between the upper cylinder 210 and the lower cylinder 200 increases and generates negative pressure. Under the action of negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block 240 is desorbed into the lower cylinder 200, so that a large amount of solvent and a small amount of phenolic compounds in the reaction solution are transferred to the lower cylinder 200, thereby increasing the concentration of the reaction solution and promoting the reaction.

[0040] In this embodiment, the solvent adsorption block 240 can be activated carbon. The adsorption of dichloromethane by activated carbon is mainly based on physical adsorption, relying on van der Waals force. The dichloromethane molecule is relatively small and can easily enter the microporous structure rich in activated carbon. The chlorine atom in its molecular structure makes the molecule have a certain polarity, which also helps to interact with the surface of activated carbon, thereby ensuring that the properties of the solvent are not easily destroyed. In addition, in the reaction system, phenolic compounds are one of the main reactants, and their concentration will gradually decrease as the reaction proceeds. Moreover, their reaction activity with cyanogen chloride is relatively high, so that the adsorption of activated carbon is also faced with competition. Compared with the solvent dichloromethane, the degree of adsorption of phenolic compounds by activated carbon during the reaction is relatively low. Moreover, cyanate esters are not easily adsorbed by activated carbon during the reaction, unless the activated carbon is specially treated to make it have a strong affinity for cyanate esters. Therefore, activated carbon is used as the adsorption material for adsorbing dichloromethane solvent, and under negative pressure, activated carbon can also achieve reverse stripping;

[0041] In addition, resin, MOF material or molecular sieve can be used instead of activated carbon according to needs. If the aforementioned materials are used, they need to be customized according to the reaction system so that they have strong adsorption capacity for the reaction solvent and poor adsorption capacity for other reactants.

[0042] A conical column 251 is connected to the middle part of the cylinder rod of the hydraulic rod 250, and a conical hole matching with the conical column 251 is opened on the top wall of the upper cylinder 210. When the hydraulic rod 250 is extended, the conical column 251 moves away from the upper cylinder 210, and when the hydraulic rod 250 is shortened, the conical column 251 is inserted into the conical hole on the top wall of the upper cylinder 210, thereby driving the upper cylinder 210 to move up to the lower cylinder 200.

[0043] The conical column 251 is located below the top wall of the upper cylinder 210, so that when the hydraulic rod 250 is extended, the conical column 251 can move away from the upper cylinder 210, so that the upper cylinder 210 is not affected at this time, ensuring that the downward movement of the solvent adsorption block 240 is not interfered with. When the conical plate 220 is clamped on the bottom wall of the lower cylinder 200 to seal the bottom of the lower cylinder 200, the conical column 251 is completely inserted into the conical hole of the upper cylinder 210 at the same time, so that the top wall of the upper cylinder 210 is also sealed, so that the continued shortening of the hydraulic rod 250 can drive the upper cylinder 210 to move upward relative to the lower cylinder 200.

[0044] The bottom end of the cylinder rod of the hydraulic rod 250 is connected to a limit plate 252, and a sleeve 230 is slidably connected to the lower part of the cone column 251 on the cylinder rod. The limit plate 252 is located in the sleeve 230, and the cone plate 220 is connected to the bottom of the sleeve 230. The solvent adsorption block 240 is sleeved on the sleeve 230. A first spring 253 is connected between the limit plate 252 and the top wall of the sleeve 230. After the cone plate 220 is clamped on the conical bottom surface, the hydraulic rod 250 continues to shorten so that the limit plate 252 moves up to the sleeve 230 and compresses the first spring 253.

[0045] When the cone column 251 and the cone plate 220 respectively block the upper cylinder 210 and the lower cylinder 200, the first spring 253 is not in a compressed state at this time, and then the hydraulic rod 250 continues to shorten. At this time, the limit plate 252 can move upward relative to the sleeve 230. At this time, the first spring 253 is compressed. The setting of the first spring 253 enables the hydraulic rod 250 to continue to shorten after the cone plate 220 blocks the lower cylinder 200.

[0046] The diameter of the cone column 251 is smaller than that of the cone plate 220 .

[0047] Since the diameter of the conical column 251 is smaller than that of the conical plate 220 , when the hydraulic rod 250 is extended, the conical column 251 can pass through the bottom wall of the lower cylinder 200 , thereby ensuring that the downward movement of the solvent adsorption block 240 is not blocked.

[0048] A hose 270 is connected between the top wall of the upper cylinder 210 and the conical bottom surface of the lower cylinder 200. The hose 270 is connected to the upper part of the upper cylinder 210 and the lower space of the lower cylinder 200 in the reactor 100. When the upper cylinder 210 moves up to the lower cylinder 200, the pressure in the space outside the inner cavity of the upper cylinder 210 and the lower cylinder 200 in the reactor 100 increases.

[0049] The upper cylinder 210 moves upward relative to the lower cylinder 200 to allow the solvent adsorption block 240 to reversely desorb. At the same time, the upward movement of the upper cylinder 210 also compresses the internal space of the reactor 100, thereby increasing the internal pressure of the reactor 100. The provision of the hose 270 enables the pressure distribution in the space inside the reactor 100 to be uniform, that is, the pressure in the lower space of the lower cylinder 200 is also increased. By increasing the pressure in the reactor 100 and reducing the amount of solvent, the reaction is further promoted.

[0050] In addition, when the upper cylinder 210 moves upward relative to the lower cylinder 200 and the two are not separated from each other, the shortening distance of the hydraulic rod 250 will not exceed a fixed limit. When the control system detects that the hydraulic rod 250 is shortened within this limit, it will control the pressure relief system of the reactor 100 to close, thereby ensuring that high pressure can be generated in the reactor 100 without being released by the pressure relief system.

[0051] The lower part of the lower cylinder 200 is connected to an L-shaped frame 263, and the L-shaped frame 263 is connected to a cylinder 262. The output end of the cylinder 262 is connected to a ring 260, and the upper surface of the ring 260 is connected to a plug post 261. The conical bottom surface of the lower cylinder 200 is provided with a socket that cooperates with the plug post 261; the inner wall of the reactor 100 is provided with a delay switch 280 for controlling the shortening of the cylinder 262. When the hydraulic rod 250 is shortened, the upper cylinder 210 abuts against the delay switch 280, so that the cylinder 262 is shortened to discharge the solvent in the lower cylinder 200 into the reaction solution.

[0052] After the temperature in the reactor 100 rises, the hydraulic rod 250 stops moving, and the temperature sensor continues to monitor the temperature in the reactor 100. When the temperature in the reactor 100 continues to rise, the hydraulic rod 250 continues to shorten in the current shortened state, so that the upper cylinder 210 is separated from the lower cylinder 200, and the negative pressure environment between the two disappears, so that the pull-out resistance of the plug 261 is reduced. At the same time, the upper cylinder 210 touches the delay switch 280, and the delay switch 280 controls the cylinder 262 to shorten immediately, so that the plug 261 pulls out the lower cylinder 200, so that the reverse-peeled solvent is discharged into the reaction solution, so that the reaction solution is diluted, thereby slowing down the reaction speed. At the same time, the phenolic compounds that may be adsorbed by the solvent adsorption block 240 are also discharged back into the reaction solution to continue to participate in the reaction;

[0053] When the upper cylinder 210 moves upward again at the current position, the side wall of the upper cylinder 210 continues to squeeze the delay switch 280 to ensure that the cylinder 262 maintains a shortened state. After the reaction is completed, the control system controls the hydraulic rod 250 to extend at a uniform speed, so that the upper cylinder 210 slides into the lower cylinder 200 again, and when the distance between the two is at the minimum, the delay switch 280 will control the cylinder 262 to extend, so that the plug 261 is inserted into the bottom of the lower cylinder 200, thereby ensuring that when the upper cylinder 210 is reset, the space between the upper cylinder 210 and the lower cylinder 200 will not generate positive pressure.

[0054] The lower space of the lower cylinder 200 in the reactor 100 is connected to a solvent supply pipe 110, which is connected to an external dichloromethane solvent supply. An external water pump is connected to the solvent supply pipe 110. A pressure-sensitive switch 122 for controlling the start of the external water pump is provided on the top of the reactor 100. When the hydraulic rod 250 is shortened to the shortest state, the upper cylinder 210 presses the pressure-sensitive switch 122 to start the external water pump.

[0055] After the hydraulic rod 250 is shortened to separate the upper cylinder 210 and the lower cylinder 200, the temperature sensor continues to monitor the temperature in the reactor 100. If the reaction temperature does not drop, the hydraulic rod 250 is shortened again to make the top of the upper cylinder 210 abut against the pressure-sensitive switch 122, and then extends until the upper cylinder 210 is just away from the pressure-sensitive switch 122, so that the external water pump runs and quantitatively replenishes the dichloromethane solvent into the reactor 100 through the solvent supply pipe 110. The amount of dichloromethane solvent replenished is adaptively adjusted according to the total volume of the reactants. It should be noted here that the rotation time of the external water pump is controlled by the control system, so that the replenishment amount of the dichloromethane solvent is controlled, and the operation timing of the external water pump starts when the control system detects that the pressure-sensitive switch 122 is pressurized.

[0056] The lower space of the lower cylinder 200 in the reactor 100 is connected to a cyanogen chloride supply pipe 120, on which a solenoid valve 121 is provided. When the hydraulic rod 250 is extended to allow the solvent adsorption block 240 to be immersed in the reaction solution, the solenoid valve 121 is closed.

[0057] In order to prevent cyanogen chloride from being adsorbed by the solvent adsorption block 240, the control system controls the solenoid valve 121 to be closed when the hydraulic rod 250 is extended, and the supply of cyanogen chloride is interrupted.

[0058] The bottom of the reactor 100 is connected to a motor 300, and the output end of the motor 300 is connected to a turntable 310, which rotates at the bottom of the reactor 100. The upper surface of the turntable 310 is connected to a first stirring blade 320, and the middle of the turntable 310 is rotatably connected to a rotating plate 330, and the rotating plate 330 is connected to a second stirring blade 340; the middle of the turntable 310 is connected to a vertical rod 360, and a sliding rod 350 is slidably connected to the vertical rod 360. A second spring 370 is connected between the sliding rod 350 and the vertical rod 360, and a spiral spring 370 is provided on the side wall of the sliding rod 350. The rotating plate 330 is provided with a through hole matched with the slide bar 350 in the middle part, and a protrusion 331 is provided on the inner wall of the through hole. The protrusion 331 slides in the spiral groove 351. When the cone plate 220 moves downward, it can press the slide bar 350 to move downward, so that the protrusion 331 slides in the spiral groove 351, so that the rotating plate 330 rotates, so that the second stirring blade 340 moves away from the first stirring blade 320, and when the cone plate 220 moves upward, it moves away from the slide bar 350, so that the second spring 370 elastically recovers and drives the second stirring blade 340 to fit the first stirring blade 320.

[0059] When the motor 300 is started, it can drive the turntable 310 to rotate synchronously, so that the first stirring blade 320 and the second stirring blade 340 both rotate to stir the reaction solution and promote the reaction. When the hydraulic rod 250 is extended, the cone plate 220 presses the slide bar 350, so that the slide bar 350 drives the rotating plate 330 to rotate through the cooperation of the spiral groove 351 and the protrusion 331, so that the second stirring blade 340 is away from the first stirring blade 320, so that the number of stirring blades involved in stirring is increased, thereby enhancing the stirring effect on the reaction solution. At this time, cyanogen chloride is not added to the reactor 100, thereby avoiding the possibility of excessively intense reaction. In the state of enhanced stirring of the reaction solution, the collision efficiency of dichloromethane and the solvent adsorption block 240 is improved, thereby accelerating the speed of adsorbing dichloromethane by the solvent adsorption block 240;

[0060] After the hydraulic rod 250 is shortened, the second spring 370 elastically recovers and drives the second stirring blade 340 to fit the first stirring blade 320. At this time, the number of stirring blades involved in stirring is reduced, so that the stirring speed of the reaction solution is restored, ensuring that when cyanogen chloride is added later, the reaction may not be too violent due to excessive stirring.

[0061] A cyanate ester synthesis reaction method with adaptive addition of an organic solvent comprises the following steps:

[0062] Add a dichloromethane reaction solution containing dissolved phenolic compounds into the reactor 100, and then slowly and evenly add cyanogen chloride into the reactor 100 through the cyanogen chloride supply pipe 120;

[0063] The temperature sensor detects the temperature in the reactor 100. When the temperature is low, it means that the reaction speed is slow. At this time, the control system controls the hydraulic rod 250 to extend so that the solvent adsorption block 240 is immersed in the reaction solution, so that the dichloromethane solvent is adsorbed by the solvent adsorption block 240, thereby increasing the concentration of phenolic compounds in dichloromethane and reducing the gap between molecules, thereby increasing the reaction speed of phenolic compounds and cyanogen chloride;

[0064] Then the hydraulic rod 250 is shortened, and after the cone plate 220 is clamped on the bottom wall of the lower cylinder 200 to seal the bottom of the lower cylinder 200, the hydraulic rod 250 continues to shorten, so that the cone column 251 is hung on the upper cylinder 210, so that the space between the upper cylinder 210 and the lower cylinder 200 is sealed, and then the hydraulic rod 250 drives the upper cylinder 210 to move upward, so that the space between the upper cylinder 210 and the lower cylinder 200 increases and generates negative pressure, and under the action of the negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block 240 is desorbed into the lower cylinder 200;

[0065] The control system continues to obtain the temperature in the reactor 100 detected by the temperature sensor. If the temperature in the reactor 100 does not rise or rises slowly after the hydraulic rod 250 is extended and shortened, the hydraulic rod 250 continues to extend and retract, and the above-mentioned solvent adsorption and desorption process is repeated until the temperature in the reactor 100 rises.

[0066] After the temperature in the reactor 100 rises, the hydraulic rod 250 stops moving, and the temperature sensor continues to monitor the temperature in the reactor 100. When the temperature in the reactor 100 continues to rise, the hydraulic rod 250 continues to shorten in the current shortened state, so that the upper cylinder 210 is separated from the lower cylinder 200, and the negative pressure environment between the two disappears. At the same time, the upper cylinder 210 touches the delay switch 280, and the delay switch 280 controls the cylinder 262 to shorten immediately, so that the plug 261 pulls out the lower cylinder 200, so that the reverse stripping solvent is discharged into the reaction solution, so that the reaction solution is diluted, thereby slowing down the reaction speed;

[0067] When the hydraulic rod 250 is shortened to the length where the upper cylinder 210 is separated from the lower cylinder 200 and the upper cylinder 210 touches the delay switch 280, the temperature sensor continues to monitor the temperature in the reactor 100. If the reaction temperature does not drop, the hydraulic rod 250 is shortened again and the top of the upper cylinder 210 abuts against the pressure-sensitive switch 122, and then extends until the upper cylinder 210 is just away from the pressure-sensitive switch 122, so that the external water pump runs and quantitatively replenishes the dichloromethane solvent into the reactor 100 through the solvent supply pipe 110.

[0068] As the reaction proceeds, when the reaction reaches the end, the temperature sensor detects that the temperature in the reactor 100 no longer rises. At this time, the hydraulic rod 250 shortens again and causes the top of the upper cylinder 210 to press the pressure-sensitive switch 122, so that the solvent is supplied to the reactor 100 again, so that the solution in the reactor 100 is diluted again, increasing the chance of collision between the remaining cyanogen chloride and phenolic compounds that have not reacted completely, thereby promoting the completion of the reaction.

[0069] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A cyanate ester synthesis reaction device with adaptive addition of organic solvent, comprising a reaction kettle (100), characterized in that: A lower cylinder (200) is fixedly connected inside the reaction kettle (100), an upper cylinder (210) is slidably connected inside the lower cylinder (200), an outer wall of the upper cylinder (210) is in contact with an inner wall of the lower cylinder (200), the lower cylinder (200) has a conical bottom surface, the conical angle of the conical bottom surface is open toward the upper part of the lower cylinder (200), and a conical hole is opened in the middle of the conical bottom surface; The top of the reaction kettle (100) is connected to a hydraulic rod (250), the middle of the hydraulic rod (250) is hung on the upper cylinder (210), the bottom of the hydraulic rod (250) is hung with a cone plate (220), a solvent adsorption block (240) is placed on the cone plate (220), the middle of the cylinder rod of the hydraulic rod (250) is connected to a cone column (251), and the top wall of the upper cylinder (210) is provided with a cone hole that matches the cone column (251); When the hydraulic rod (250) is extended, it can move downward on the upper cylinder (210), the cone column (251) is away from the upper cylinder (210), the solvent adsorption block (240) moves downward and is immersed in the reaction solution in the reactor (100) to adsorb the dichloromethane solvent, thereby increasing the concentration of the reaction solution; and, when the hydraulic rod (250) is shortened, the cone plate (220) is clamped on the conical bottom surface, so that after the hydraulic rod (250) continues to shorten, the hydraulic rod (250) can move upward on the cone plate (220), and the cone column ( The hydraulic rod (251) is inserted into the conical hole on the top wall of the upper cylinder (210), so that the space between the upper cylinder (210) and the lower cylinder (200) is sealed. Then, the hydraulic rod (250) drives the upper cylinder (210) to move upward, so that the space between the upper cylinder (210) and the lower cylinder (200) increases and generates negative pressure. Under the action of the negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block (240) is desorbed into the lower cylinder (200), so that a large amount of solvent and a small amount of phenolic compounds in the reaction solution are transferred to the lower cylinder (200).

2. The cyanate synthesis reaction device with adaptive addition of organic solvent according to claim 1, characterized in that: The bottom end of the cylinder rod of the hydraulic rod (250) is connected to a limit plate (252); a sleeve (230) is slidably connected to the cylinder rod at the bottom of the cone column (251); the limit plate (252) is located in the sleeve (230); the cone plate (220) is connected to the bottom of the sleeve (230); the solvent adsorption block (240) is sleeved on the sleeve (230); a first spring (253) is connected between the limit plate (252) and the top wall of the sleeve (230); after the cone plate (220) is clamped on the conical bottom surface, the hydraulic rod (250) continues to shorten so that the limit plate (252) moves up to the sleeve (230) and compresses the first spring (253).

3. The cyanate synthesis reaction device with adaptive addition of organic solvent according to claim 2, characterized in that: The diameter of the cone column (251) is smaller than that of the cone plate (220).

4. The cyanate synthesis reaction device with adaptive addition of organic solvent according to claim 3, characterized in that: A hose (270) is connected between the top wall of the upper cylinder (210) and the conical bottom surface of the lower cylinder (200); the hose (270) is connected to the upper portion of the upper cylinder (210) and the lower portion of the lower cylinder (200) in the reactor (100); when the upper cylinder (210) moves upward on the lower cylinder (200), the pressure in the space outside the inner cavities of the upper cylinder (210) and the lower cylinder (200) in the reactor (100) increases.

5. The cyanate ester synthesis reaction device with adaptive addition of organic solvent according to claim 4, characterized in that: The lower part of the lower cylinder (200) is connected to an L-shaped frame (263), the L-shaped frame (263) is connected to a cylinder (262), the output end of the cylinder (262) is connected to a ring (260), the upper surface of the ring (260) is connected to an insertion column (261), and the conical bottom surface of the lower cylinder (200) is provided with an insertion hole that matches the insertion column (261); The inner wall of the reaction kettle (100) is provided with a delay switch (280) for controlling the shortening of the cylinder (262); when the hydraulic rod (250) shortens, the upper cylinder (210) abuts against the delay switch (280), so that the cylinder (262) shortens to allow the solvent in the lower cylinder (200) to be discharged into the reaction solution.

6. The cyanate ester synthesis reaction device with adaptive addition of organic solvent according to claim 5, characterized in that: The lower space of the lower cylinder (200) in the reaction kettle (100) is connected to a solvent supply pipe (110), the solvent supply pipe (110) is connected to an external dichloromethane solvent supply location, an external water pump is connected to the solvent supply pipe (110), a pressure-sensitive switch (122) for controlling the start of the external water pump is arranged on the top of the reaction kettle (100), and when the hydraulic rod (250) is shortened to the shortest state, the upper cylinder (210) presses the pressure-sensitive switch (122) to start the external water pump.

7. The cyanate synthesis reaction device with adaptive addition of organic solvent according to claim 6, characterized in that: The lower space of the lower cylinder (200) in the reaction kettle (100) is connected to a cyanogen chloride supply pipe (120), and a solenoid valve (121) is provided on the cyanogen chloride supply pipe (120). When the hydraulic rod (250) is extended so that the solvent adsorption block (240) is immersed in the reaction solution, the solenoid valve (121) is closed.

8. The cyanate ester synthesis reaction device with adaptive addition of organic solvent according to claim 7, characterized in that: The bottom of the reaction kettle (100) is connected to a motor (300), the output end of the motor (300) is connected to a rotating disk (310), the rotating disk (310) rotates at the bottom of the reaction kettle (100), the upper surface of the rotating disk (310) is connected to a first stirring blade (320), the middle of the rotating disk (310) is rotatably connected to a rotating plate (330), and the rotating plate (330) is connected to a second stirring blade (340); The middle of the rotating disk (310) is connected to a vertical rod (360), and a sliding rod (350) is slidably connected to the vertical rod (360). A second spring (370) is connected between the sliding rod (350) and the vertical rod (360). A spiral groove (351) is provided on the side wall of the sliding rod (350). The middle of the rotating plate (330) is provided with an insertion hole that matches the sliding rod (350), and a protrusion (331) is provided on the inner wall of the insertion hole. The protrusion (331) slides on the spiral groove (351). 1), when the cone plate (220) moves downward, it can press the slide bar (350) to move downward, so that the protrusion (331) slides in the spiral groove (351), so that the rotating plate (330) rotates, so that the second stirring blade (340) moves away from the first stirring blade (320), and when the cone plate (220) moves upward, it moves away from the slide bar (350), so that the second spring (370) elastically recovers and drives the second stirring blade (340) to fit the first stirring blade (320).

9. A method for cyanate synthesis reaction by adaptively adding an organic solvent, applied to the cyanate synthesis reaction device by adaptively adding an organic solvent according to claim 8, characterized in that: The following steps are involved: Adding a dichloromethane reaction solution in which a phenolic compound is dissolved into the reaction kettle (100), and then slowly and evenly adding cyanogen chloride into the reaction kettle (100) through a cyanogen chloride supply pipe (120); The temperature sensor detects the temperature in the reaction kettle (100). When the temperature is low, it indicates that the reaction speed is slow. At this time, the control system controls the hydraulic rod (250) to extend so that the solvent adsorption block (240) is immersed in the reaction solution, so that the dichloromethane solvent is adsorbed by the solvent adsorption block (240), thereby increasing the concentration of the phenolic compound in the dichloromethane and reducing the gap between molecules, thereby increasing the reaction speed of the phenolic compound and cyanogen chloride; Then, the hydraulic rod (250) is shortened, and after the cone plate (220) is clamped on the bottom wall of the lower cylinder (200) so that the bottom of the lower cylinder (200) is sealed, the hydraulic rod (250) continues to shorten so that the cone column (251) is hung on the upper cylinder (210), so that the space between the upper cylinder (210) and the lower cylinder (200) is sealed, and then the hydraulic rod (250) drives the upper cylinder (210) to move upward, so that the space between the upper cylinder (210) and the lower cylinder (200) increases and generates negative pressure, and under the action of the negative pressure, the dichloromethane solvent adsorbed by the solvent adsorption block (240) is desorbed into the lower cylinder (200); The control system continues to obtain the temperature in the reactor (100) detected by the temperature sensor. If the temperature in the reactor (100) does not rise or rises slowly after the hydraulic rod (250) is extended and shortened, the hydraulic rod (250) continues to extend and shorten, and the solvent adsorption and desorption processes are repeated until the temperature in the reactor (100) rises. After the temperature in the reactor (100) rises, the hydraulic rod (250) stops moving, and the temperature sensor continues to monitor the temperature in the reactor (100). When the temperature in the reactor (100) continues to rise, the hydraulic rod (250) continues to shorten in the current shortened state, so that the upper cylinder (210) is separated from the lower cylinder (200), and the negative pressure environment between the two disappears. At the same time, the upper cylinder (210) touches the delay switch (280), and the delay switch (280) controls the cylinder (262) to shorten immediately, so that the plug (261) pulls out the lower cylinder (200), so that the desorbed solvent is discharged into the reaction solution, so that the reaction solution is diluted, thereby slowing down the reaction speed; When the hydraulic rod (250) is shortened to a length where the upper cylinder (210) is separated from the lower cylinder (200) and the upper cylinder (210) touches the delay switch (280), the temperature sensor continues to monitor the temperature in the reaction kettle (100). If the reaction temperature does not drop, the hydraulic rod (250) is shortened again and the top of the upper cylinder (210) is brought into contact with the pressure-sensitive switch (122). The hydraulic rod (250) is then extended to a length where the upper cylinder (210) is just away from the pressure-sensitive switch (122), so that the external water pump is operated and the dichloromethane solvent is quantitatively added to the reaction kettle (100) through the solvent supply pipe (110); As the reaction proceeds, when the reaction reaches the end, the temperature sensor detects that the temperature in the reactor (100) no longer rises. At this time, the hydraulic rod (250) is shortened again and the top of the upper cylinder (210) presses the pressure-sensitive switch (122), so that the solvent is supplied to the reactor (100) again, so that the solution in the reactor (100) is diluted again, so that the collision chance of the remaining cyanogen chloride and phenolic compounds that have not reacted completely increases, thereby promoting the completion of the reaction.

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