A distillation separation mechanism and method for a cyanate synthesis reaction device

Abstract

The invention discloses a distillation separation mechanism and method for a cyanate synthesis reaction device, belonging to the field of cyanate synthesis. The mechanism comprises a distillation assembly, a distillation cylinder of the distillation assembly is connected to a reaction kettle, and further comprises a first collecting assembly for collecting cyanogen chloride and hydrogen chloride, a second collecting assembly for collecting bisphenol compounds, and a third collecting assembly for collecting cyanate. The distillation assembly sequentially connects the three. In the second collecting assembly, a second condensing tube is connected between the second collecting cylinder and the distillation cylinder, the second condensing tube is sleeved on the tube, a slide plate in the second collecting cylinder is connected to a piston rod and an insert rod, a tension spring is arranged between the piston rod and the piston cylinder, when the product in the distillation cylinder boils violently, the water flow rate of the second water inlet pipe increases, the water inlet pressure is large, the pressure moves down the piston rod and the slide plate through a branch pipe, the volume of the connected space decreases, the boiling slows down, the insert rod moves down to raise the second collecting cylinder, the condensing tube tilts, and the liquid drops reflux, thereby ensuring the amount of cyanate collected.

Description

Technical Field

[0001] The invention relates to the technical field of cyanate synthesis, and in particular to a distillation separation mechanism and method for a cyanate synthesis reaction device. Background Art

[0002] In the field of cyanate synthesis and subsequent product separation, obtaining high-purity cyanate esters efficiently and accurately has always been a key goal. Cyanate esters are usually generated by the reaction of bisphenol compounds and cyanogen chloride. However, after the reaction, the reaction mixture contains unreacted reactants such as cyanogen chloride, bisphenol compounds, and cyanate esters generated by the reaction, as well as impurities such as by-product hydrogen chloride. How to effectively separate these components has become an urgent problem to be solved.

[0003] The traditional distillation separation method exposes many drawbacks when dealing with the separation of bisphenol compounds and cyanate esters. On the one hand, as a commonly used heating method, the oil bath has the advantage of uniform heating, but its temperature control has obvious lag, and the heating and cooling processes are relatively slow. In the separation stage of bisphenol compounds, when the mixture in the distillation cylinder is heated to near the boiling point of the bisphenol compounds, it is vaporized and enters the condensation collection process. Once the product in the distillation cylinder boils violently, it is difficult for the oil bath to respond quickly to lower the temperature. This will not only cause excessive vaporization of the bisphenol compounds, affecting their collection efficiency, but also excessive boiling may cause sharp fluctuations in pressure in the system, destroying the established negative pressure distillation environment, and thus interfering with the subsequent separation accuracy of cyanate esters.

[0004] On the other hand, in the process of condensing and collecting bisphenol compounds, conventional devices simply rely on the cooperation of condensing tubes and condensing cylinders, and cannot dynamically adapt to the unstable conditions in the distillation process. When violent boiling occurs in the distillation cylinder and a large amount of steam flows into the condensing tube, it is difficult to ensure that the steam condenses quickly and fully by relying solely on fixed condensation conditions. In addition, due to the certain difference in boiling points between bisphenol compounds and cyanate esters, if the problems caused by violent boiling cannot be dealt with in time, high-boiling-point cyanate esters are easily entrained in the fraction of low-boiling-point bisphenol compounds, resulting in the loss of cyanate esters, which ultimately affects the yield and purity of cyanate esters and cannot meet the demand for high-purity cyanate esters in industrial production or scientific research. Summary of the invention

[0005] The object of the present invention is to provide a distillation separation mechanism and method for a cyanate synthesis reaction device, which solves the problem of poor separation effect of bisphenol compounds in the process of oil bath heating distillation separation of cyanate in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solution: a distillation separation mechanism of a cyanate synthesis reaction device, comprising a distillation assembly, wherein the distillation assembly comprises a distillation cylinder, wherein the distillation cylinder is connected to a reaction kettle, and further comprises a first collecting assembly for collecting cyanogen chloride and hydrogen chloride, a second collecting assembly for collecting bisphenol compounds, and a third collecting assembly for collecting cyanate, wherein the distillation assembly is sequentially connected to the first collecting assembly, the second collecting assembly, and the third collecting assembly;

[0007] The second collecting assembly comprises a second collecting cylinder, a second condensing tube is connected between the second collecting cylinder and the distilling cylinder, a second condensing cylinder is sleeved on the second condensing tube, a slide plate is slidably connected in the second collecting cylinder, a piston rod is connected to the slide plate, a piston cylinder is connected to the second collecting cylinder, the piston rod is slidably connected in the piston cylinder, a tension spring is connected between the piston rod and the piston cylinder, an insertion rod is connected to the lower surface of the slide plate, and the insertion rod passes through the bottom wall of the second collecting cylinder;

[0008] The second condensing cylinder is connected to a second water inlet pipe and a second drain pipe, and the second water inlet pipe is provided with a branch pipe connected to the piston cylinder. After the product in the distillation cylinder is separated into cyanogen chloride and hydrogen chloride, the distillation cylinder is connected to the second collecting cylinder. When the product in the distillation cylinder boils violently, the water inlet pressure of the second water inlet pipe increases to quickly condense the steam in the second condensing tube, and the slide moves down to the second collecting tube to reduce the negative pressure intensity in the distillation tube. At the same time, the insertion rod lifts the second collecting tube to make the second collecting tube rise, so that the condensed liquid in the second condensing tube flows back into the distillation tube.

[0009] Preferably, the second collecting assembly also includes a first hemispherical shell, a second hemispherical shell and a connecting pipe, the first hemispherical shell is connected to one end of the second condenser away from the second collecting cylinder, the second hemispherical shell is connected to the connecting pipe, the connecting pipe is connected to the distillation cylinder, and the first hemispherical shell is hinged in the second hemispherical shell.

[0010] Preferably, an outer cylinder is connected to the bottom wall of the second collecting cylinder, the insertion rod slides in the outer cylinder, a cavity is opened at the bottom of the insertion rod, and a reset rod is slidably connected in the cavity, a ring is connected to the upper part of the reset rod in the cavity, and the cavity is filled with a liquid medium. After the insertion rod slides toward the outside of the second collecting cylinder, the second collecting cylinder applies pressure on the reset rod, so that the liquid medium in the cavity located at the lower part of the ring slowly flows to the upper part of the ring, so that the height of the second collecting cylinder drops to its original position.

[0011] Preferably, the distillation component also includes a transmission pipe connected to the reaction kettle and the distillation cylinder, and a valve is provided on the transmission pipe. The first collecting component, the second collecting component and the third collecting component are commonly connected with a pressure pipe, and the pressure pipe is connected to an external pressure pump. When the valve is closed and the external pressure pump is turned on, the pressure pipe applies negative pressure to the first collecting component, the second collecting component and the third collecting component.

[0012] Preferably, the first collecting assembly and the third collecting assembly respectively include a first collecting cylinder and a third collecting cylinder, the first collecting cylinder and the third collecting cylinder are both connected to a first condenser, the two first condensers are both connected to the distillation cylinder, the two first condensers are both sleeved with a first condenser cylinder, the two first condensers are both connected to a first water inlet pipe and a first drain pipe, and the two first water inlet pipes and the second water inlet pipe are connected to the same external water pump.

[0013] Preferably, a switching mechanism is also included, which includes three ball valves arranged on the two first condensers and the second condenser, and an electric rotating rod is rotatably connected to the middle part of the top wall of the distillation cylinder. The electric rotating rod rotates from the first collecting component to the second collecting component and the third collecting component, and every time the electric rotating rod rotates ninety degrees, the first collecting component, the second collecting component or the third collecting component is connected to the distillation cylinder.

[0014] Preferably, the ball valve includes a valve housing, in which a valve core is rotatably connected, and the valve core is connected to a bevel gear through a valve stem, and a fan gear that cooperates with the bevel gear is connected to the side wall of the electric rotating rod, and after the fan gear approaches and meshes with the bevel gear, the electric rotating rod continues to rotate to increase the opening of the ball valve, and when the bevel gear is located in the middle of the fan gear, the opening of the ball valve is maximum and the electric rotating rod stops rotating, and when the bevel gear is located in the middle of the fan gear and the electric rotating rod continues to rotate so that the fan gear moves away from the bevel gear, the opening of the ball valve decreases until it is closed.

[0015] Preferably, a pressure sensor is connected to the distillation cylinder. After the external pressure pump stops running, when the pressure sensor detects that the pressure value in the distillation cylinder is stable, the electric rotating rod rotates ninety degrees.

[0016] Preferably, the distillation cylinder is connected to a buckle cylinder, a sliding rod is slidably connected inside the buckle cylinder, the diameter of the sliding rod is smaller than the inner diameter of the buckle cylinder, and a position sensor for detecting the vertical sliding of the sliding rod is provided inside the buckle cylinder, a floating plate is connected to the bottom end of the sliding rod, and when the distillation cylinder is connected to the second collecting assembly, the product in the distillation cylinder boils, causing the floating plate to move vertically back and forth, thereby increasing the pumping speed of the external water pump.

[0017] A distillation separation method for a cyanate synthesis reaction device comprises the following steps:

[0018] Close the valve, control the first collecting cylinder to be connected with the distillation cylinder first, start the external pressure pump to rotate forward, pump nitrogen or other inert gases into the entire mechanism, so that the air and moisture in the entire mechanism are discharged;

[0019] Connect the transfer pipe to the reactor, open the valve, transfer the product in the reactor to the distillation cylinder, then place the distillation cylinder in an oil bath, close the valve after the product is completely transferred to the distillation cylinder, control the operation of the oil bath, and heat the distillation cylinder to a temperature range from room temperature to 50 degrees;

[0020] The external pressure pump is controlled to reverse, and the whole mechanism is depressurized to 1-10 mmHg. The cyanogen chloride and hydrogen chloride in the product are first collected by the first collecting component. At the same time, the pressure sensor detects the pressure in the distillation cylinder. When the pressure is higher than 1-10 mmHg, the control system controls the external pressure pump to start, and the distillation cylinder is depressurized again to the range of 1-10 mmHg.

[0021] The pressure sensor continuously detects the pressure in the distillation cylinder. When the internal pressure of the distillation cylinder no longer fluctuates within the temperature range of room temperature to fifty degrees, it indicates that cyanogen chloride and hydrogen chloride have been separated. After the distillation cylinder is connected to the first collection cylinder for a period of time, the control system controls the electric rotating rod to rotate so that the distillation cylinder is connected to the second collection cylinder.

[0022] The oil bath pot continues to heat up to the boiling point temperature of the bisphenol compound under the pressure state of 1-10mmHg, so that the bisphenol compound is distilled and separated from the product. The control system continues to control the operation of the external pressure pump through the detection of the pressure sensor, so that the distillation cylinder maintains a negative pressure in the range of 1-10mmHg. When the product in the distillation cylinder boils more due to the heat, the vertical sliding distance of the slide rod increases. When the displacement sensor detects the increase in the sliding distance of the slide rod, the control system controls the pumping speed of the external water pump to increase. At the same time, the control system no longer performs the decompression action according to the value of the pressure sensor, and then flows in The water pressure of the second water inlet pipe increases, which improves the condensation effect of the second condenser. Under the influence of the water pressure, the slide moves downward, which increases the height of the second collecting cylinder. At the same time, the total volume of the internal space of the distillation cylinder and the space at the lower part of the slide in the second collecting cylinder for collecting bisphenol compounds is reduced, which reduces the negative pressure intensity in the distillation cylinder, thereby slowing down the boiling degree of the product. At the same time, the droplets condensed in the second condenser flow back into the distillation cylinder, so that the high-boiling-point cyanate ester that may be entrained in the fraction of the low-boiling-point bisphenol compound can flow back into the distillation cylinder to avoid being collected by the second collecting cylinder and causing loss;

[0023] After the insertion rod extends out of the second collecting cylinder, the reset rod is in a state of contacting the ground. At this time, the gravity of the entire second collecting cylinder applies pressure to the reset rod, causing the reset rod to slide into the insertion rod, and the liquid medium in the cavity of the insertion rod slowly flows to the upper part of the ring through the deceleration of the ring, so that the reset rod retracts, causing the second collecting cylinder to descend, so that the boiling degree of the product in the distillation cylinder is relieved, and the bisphenol compound in the product continues to be separated;

[0024] When the pressure of the distillation cylinder no longer fluctuates at the boiling point temperature of the bisphenol compound under the pressure state of 1-10 mmHg, it indicates that the bisphenol compound in the product has been separated. After the distillation cylinder is connected to the second collection cylinder for a period of time, the control system controls the electric rotating rod to rotate so that the distillation cylinder is connected to the third collection cylinder.

[0025] The oil bath continues to heat up to the boiling point of the cyanate ester under a pressure of 1-10 mmHg, so that the bisphenol compound is distilled and separated from the product. At the same time, the control system controls the operation of the external pressure pump in real time according to the value of the pressure sensor to ensure that the distillation cylinder is within the pressure range of 1-10 mmHg until the cyanate ester is completely distilled and the entire mechanism stops running.

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

[0027] In the present invention, when the product in the distillation cylinder boils violently, the water flow rate from the second water inlet pipe to the second condensing cylinder increases, thereby increasing the water inlet pressure. At this time, the pressure is transmitted to the piston cylinder through the branch pipe of the second water inlet pipe, so that the pressure pushes the piston rod to overcome the tension of the tension spring and move downward, thereby causing the slide plate to move downward relative to the second collecting cylinder. At this time, the second collecting cylinder is connected to the distillation cylinder through the second condensing pipe, and the total volume of the connecting space between the two decreases, thereby reducing the negative pressure. At this time, the boiling degree of the product in the distillation cylinder is slowed down, and the water inlet pressure is increased while strengthening the condensation effect on the second condensing pipe. As a result, the steam inside it is accelerated to condense. When the slide plate moves downward, the insertion rod connected to the lower part of the slide plate moves downward synchronously. At this time, the insertion rod moves out from under the bottom wall of the second collecting cylinder, thereby increasing the height of the second collecting cylinder. When the height of the second collecting cylinder increases, the second condenser tube will tilt, so that the droplets formed by the accelerated condensation inside it will flow back into the distillation cylinder, so that the high-boiling-point cyanate ester that may be entrained in the fraction of low-boiling-point bisphenol compounds can flow back into the distillation cylinder, avoiding loss caused by being collected by the second collecting cylinder, thereby ensuring that the amount of cyanate ester obtained by the final distillation separation will not be reduced. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0029] Figure 2 It is a schematic diagram of the structure of three collecting components of the present invention;

[0030] Figure 3 It is a structural schematic diagram of the distillation cylinder of the present invention;

[0031] Figure 4 For the present invention Figure 3 The structural diagram of part B;

[0032] Figure 5 It is a structural schematic diagram of the first condenser pipe of the present invention;

[0033] Figure 6 It is a structural schematic diagram of the floating plate of the present invention;

[0034] Figure 7 It is a structural schematic diagram of the second collecting component of the present invention;

[0035] Figure 8 For the present invention Figure 7 The structural diagram of part A in the figure;

[0036] Fig. 9 It is a structural schematic diagram of the second collecting cylinder of the present invention;

[0037] Fig.10 It is a structural schematic diagram of the piston rod of the present invention;

[0038] Fig.11 It is a schematic structural diagram of the circular ring of the present invention.

[0039] In the figure: 100, distillation assembly; 110, distillation cylinder; 120, transmission pipe; 121, valve; 130, pressure pipe; 140, buckle cylinder; 150, slide rod; 160, floating plate; 170, pressure sensor; 200, first collection assembly; 210, first collection cylinder; 220, first condensation pipe; 230, first condensation cylinder; 240, first water inlet pipe; 250, first drainage pipe; 300, second collection assembly; 310, second collection cylinder; 311, outer cylinder; 320, second condensation pipe; 321 , first hemispherical shell; 322, second hemispherical shell; 323, connecting pipe; 330, second condensing cylinder; 331, second water inlet pipe; 332, second drain pipe; 340, slide plate; 350, piston cylinder; 360, piston rod; 361, tension spring; 370, plug rod; 380, reset rod; 390, ring; 400, third collecting assembly; 410, third collecting cylinder; 500, switching mechanism; 510, electric rotating rod; 520, fan gear; 530, valve housing; 540, valve core; 550, bevel gear. DETAILED DESCRIPTION

[0040] 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.

[0041] Reference Figure 1-Figure 11 The present embodiment provides a technical solution: a distillation separation mechanism of a cyanate synthesis reaction device, comprising a distillation assembly 100, the distillation assembly 100 comprises a distillation cylinder 110, the distillation cylinder 110 is connected to a reactor, and further comprises a first collecting assembly 200 for collecting cyanogen chloride and hydrogen chloride, a second collecting assembly 300 for collecting bisphenol compounds, and a third collecting assembly 400 for collecting cyanate, the distillation assembly 100 is sequentially connected to the first collecting assembly 200, the second collecting assembly 300 and the third collecting assembly 400; the second collecting assembly 300 comprises a second collecting cylinder 310, a second condensing tube 320 is connected between the second collecting cylinder 310 and the distillation cylinder 110, a second condensing tube 330 is sleeved on the second condensing tube 320, a slide plate 340 is slidably connected in the second collecting cylinder 310, a piston rod 360 is connected to the slide plate 340, a piston cylinder 350 is connected to the second collecting cylinder 310, and the piston rod 360 slides It is connected to the piston cylinder 350, and a tension spring 361 is connected between the piston rod 360 and the piston cylinder 350, and an insertion rod 370 is connected to the lower surface of the slide plate 340, and the insertion rod 370 passes through the bottom wall of the second collecting cylinder 310; the second condensing cylinder 330 is connected to the second water inlet pipe 331 and the second drain pipe 332, and the second water inlet pipe 331 is provided with a branch pipe connected to the piston cylinder 350. After the product in the distillation cylinder 110 is separated from cyanogen chloride and hydrogen chloride, the distillation cylinder 110 is connected to the second collecting cylinder 310. When the product in the distillation cylinder 110 boils violently, the water inlet pressure of the second water inlet pipe 331 increases so that the steam in the second condensing pipe 320 is quickly condensed, and the slide plate 340 moves down to the second collecting cylinder 310 to reduce the negative pressure strength in the distillation cylinder 110. At the same time, the insertion rod 370 lifts the second collecting cylinder 310 to make the second collecting cylinder 310 rise, so that the condensed liquid in the second condensing pipe 320 flows back to the distillation cylinder 110.

[0042] First, nitrogen or other inert gas is pumped into the entire mechanism to discharge air and moisture in the entire mechanism, the distillation cylinder 110 is connected to the reactor for synthesizing cyanate ester, and the product synthesized from the bisphenol compound and cyanogen chloride is transferred from the reactor to the distillation cylinder 110, and then the entire mechanism is evacuated, the distillation cylinder 110 is first connected to the first collecting component 200 to separate cyanogen chloride and hydrogen chloride, and then connected to the second collecting component 300 to separate the bisphenol compound, and finally connected to the third collecting component 400 to collect the final product cyanate ester;

[0043] When collecting bisphenol compounds, the oil bath is heated so that the product in the distillation cylinder 110 reaches the boiling point of the bisphenol compounds, and the evaporated bisphenol compound gas enters the second condenser tube 320. Cold water is passed into the second condenser tube 330 sleeved on the second condenser tube 320 so that the evaporated bisphenol compounds are condensed into droplets and fall into the second collection tube 310. The side wall of the slide plate 340 is in contact with the inner wall of the second collection tube 310, and a hole is opened in the middle to match the second condenser tube 320, and the second condenser tube 320 is in contact with the inner wall of the hole to ensure the airtightness of the lower space of the slide plate 340, and at the same time, the condensed droplets can be collected by the second condenser tube 330. The lower space of the slide plate 340 is in a negative pressure state, and the tension spring 361 applies a pulling force to the slide plate 340, so that the slide plate 340 does not slide down too much at this time. The oil bath is heated evenly, but its temperature The change process is relatively slow, so when the product in the distillation cylinder 110 boils violently, the temperature cannot be reduced in time. Therefore, when the product in the distillation cylinder 110 boils violently, the water flow from the second water inlet pipe 331 to the second condensation cylinder 330 increases, thereby increasing the water inlet pressure. At this time, the pressure is transmitted to the piston cylinder 350 through the branch pipe of the second water inlet pipe 331, so that the pressure pushes the piston rod 360 to overcome the tension of the tension spring 361 and move downward, thereby causing the slide plate 340 to move downward relative to the second collecting cylinder 310. At this time, the second collecting cylinder 310 is connected to the distillation cylinder 110 through the second condensation pipe 320, and the total volume of the connecting space between the two decreases, thereby reducing the negative pressure. At this time, the boiling degree of the product in the distillation cylinder 110 will be slowed down. While the water inlet pressure increases, the condensation effect on the second condensation pipe 320 is enhanced, so that the steam inside it is accelerated to condense.

[0044] When the slide plate 340 moves downward, the rod 370 connected to the lower part of the slide plate 340 moves downward synchronously. At this time, the rod 370 moves out from under the bottom wall of the second collecting cylinder 310, thereby increasing the height of the second collecting cylinder 310. When the height of the second collecting cylinder 310 increases, the second condenser 320 will tilt, so that the droplets formed by accelerated condensation inside it will flow back into the distillation cylinder 110, so that the high-boiling-point cyanate esters that may be entrained in the fraction of low-boiling-point bisphenol compounds can flow back into the distillation cylinder 110, avoiding loss caused by being collected by the second collecting cylinder 310, thereby ensuring that the amount of cyanate ester obtained by the final distillation separation will not be reduced.

[0045] The second collection component 300 also includes a first hemispherical shell 321, a second hemispherical shell 322 and a connecting pipe 323. The first hemispherical shell 321 is connected to one end of the second condenser 320 away from the second collection cylinder 310, the second hemispherical shell 322 is connected to the connecting pipe 323, the connecting pipe 323 is connected to the distillation cylinder 110, and the first hemispherical shell 321 is hinged in the second hemispherical shell 322.

[0046] The first hemispherical shell 321 rotates inside the second hemispherical shell 322, so that when the second collecting cylinder 310 rises, the first hemispherical shell 321 can rotate relative to the second hemispherical shell 322, thereby ensuring that the second condenser 320 is connected to the distillation cylinder 110 while preventing the rising of the second collecting cylinder 310 from interference.

[0047] The outer cylinder 311 is connected to the bottom wall of the second collecting cylinder 310, and the insertion rod 370 slides in the outer cylinder 311. A cavity is opened at the bottom of the insertion rod 370, and a reset rod 380 is slidably connected in the cavity. A ring 390 is connected to the upper part of the reset rod 380 in the cavity, and the cavity is filled with a liquid medium. After the insertion rod 370 slides to the outside of the second collecting cylinder 310, the second collecting cylinder 310 applies pressure on the reset rod 380, so that the liquid medium in the cavity located at the lower part of the ring 390 slowly flows to the upper part of the ring 390, so that the height of the second collecting cylinder 310 drops to its original position.

[0048] The outer cylinder 311 passes through the bottom wall of the second collection cylinder 310, and the insertion rod 370 is inserted into the outer cylinder 311 and fits with the inner wall of the outer cylinder 311 to ensure the airtightness of the second collection cylinder 310. When the slide plate 340 moves downward, the insertion rod 370 can move downward on the outer cylinder 311, and the reset rod 380 slides on the bottom end of the insertion rod 370, so that the reset rod 380 first contacts the ground. At this time, the overall weight of the second collection cylinder 310 presses down on the reset rod 380, so that the reset rod 380 can move up on the insertion rod 370. At this time, the liquid medium at the lower part of the ring 390 in the cavity slowly passes through the hole in the middle of the ring 390. When the liquid flows to the upper part of the ring 390, the reset rod 380 slowly moves up to the insertion rod 370. At this time, the height of the second collecting cylinder 310 slowly decreases, ensuring that the condensed droplets in the second condenser 320 have enough time to flow back into the distillation cylinder 110. At this time, the second condenser 320 also returns to its original position. Since the overall length of the reset rod 380 and the insertion rod 370 is shortened, the second collecting cylinder 310 descends, and the slide 340 maintains its position after the downward movement. Therefore, the boiling degree of the product in the distillation cylinder 110 is alleviated and the distillation and separation of the bisphenol compounds can continue.

[0049] The distillation component 100 also includes a transmission pipe 120 connected to the reaction kettle and the distillation cylinder 110, and a valve 121 is provided on the transmission pipe 120. The first collection component 200, the second collection component 300 and the third collection component 400 are commonly connected with a pressure pipe 130, and the pressure pipe 130 is connected to an external pressure pump. When the valve 121 is closed and the external pressure pump is turned on, the pressure pipe 130 applies negative pressure to the first collection component 200, the second collection component 300 and the third collection component 400.

[0050] When an inert gas such as nitrogen is introduced into the first collecting assembly 200, the second collecting assembly 300 and the third collecting assembly 400, the transmission pipe 120 is not connected to the reactor at this time, and the valve 121 is in an open state. In the initial state, the distillation cylinder 110 is connected to the first collecting assembly 200, and the nitrogen enters the first collecting cylinder 210, the second collecting cylinder 310 and the third collecting cylinder 410 respectively through the pressure pipe 130. At this time, the first collecting cylinder 210 is connected to the distillation cylinder 110 through the first condenser 220. 0 and the third collecting cylinder 410 are interconnected through the pressure pipe 130, so that the air and water vapor in the whole mechanism are discharged through the transmission pipe 120, so that the whole mechanism is filled with nitrogen. After the product in the reactor is transferred to the distillation cylinder 110, the valve 121 is closed, and the external pressure pump is controlled to reverse, so that the external pressure pump can evacuate the first collecting cylinder 210, the second collecting cylinder 310, the third collecting cylinder 410 and the distillation cylinder 110, so that the boiling point of the product is reduced, ensuring that it can be distilled, and at the same time, the product will not be damaged by high temperature;

[0051] Solenoid valves may also be provided at the connection between the pressure tube 130 and the first collecting cylinder 210 , the second collecting cylinder 310 and the third collecting cylinder 410 . The solenoid valves corresponding to the collecting cylinders in the collecting state are in the open state, and the other solenoid valves are in the closed state.

[0052] The first collecting assembly 200 and the third collecting assembly 400 respectively include a first collecting cylinder 210 and a third collecting cylinder 410, both the first collecting cylinder 210 and the third collecting cylinder 410 are connected with a first condenser 220, both the two first condenser tubes 220 are connected with the distillation cylinder 110, both the first condenser tubes 220 are sleeved with a first condenser tube 230, both the first condenser tubes 230 are connected with a first water inlet pipe 240 and a first drain pipe 250, and the two first water inlet pipes 240 and the second water inlet pipe 331 are connected to the same external water pump.

[0053] After the whole mechanism is depressurized, the oil bath is controlled to operate, and the distillation cylinder 110 is heated to a temperature range from room temperature to fifty degrees, so that the cyanogen chloride and hydrogen chloride in the product are separated and collected by the first collecting component 200, and then the second collecting component 300 collects the bisphenol compound. After the bisphenol compound is distilled and separated, the oil bath continues to heat up to allow the cyanate ester to boil. At this time, the distillation cylinder 110 is connected to the third collecting cylinder 410 to collect the cyanate ester. The external water pump is connected to the two first water inlet pipes 240 and the one second water inlet pipe 331, and the two first water inlet pipes 240 and the one second water inlet pipe 331 are provided with solenoid valves. The control system controls the solenoid valves on the water inlet pipes corresponding to the collecting cylinder connected to the distillation cylinder 110 to be in an open state, and the others are in a closed state to ensure that the flow rate and pressure of the condensed water are sufficient.

[0054] It also includes a switching mechanism 500, which includes three ball valves arranged on the two first condensing tubes 220 and the second condensing tube 320. An electric rotating rod 510 is rotatably connected to the middle of the top wall of the distillation cylinder 110. The electric rotating rod 510 rotates from the first collecting component 200 to the second collecting component 300 and the third collecting component 400, and every time the electric rotating rod 510 rotates ninety degrees, the first collecting component 200, the second collecting component 300 or the third collecting component 400 is connected to the distillation cylinder 110.

[0055] The ball valve is used to control the connection state between the corresponding condenser and the distillation cylinder 110, and only one of them is in the open state at the same time, ensuring that the cyanogen chloride and hydrogen chloride, bisphenol compounds and cyanate esters in the product are distilled and separated respectively. Three condensers are set to ensure that the distilled and separated products will not be impure due to residues. The electric rotary rod 510 is used to drive the three ball valves to open and close in sequence.

[0056] The ball valve includes a valve housing 530, in which a valve core 540 is rotatably connected. The valve core 540 is connected to a bevel gear 550 through a valve stem. A fan gear 520 that cooperates with the bevel gear 550 is connected to the side wall of the electric rotating rod 510. After the fan gear 520 approaches and meshes with the bevel gear 550, the electric rotating rod 510 continues to rotate to increase the opening of the ball valve. When the bevel gear 550 is located in the middle of the fan gear 520, the opening of the ball valve is maximum, and the electric rotating rod 510 stops rotating. Moreover, when the bevel gear 550 is located in the middle of the fan gear 520 and the electric rotating rod 510 continues to rotate so that the fan gear 520 is away from the bevel gear 550, the opening of the ball valve is reduced until it is closed.

[0057] The electric rotating rod 510 rotates unidirectionally to open and close the three ball valves in sequence. When the electric rotating rod 510 rotates, the fan gear 520 revolves around the electric rotating rod 510 as the center. After the fan gear 520 approaches and contacts the bevel gear 550, the electric rotating rod 510 continues to rotate. At this time, the fan gear 520 drives the bevel gear 550 to rotate. When the axis of the fan gear 520 points to the middle of the fan gear 520, the valve core 540 rotates ninety degrees, so that the ball valve is opened to the maximum opening. When the fan gear 520 continues to be driven by the electric rotating rod 510 to move at the current position, the valve core 540 continues to rotate unidirectionally, so that the opening of the ball valve is reduced. When the fan gear 520 is separated from the bevel gear 550, the ball valve is completely closed.

[0058] The valve core 540 is spherical with a through hole in the middle. The axis of the bevel gear 550 is perpendicular to the axis of the through hole in the middle of the valve core 540, so that the unidirectional rotation of the bevel gear 550 can drive the ball valve from a closed state to an open state, and the opening increases to the maximum and then continues to decrease until it is closed.

[0059] The distillation cylinder 110 is connected to a pressure sensor 170. After the external pressure pump stops running, when the pressure sensor 170 detects that the pressure value in the distillation cylinder 110 is stable, the electric rotating rod 510 rotates ninety degrees.

[0060] The pressure sensor 170 detects the pressure in the distillation cylinder 110. When the pressure is higher than 1-10 mmHg, the control system controls the external pressure pump to start, and the distillation cylinder 110 is depressurized to the range of 1-10 mmHg again. The pressure sensor 170 continuously detects the pressure in the distillation cylinder 110. When the distillation cylinder 110 is within the required temperature range and the internal pressure no longer fluctuates, it indicates that the substances to be distilled and separated have been separated. After maintaining the distillation cylinder 110 in communication with the first collection cylinder 210 for a period of time, the control system controls the electric rotating rod 510 to rotate and switch to communicate with the next collection component until the distillation and separation of the cyanate ester is completed;

[0061] In addition, when the bisphenol compound is distilled and separated, if the product boils violently, the control system will no longer perform the decompression action according to the value of the pressure sensor 170, thereby avoiding the intensification of the boiling of the product.

[0062] The distillation cylinder 110 is connected to a buckle cylinder 140, and a slide rod 150 is slidably connected inside the buckle cylinder 140. The diameter of the slide rod 150 is smaller than the inner diameter of the buckle cylinder 140, and a position sensor for detecting the vertical sliding of the slide rod 150 is arranged inside the buckle cylinder 140. The bottom end of the slide rod 150 is connected to a float plate 160. When the distillation cylinder 110 is connected to the second collecting assembly 300, the product in the distillation cylinder 110 boils, causing the float plate 160 to move back and forth vertically, thereby increasing the pumping speed of the external water pump.

[0063] When the product in the distillation cylinder 110 boils more intensely due to heat, the vertical sliding distance of the slide rod 150 increases. When the displacement sensor detects the increase in the sliding distance of the slide rod 150, the control system controls the external water pump to increase the pumping speed, thereby reducing the negative pressure in the distillation cylinder 110, accelerating the condensation speed of the second condenser 320, and allowing high-boiling-point cyanate esters that may be entrained in the fraction of low-boiling-point bisphenol compounds to flow back into the distillation cylinder 110.

[0064] A distillation separation method for a cyanate synthesis reaction device, applied to a distillation separation mechanism of the cyanate synthesis reaction device, comprises the following steps:

[0065] Close the valve 121, control the first collecting cylinder 210 to be connected with the distillation cylinder 110 first, start the external pressure pump to rotate forward, pump nitrogen or other inert gas into the entire mechanism, so that the air and moisture in the entire mechanism are discharged;

[0066] Connect the transfer pipe 120 to the reactor, open the valve 121, transfer the product in the reactor to the distillation cylinder 110, and then place the distillation cylinder 110 in an oil bath. After the product is completely transferred to the distillation cylinder 110, close the valve 121, and control the operation of the oil bath to heat the distillation cylinder 110 to a temperature range from room temperature to 50 degrees.

[0067] The external pressure pump is controlled to reverse and the whole mechanism is depressurized to 1-10 mmHg. The cyanogen chloride and hydrogen chloride in the product are first collected by the first collecting assembly 200. At the same time, the pressure sensor 170 detects the pressure in the distillation cylinder 110. When the pressure is higher than 1-10 mmHg, the control system controls the external pressure pump to start and depressurize the distillation cylinder 110 again to the range of 1-10 mmHg.

[0068] The pressure sensor 170 continuously detects the pressure in the distillation cylinder 110. When the internal pressure of the distillation cylinder 110 no longer fluctuates within the temperature range of room temperature to 50 degrees, it indicates that cyanogen chloride and hydrogen chloride have been separated. After the distillation cylinder 110 is connected to the first collection cylinder 210 for a period of time, the control system controls the electric rotating rod 510 to rotate, so that the distillation cylinder 110 is connected to the second collection cylinder 310.

[0069] The oil bath pot continues to heat up to the boiling point temperature of the bisphenol compound under the pressure state of 1-10 mmHg, so that the bisphenol compound is distilled and separated from the product. The control system continues to control the operation of the external pressure pump through the detection of the pressure sensor 170, so that the distillation cylinder 110 maintains a negative pressure in the range of 1-10 mmHg. When the product in the distillation cylinder 110 intensifies boiling due to heat, the vertical sliding distance of the slide bar 150 increases. When the displacement sensor detects that the sliding distance of the slide bar 150 increases, the control system controls the pumping speed of the external water pump to increase. At the same time, the control system no longer performs the decompression action according to the value of the pressure sensor 170, and then flows into the second water inlet pipe 331. The water pressure increases, which improves the condensation effect of the second condenser 320. Under the influence of the water pressure, the slide plate 340 moves downward, so that the height of the second collecting cylinder 310 increases. At the same time, the internal space of the distillation cylinder 110 and the total volume of the space at the lower part of the slide plate 340 in the second collecting cylinder 310 for collecting bisphenol compounds are reduced, so that the negative pressure intensity in the distillation cylinder 110 is reduced, thereby slowing down the boiling degree of the product. At the same time, the droplets condensed in the second condenser 320 flow back into the distillation cylinder 110, so that the high-boiling-point cyanate esters that may be entrained in the fraction of low-boiling-point bisphenol compounds can flow back into the distillation cylinder 110 to avoid being collected by the second collecting cylinder 310 and causing losses;

[0070] After the insertion rod 370 extends out of the second collection cylinder 310, the reset rod 380 is in contact with the ground. At this time, the gravity of the entire second collection cylinder 310 applies pressure to the reset rod 380, causing the reset rod 380 to slide into the insertion rod 370, and the liquid medium in the cavity of the insertion rod 370 slowly flows to the upper part of the ring 390 through the deceleration of the ring 390, so that the reset rod 380 retracts, causing the second collection cylinder 310 to descend, so that the boiling degree of the product in the distillation cylinder 110 is relieved, and the bisphenol compound in the product continues to be separated;

[0071] When the pressure of the distillation cylinder 110 no longer fluctuates at the boiling point temperature of the bisphenol compound under the pressure state of 1-10 mmHg, it indicates that the bisphenol compound in the product has been separated. After the distillation cylinder 110 is connected to the second collection cylinder 310 for a period of time, the control system controls the electric rotating rod 510 to rotate, so that the distillation cylinder 110 is connected to the third collection cylinder 410.

[0072] The oil bath continues to heat up to the boiling point of the cyanate ester under a pressure of 1-10 mmHg, so that the bisphenol compound is distilled and separated from the product. At the same time, the control system controls the operation of the external pressure pump in real time according to the value of the pressure sensor 170 to ensure that the distillation cylinder 110 is within the pressure range of 1-10 mmHg until the cyanate ester is completely distilled and the entire mechanism stops running.

[0073] 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 distillation separation mechanism of a cyanate synthesis reaction device, comprising a distillation assembly (100), wherein the distillation assembly (100) comprises a distillation cylinder (110), wherein the distillation cylinder (110) is connected to a reaction kettle, and characterized in that: It also includes a first collecting component (200) for collecting cyanogen chloride and hydrogen chloride, a second collecting component (300) for collecting bisphenol compounds, and a third collecting component (400) for collecting cyanate esters, and the distillation component (100) is sequentially connected to the first collecting component (200), the second collecting component (300), and the third collecting component (400); The second collecting assembly (300) comprises a second collecting cylinder (310), a second condensing tube (320) is connected between the second collecting cylinder (310) and the distilling cylinder (110), a second condensing cylinder (330) is sleeved on the second condensing tube (320), a slide plate (340) is slidably connected inside the second collecting cylinder (310), a hole matching with the second condensing tube (320) is opened in the middle of the slide plate (340), the second condensing tube (320) is in contact with the inner wall of the hole, and the second condensing tube (320) is away from the One end of the distillation cylinder (110) is located at the lower part of the slide plate (340), the slide plate (340) is connected to a piston rod (360), the second collection cylinder (310) is connected to a piston cylinder (350), the piston rod (360) is slidably connected in the piston cylinder (350), and a tension spring (361) is connected between the piston rod (360) and the piston cylinder (350), and the lower surface of the slide plate (340) is connected to an insertion rod (370), and the insertion rod (370) passes through the bottom wall of the second collection cylinder (310); The second condensing cylinder (330) is connected to a second water inlet pipe (331) and a second drain pipe (332). The second water inlet pipe (331) is provided with a branch pipe connected to the piston cylinder (350). After the product in the distillation cylinder (110) is separated into cyanogen chloride and hydrogen chloride, the distillation cylinder (110) is connected to the second collecting cylinder (310). When the product in the distillation cylinder (110) boils violently, the water inlet pressure of the second water inlet pipe (331) increases so that the steam in the second condensing tube (320) is quickly condensed, and the slide plate (340) moves downward to the second collecting cylinder (310) to reduce the negative pressure strength in the distillation cylinder (110). At the same time, the insertion rod (370) lifts the second collecting cylinder (310) so that the second collecting cylinder (310) rises, so that the condensed liquid in the second condensing tube (320) flows back into the distillation cylinder (110).

2. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 1, characterized in that: The second collecting assembly (300) also includes a first hemispherical shell (321), a second hemispherical shell (322) and a connecting pipe (323), wherein the first hemispherical shell (321) is connected to one end of the second condensing tube (320) away from the second collecting cylinder (310), the second hemispherical shell (322) is connected to the connecting pipe (323), the connecting pipe (323) is connected to the distillation cylinder (110), and the first hemispherical shell (321) is hinged in the second hemispherical shell (322).

3. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 2, characterized in that: An outer cylinder (311) is connected to the bottom wall of the second collecting cylinder (310), the insertion rod (370) slides in the outer cylinder (311), a cavity is opened at the bottom of the insertion rod (370), and a reset rod (380) is slidably connected in the cavity, a circular ring (390) is connected to the upper part of the reset rod (380) in the cavity, and the cavity is filled with a liquid medium. After the insertion rod (370) slides toward the outside of the second collecting cylinder (310), the second collecting cylinder (310) applies pressure to the reset rod (380), so that the liquid medium in the cavity located at the lower part of the circular ring (390) slowly flows to the upper part of the circular ring (390), so that the height of the second collecting cylinder (310) drops to its original position.

4. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 3, characterized in that: The distillation component (100) further comprises a transmission pipe (120) connected to the reaction kettle and the distillation cylinder (110), wherein the transmission pipe (120) is provided with a valve (121), and the first collecting component (200), the second collecting component (300) and the third collecting component (400) are commonly connected with a pressure pipe (130), and the pressure pipe (130) is connected to an external pressure pump. When the valve (121) is closed and the external pressure pump is turned on, the pressure pipe (130) applies negative pressure to the first collecting component (200), the second collecting component (300) and the third collecting component (400).

5. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 4, characterized in that: The first collecting assembly (200) and the third collecting assembly (400) respectively include a first collecting cylinder (210) and a third collecting cylinder (410); the first collecting cylinder (210) and the third collecting cylinder (410) are both connected to a first condenser (220); the two first condenser tubes (220) are both connected to the distillation cylinder (110); the two first condenser tubes (220) are both sleeved with a first condenser tube (230); the two first condenser tubes (230) are both connected to a first water inlet pipe (240) and a first drain pipe (250); the two first water inlet pipes (240) and the second water inlet pipe (331) are connected to the same external water pump.

6. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 5, characterized in that: The invention also includes a switching mechanism (500), wherein the switching mechanism (500) includes three ball valves arranged on the two first condensing tubes (220) and the second condensing tube (320), and an electric rotating rod (510) is rotatably connected to the middle part of the top wall of the distillation cylinder (110), and the electric rotating rod (510) rotates from the first collecting component (200) to the second collecting component (300) and the third collecting component (400), and when the electric rotating rod (510) rotates ninety degrees, the first collecting component (200), the second collecting component (300) or the third collecting component (400) is connected to the distillation cylinder (110).

7. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 6, characterized in that: The ball valve comprises a valve housing (530), a valve core (540) being rotatably connected inside the valve housing (530), the valve core (540) being connected to a bevel gear (550) via a valve stem, a fan-shaped gear (520) cooperating with the bevel gear (550) being connected to the side wall of the electric rotating rod (510), after the fan-shaped gear (520) approaches and meshes with the bevel gear (550), the electric rotating rod (510) continues to rotate so that the opening of the ball valve increases, when the bevel gear (550) is located in the middle of the fan-shaped gear (520), the opening of the ball valve is maximum, and the electric rotating rod (510) stops rotating, and when the bevel gear (550) is located in the middle of the fan-shaped gear (520) and the electric rotating rod (510) continues to rotate so that the fan-shaped gear (520) moves away from the bevel gear (550), the opening of the ball valve decreases until it is closed.

8. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 7, characterized in that: The distillation cylinder (110) is connected to a pressure sensor (170). After the external pressure pump stops running, when the pressure sensor (170) detects that the pressure value in the distillation cylinder (110) is stable, the electric rotating rod (510) rotates ninety degrees.

9. The distillation separation mechanism of the cyanate synthesis reaction device according to claim 8, characterized in that: The distillation cylinder (110) is connected to a buckle cylinder (140), and a slide rod (150) is slidably connected inside the buckle cylinder (140). The diameter of the slide rod (150) is smaller than the inner diameter of the buckle cylinder (140), and a position sensor for detecting the vertical sliding of the slide rod (150) is arranged inside the buckle cylinder (140). The bottom end of the slide rod (150) is connected to a float plate (160). When the distillation cylinder (110) is connected to the second collecting assembly (300), the product in the distillation cylinder (110) boils, causing the float plate (160) to move back and forth vertically, thereby increasing the pumping speed of the external water pump.

10. A distillation separation method for a cyanate synthesis reaction device, applied to the distillation separation mechanism of the cyanate synthesis reaction device according to claim 9, characterized in that: The following steps are involved: The valve (121) is closed, the first collecting cylinder (210) is controlled to be connected with the distillation cylinder (110) first, and the external pressure pump is started to rotate forward to pump nitrogen or other inert gas into the entire mechanism, so that the air and moisture in the entire mechanism are discharged; Connect the transfer pipe (120) to the reactor, open the valve (121), transfer the product in the reactor to the distillation cylinder (110), place the distillation cylinder (110) in an oil bath, close the valve (121) after the product is completely transferred to the distillation cylinder (110), control the operation of the oil bath, and heat the distillation cylinder (110) to a temperature range from room temperature to fifty degrees; The external pressure pump is controlled to reverse and the entire mechanism is depressurized to 1-10 mmHg. The cyanogen chloride and hydrogen chloride in the product are first collected by the first collecting component (200). At the same time, the pressure sensor (170) detects the pressure in the distillation cylinder (110). When the pressure is higher than 1-10 mmHg, the control system controls the external pressure pump to start and the distillation cylinder (110) is depressurized again to the range of 1-10 mmHg. The pressure sensor (170) continuously detects the pressure inside the distillation cylinder (110). When the internal pressure of the distillation cylinder (110) no longer fluctuates within a temperature range from room temperature to fifty degrees, it indicates that cyanogen chloride and hydrogen chloride have been separated. After the distillation cylinder (110) and the first collection cylinder (210) are connected for a period of time, the control system controls the electric rotating rod (510) to rotate, so that the distillation cylinder (110) is connected to the second collection cylinder (310); The oil bath pot continues to be heated to the boiling point temperature of the bisphenol compound under a pressure state of 1-10 mmHg, so that the bisphenol compound is distilled and separated from the product. The control system continues to control the operation of the external pressure pump through the detection of the pressure sensor (170), so that the distillation cylinder (110) maintains a negative pressure in the range of 1-10 mmHg. When the product in the distillation cylinder (110) boils more due to the heat, the vertical sliding distance of the slide bar (150) increases. When the displacement sensor detects that the sliding distance of the slide bar (150) increases, the control system controls the pump speed of the external water pump to increase. At the same time, the control system no longer performs a decompression action according to the value of the pressure sensor (170). Subsequently, the water pressure flowing in the second water inlet pipe (331) increases. , improving the condensation effect of the second condenser (320), under the influence of water pressure, the slide plate (340) moves downward, so that the height of the second collecting cylinder (310) increases, and at the same time, the internal space of the distillation cylinder (110) and the total volume of the space in the second collecting cylinder (310) at the lower part of the slide plate (340) for collecting bisphenol compounds are reduced, so that the negative pressure intensity in the distillation cylinder (110) is reduced, thereby slowing down the boiling degree of the product. At the same time, the droplets condensed in the second condenser (320) flow back into the distillation cylinder (110), so that the high-boiling-point cyanate ester that may be entrained in the fraction of the low-boiling-point bisphenol compound can flow back into the distillation cylinder (110), avoiding being collected by the second collecting cylinder (310) and causing loss; After the insertion rod (370) extends out of the second collection cylinder (310), the reset rod (380) is in a state of contacting the ground. At this time, the gravity of the entire second collection cylinder (310) applies pressure to the reset rod (380), causing the reset rod (380) to slide into the insertion rod (370), and the liquid medium in the cavity of the insertion rod (370) slowly flows to the upper part of the ring (390) through the deceleration of the ring (390), so that the reset rod (380) retracts, causing the second collection cylinder (310) to descend, so that the boiling degree of the product in the distillation cylinder (110) is relieved, and the bisphenol compound in the product continues to be separated; When the pressure of the distillation cylinder (110) no longer fluctuates at the boiling point temperature of the bisphenol compound under a pressure state of 1-10 mmHg, it indicates that the bisphenol compound in the product has been separated. After the distillation cylinder (110) and the second collection cylinder (310) are maintained in communication for a period of time, the control system controls the electric rotating rod (510) to rotate, so that the distillation cylinder (110) is connected to the third collection cylinder (410); The oil bath pot continues to be heated to the boiling point of the cyanate ester under a pressure state of 1-10 mmHg, so that the bisphenol compound is distilled and separated from the product. At the same time, the control system controls the operation of the external pressure pump in real time according to the value of the pressure sensor (170) to ensure that the distillation cylinder (110) is within the pressure range of 1-10 mmHg until the cyanate ester is completely distilled and the entire mechanism stops operating.

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