CN113578236A - Efficient and safe cyanate ester polymerization equipment and polymerization process - Google Patents
Efficient and safe cyanate ester polymerization equipment and polymerization process Download PDFInfo
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- CN113578236A CN113578236A CN202110903954.3A CN202110903954A CN113578236A CN 113578236 A CN113578236 A CN 113578236A CN 202110903954 A CN202110903954 A CN 202110903954A CN 113578236 A CN113578236 A CN 113578236A
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Abstract
The invention relates to efficient and safe cyanate ester polymerization equipment and a polymerization process, and belongs to the technical field of high polymer materials. The polymerization equipment comprises a steel platform, a preheating tank is arranged at the top of the steel platform, a plurality of polymerization devices, a quenching device and an extrusion device are sequentially arranged below the preheating tank, and the polymerization process comprises the following steps: preheating a polymerization monomer to form a molten material at a temperature higher than the melting temperature of 4-7 ℃, discharging the molten material into a polymerization device, heating and polymerizing until the polymerization degree is lower than a target value of 0.02-0.05/105 ℃, pumping a solvent and stirring to form a mixed material, discharging the mixed material into a quenching device, rapidly cooling to terminate the reaction, and cooling, extruding and collecting the polymer through an extruding device. The invention realizes preheating of the polymerization monomer, rapid heating polymerization of the polymerization monomer and rapid cooling of the polymer, and the whole reaction process is controlled, safe and efficient.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to efficient and safe cyanate ester polymerization equipment and a polymerization process.
Background
Cyanate resin is known as the most competitive resin type for preparing structure-function materials due to its excellent dielectric properties, outstanding heat resistance and good comprehensive mechanical properties, and its main uses have 3 aspects: the composite material is used for a high-performance printed circuit board substrate, a high-performance wave-transparent structure material substrate and a structural composite material substrate for aerospace.
In the prior art, the cyanate ester polymerization process comprises the following steps: feeding the materials into a reaction kettle at one time, heating until the monomers are melted, starting stirring, continuously heating to monitor the polymerization degree change of the materials in real time, adding butanone after the polymerization degree reaches a target, cooling and stopping the reaction. This polymerization process suffers from two disadvantages:
1. when the capacity of a refrigeration system is insufficient, the polymerization process is easy to lose control, the whole system can emit a large amount of heat, and the safety risk coefficient is high;
2. finished GT produced by the polymerization process has generally higher index, is greatly influenced by monomer GT and is difficult to meet the requirement of quality stability.
Disclosure of Invention
In order to overcome the technical problems mentioned in the background art, the invention aims to provide efficient and safe cyanate ester polymerization equipment and a polymerization process.
The purpose of the invention can be realized by the following technical scheme:
an efficient and safe cyanate ester polymerization process comprises the following steps:
firstly, conveying a polymerization monomer raw material into a preheating tank of polymerization equipment, heating to a temperature 4-7 ℃ higher than the melting temperature of the polymerization monomer, and stirring until the polymerization monomer is completely melted to obtain a molten material;
pumping the molten material into a polymerization device, driving a heater by a first motor to stir the molten material to raise the temperature to a polymerization temperature, carrying out polymerization reaction by heat preservation and stirring, stopping heating when the polymerization degree is lower than a target value of 0.02-0.05/105 ℃, pumping a solvent and stirring to obtain a mixture;
discharging the mixture into a quenching tank, releasing a coolant into a cooling flow channel, rapidly cooling the mixture, and terminating the polymerization reaction;
and fourthly, sucking the mixture subjected to rapid cooling into an extrusion device, slowly cooling to a collection temperature, and extruding for storage.
A high-efficiency and safe cyanate ester polymerization device comprises a steel platform, wherein a preheating tank is arranged at the top of the steel platform, a plurality of polymerization devices are communicated below the preheating tank, the polymerization devices are fixedly connected with the steel platform through trusses, a quenching device is arranged below the polymerization devices, and an extrusion device is arranged below the quenching device;
the polymerization device comprises a reaction tube and a heater arranged in the reaction tube, wherein a driving shaft is fixed at the top of the heater, the driving shaft penetrates through the top wall of the reaction tube, the driving shaft is rotatably installed with the reaction tube through a sealing bearing seat, a carbon brush is fixed on the peripheral side wall of the driving shaft, an electrode is arranged on a steel platform, the heater is powered through the carbon brush, a driven gear is fixed at the top end of the driving shaft, a first motor is arranged on the bottom surface of the steel platform, a driving gear is fixed at the output end of the first motor, the driving gear is in meshing transmission connection with the driven gear through a chain, the heater comprises an I-shaped installation seat and a plurality of electric heating tubes fixed between the I-shaped installation seats, the electric heating tubes are electrically connected with the carbon brush, the heater is rotated and powered, stirring and heating are carried out from the middle part of the reaction tube, the traditional side wall heating type polymerization kettle is avoided, and local heating is carried out on the near layer of the inner wall, resulting in over-reaction and thus formation of a polymer with higher viscosity, which affects the heat transfer of the polymer.
The two sides of the side wall of the upper part of the reaction tube are respectively provided with a first feeding tube and a solvent tube for feeding molten materials and leading in solvent, and the bottom wall of the reaction tube is provided with a first discharging tube for discharging mixed materials.
The wall of the reaction tube is provided with a heat insulation material, so that heat loss is reduced and energy consumption is reduced during continuous polymerization reaction.
The quenching device comprises a plurality of cooling unit, and every cooling unit includes the cooling tank and sets up in the installation central siphon at cooling tank center, is provided with the baffle between the inner wall of cooling tank and the week lateral wall of installation central siphon, separates the inner chamber of cooling tank for cooling runner and material runner, cooling runner and material runner are the heliciform, and cooling runner and material runner distribute in turn, and the roof of cooling tank is provided with the second feed pipe, and the diapire of cooling tank is provided with the second and arranges the material pipe, and row's material pipe of second feed pipe and second all with material runner intercommunication, one side of cooling tank is provided with the cooling and advances the pipe, and the opposite side of cooling tank is provided with the cooling exit tube, and the cooling advances the pipe and all with the cooling runner intercommunication.
The cooling outlet pipe is located at one side close to the second feeding pipe, and the cooling inlet pipe is located at one side close to the second discharging pipe, so that the refrigerant and the mixture form convection, and the heat exchange efficiency is higher.
One end of the cooling inlet pipe is communicated with a throttle valve, the throttle valve is communicated with a compressed refrigerant pipeline and used for controlling the decompression and release of the compressed refrigerant, so that the refrigerant is vaporized and absorbs heat to cool the mixture, a flow meter is arranged in the cooling inlet pipe and used for accurately monitoring the introduction amount of the compressed refrigerant and controlling the temperature of the mixture to be reduced, all cooling outlet pipes are communicated with a gas collecting pipe, the gas collecting pipe is communicated with compression equipment, the vaporized refrigerant is collected and is compressed and recycled by the compression equipment.
And a cleaning pipe is arranged on one side of each cooling tank, and when the reaction is stopped, a cleaning agent is introduced from the cleaning pipe to clean the quenching device.
The width-depth ratio of the material flow channel is 0.5-0.7:1, the width-depth ratio of the cooling flow channel is 0.13-0.2:1, and under the size, the refrigerant and the mixture fully exchange heat, and the cooling speed is high.
The number of spiral turns of the material flow channel and the cooling flow channel of each cooling unit is 4-7.
The extruding device comprises an extruding pipe, a screw extruder is arranged at one end of the extruding pipe, a third feeding pipe is communicated with a feeding end of the screw extruder, a tubular heat exchanger is communicated with an extruding end of the screw extruder, a water inlet pipe is communicated with the bottom surface of the tubular heat exchanger, a water outlet pipe is communicated with the top surface of the tubular heat exchanger, cooling water is introduced into the tubular cooler when the extruding device is extruded, and the mixture after being rapidly cooled is further cooled to a collecting temperature.
The invention has the beneficial effects that:
1. according to the efficient and safe cyanate ester polymerization equipment provided by the invention, the polymerization monomer is firstly heated to 4-7 ℃ above the melting temperature through the preheating tank, then the polymerization monomer is pumped into the polymerization device, the polymerization monomer is heated and polymerized by the rotating heater, the polymerization monomer is continuously heated in a uniform molten state and is uniformly heated, and the polymerization monomer is stirred and heated from the middle part of the reaction tube through the heater, so that the polymerization monomer is prevented from contacting with the inner wall of the high-temperature large-area polymerization kettle, a polymer with higher viscosity is formed at the near layer of the inner wall, the heat exchange of the polymerization monomer at the middle part is influenced, the polymerization is prevented from being nonuniform, and the reaction is out of control at the inner wall of the polymerization kettle, so that the potential safety hazard is formed.
2. The invention provides a quenching device composed of a plurality of cooling units, wherein a cooling flow channel and a material flow channel which are spirally arranged in the same direction are arranged in a cooling tank, when the polymerization is about to reach a target value, the polymerization is discharged into the material flow channel, in the discharging process, the polymerization is promoted by using waste heat, then a compressed refrigerant is introduced into the cooling flow channel through a throttle valve, the vaporization process rapidly absorbs heat, through reasonable flow channel parameter design, the polymer is rapidly cooled to be below the polymerization temperature, the polymerization reaction is immediately stopped, and the reaction is prevented from being out of control to emit a large amount of heat.
3. The efficient and safe cyanate ester polymerization equipment provided by the invention realizes preheating of the polymerization monomers, rapid heating polymerization of the polymerization monomers and rapid cooling of the polymer, the whole reaction process is controlled, the equipment is suitable for most cyanate ester resin polymerization reactions, and the prepolymer GT is 60-80 min.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a high-efficiency and safe cyanate ester polymerization apparatus according to the present invention;
FIG. 2 is a schematic view of a polymerization apparatus;
FIG. 3 is a schematic view of a quenching apparatus;
FIG. 4 is a schematic view of the internal structure of the cooling tank;
FIG. 5 is a schematic view showing an external structure of an extrusion apparatus;
fig. 6 is a schematic view of the internal structure of the extruded tube.
In the drawings, the components represented by the respective reference numerals are listed below:
11. a steel platform; 12. a polymerization apparatus; 13. a first motor; 14. a preheating tank; 15. a quenching device; 16. an extrusion device; 21. a reaction tube; 22. a first feeding pipe; 23. an electrode; 24. a drive shaft; 25. a carbon brush; 26. an I-shaped mounting seat; 27. a solvent tube; 28. an electric heating tube; 29. a first discharging pipe; 31. a cooling tank; 32. a gas collecting pipe; 33. cooling out the pipe; 34. cleaning the tube; 35. a second feed pipe; 36. cooling the inlet pipe; 37. a throttle valve; 38. installing an axle tube; 39. a second discharge pipe; 41. a material flow passage; 42. a cooling flow channel; 51. extruding a pipe; 61. a third feeding pipe; 62. a screw extruder; 63. a water outlet pipe; 64. a shell and tube heat exchanger; 65. and (4) a water inlet pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, a high-efficiency and safe cyanate ester polymerization apparatus includes a steel platform 11, a preheating tank 14 is disposed on the top of the steel platform 11, a plurality of polymerization devices 12 are communicated below the preheating tank 14, the polymerization devices 12 are all fixedly connected to the steel platform 11 through a truss, a quenching device 15 is disposed below the polymerization devices 12, and an extrusion device 16 is disposed below the quenching device 15;
the polymerization device 12 comprises a reaction tube 21 and a heater arranged in the reaction tube 21, wherein a driving shaft 24 is fixed at the top of the heater, the driving shaft 24 penetrates through the top wall of the reaction tube 21, the driving shaft 24 is rotatably installed with the reaction tube 21 through a sealing bearing seat, a carbon brush 25 is fixed on the peripheral side wall of the driving shaft 24, an electrode 23 is arranged on a steel platform 11, the heater is powered by the carbon brush 25, a driven gear is fixed at the top end of the driving shaft 24, a first motor 13 is arranged on the bottom surface of the steel platform 11, a driving gear is fixed at the output end of the first motor 13 and is in meshing transmission connection with the driven gear through a chain, the heater comprises an I-shaped installation seat 26 and a plurality of electric heating tubes 28 fixed between the I-shaped installation seats 26, the electric heating tubes 28 are electrically connected with the carbon brush 25 to enable the heater to rotate and supply power, and stirring and heating are carried out from the middle part of the reaction tube 21, the phenomenon that the traditional side wall heating type polymerization kettle is locally heated at the near layer of the inner wall to cause over-reaction, so that a polymer with higher viscosity is formed and the heat exchange of the polymer is influenced is avoided.
The two sides of the upper side wall of the reaction tube 21 are respectively provided with a first feeding tube 22 and a solvent tube 27 for feeding molten material and introducing solvent, and the bottom wall of the reaction tube 21 is provided with a first discharging tube 29 for discharging mixed material.
The wall of the reaction tube 21 is provided with a heat insulating material, so that heat loss is reduced and energy consumption is reduced during continuous polymerization reaction.
The quenching device 15 comprises a plurality of cooling unit, and every cooling unit includes cooling tank 31 and sets up in the installation central siphon 38 at cooling tank 31 center, is provided with the baffle between the inner wall of cooling tank 31 and the side wall all around of installation central siphon 38, separates the inner chamber of cooling tank 31 for cooling runner 42 and material runner 41, cooling runner 42 and material runner 41 are the heliciform, and cooling runner 42 and material runner 41 distribute in turn, and the roof of cooling tank 31 is provided with second feed pipe 35, and the diapire of cooling tank 31 is provided with second row material pipe 39, and second feed pipe 35 and second row material pipe 39 all communicate with material runner 41, and one side of cooling tank 31 is provided with the cooling and advances pipe 36, and the opposite side of cooling tank 31 is provided with cooling exit tube 33, and cooling exit tube 36 and cooling exit tube 33 all communicate with cooling runner 42.
The cooling outlet pipe 33 is positioned at one side close to the second feeding pipe 35, and the cooling inlet pipe 36 is positioned at one side close to the second discharging pipe 39, so that the refrigerant and the mixture form convection, and the heat exchange efficiency is higher.
One end of the cooling inlet pipe 36 is communicated with a throttle valve 37, the throttle valve 37 is communicated with a compressed refrigerant pipeline and used for controlling the pressure reduction and release of the compressed refrigerant, so that the refrigerant is vaporized and absorbs heat to cool the mixture, a flow meter is arranged in the cooling inlet pipe 36 and used for accurately monitoring the introduction amount of the compressed refrigerant and controlling the temperature reduction of the mixture, all cooling outlet pipes 33 are communicated with a gas collecting pipe 32, the gas collecting pipe 32 is communicated with compression equipment, the vaporized refrigerant is collected and is compressed and recycled by the compression equipment again.
A cleaning pipe 34 is provided on one side of each cooling tank 31, and when the reaction is stopped, a cleaning agent is introduced from the cleaning pipe 34 to clean the quenching device 15.
The width-depth ratio of the material flow passage 41 is 0.6:1, the width-depth ratio of the cooling flow passage 42 is 0.15:1, under the size, the refrigerant and the mixture fully exchange heat, and the cooling speed is high.
The number of spiral turns of the material flow passage 41 and the cooling flow passage 42 of each cooling unit is 5.
The extruding device 16 comprises an extruding pipe 51, a screw extruder 62 is arranged at one end of the extruding pipe 51, the feeding end of the screw extruder 62 is communicated with a third feeding pipe 61, the extruding end of the screw extruder 62 is communicated with a tubular heat exchanger 64, the bottom surface of the tubular heat exchanger 64 is communicated with a water inlet pipe 65, the top surface of the tubular heat exchanger 64 is communicated with a water outlet pipe 63, and when the extruding device is used for extruding, cooling water is introduced into the tubular cooler to further cool the mixture after rapid cooling to a collecting temperature.
The first feeding pipe 22 is connected with the preheating tank 14 through a pipeline, the first discharging pipe 29 is connected with the second feeding pipe 35 through a pipeline, and the second discharging pipe 39 is connected with the third feeding pipe 61 through a pipeline.
Every two groups of quenching devices 15 are communicated with one group of extrusion devices 16.
Electric valves and flowmeters are arranged in pipelines related to the polymerization equipment and are controlled by PLC programming.
Example 1
The embodiment of the present invention provides a bisphenol a cyanate ester resin, and the specific preparation process includes the following steps:
firstly, conveying a polymerization monomer raw material into a preheating tank 14 of polymerization equipment, heating to 122 ℃ (the raw material calibration melting temperature is 118 ℃), and stirring until the polymerization monomer is completely melted to obtain a molten material;
secondly, pumping the molten material into a polymerization device 12, driving a heater by a first motor 13 to stir the molten material and heat the molten material to 145 ℃, carrying out polymerization reaction by heat preservation and stirring until the polymerization degree reaches 1.56 (the target value is 1.58), stopping heating, pumping a solvent and stirring to obtain a mixture;
thirdly, discharging the mixture into a quenching tank, releasing the coolant into a cooling flow passage 42, rapidly cooling the mixture, and terminating the polymerization reaction;
and fourthly, sucking the mixture subjected to rapid temperature reduction into an extrusion device 16, slowly cooling to a collection temperature, extruding and storing.
Example 2
The embodiment of the present invention provides a bisphenol C type cyanate ester resin, and the specific preparation process includes the following steps:
firstly, conveying a polymerization monomer raw material into a preheating tank 14 of polymerization equipment, heating to 135 ℃ (the raw material calibration melting temperature is 128 ℃), and stirring until the polymerization monomer is completely melted to obtain a molten material;
secondly, pumping the molten material into a polymerization device 12, driving a heater by a first motor 13 to stir the molten material and heat the molten material to 160 ℃, preserving heat and stirring the molten material for polymerization reaction, stopping heating, pumping a solvent and stirring the mixture to obtain a mixture, wherein the polymerization degree reaches 1.52 (the target value is 1.57);
thirdly, discharging the mixture into a quenching tank, releasing the coolant into a cooling flow passage 42, rapidly cooling the mixture, and terminating the polymerization reaction;
and fourthly, sucking the mixture subjected to rapid temperature reduction into an extrusion device 16, slowly cooling to a collection temperature, extruding and storing.
The measured values of the cyanate ester prepolymer GT in example 1 and the measured value of the cyanate ester prepolymer GT in example 2 were 60min and 80min, respectively.
The working principle of the high-efficiency and safe cyanate ester polymerization equipment is as follows: adding a polymerization monomer into a preheating tank 14, heating the polymerization to be molten, wherein the polymerization reaction is not enough to occur at the temperature, but preheating the polymerization monomer to be molten, heating the polymerization monomer uniformly during polymerization, then discharging the polymerization monomer into a reaction tube 21, driving a heater by a first motor 13 to stir, enabling an electric brush to be in contact with an electrode 23 to supply power to an electric heating tube 28, enabling the heater to stir and heat the polymerization monomer in the middle of the reaction tube 21, then discharging the polymer into a material flow channel 41, introducing a compressed refrigerant into a cooling flow channel 42 through a throttle valve 37, rapidly absorbing heat during vaporization, rapidly cooling the polymer to enable the polymer to be lower than the polymerization temperature, thereby stopping the reaction, collecting and cooling the vaporized refrigerant by a gas collecting tube 32, recompressing the cooled refrigerant for cooling, extruding the quenched polymer into a tubular heat exchanger 64 through a screw extruder 62, and slowly cooling the polymer to the collection temperature through cooling water, and finally discharging and collecting to complete the cyanate ester polymerization.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (9)
1. A high-efficiency and safe cyanate ester polymerization device comprises a steel platform (11), wherein the top of the steel platform (11) is provided with a preheating tank (14), and is characterized in that a plurality of polymerization devices (12), a quenching device (15) and an extrusion device (16) are sequentially arranged below the preheating tank (14);
the quenching device (15) is composed of a plurality of cooling units, each cooling unit comprises a cooling tank (31) and an installation shaft tube (38) arranged in the center of the cooling tank (31), a partition plate is arranged between the inner wall of the cooling tank (31) and the peripheral side wall of the installation shaft tube (38), and the inner cavity of the cooling tank (31) is divided into a cooling flow channel (42) and a material flow channel (41).
2. The efficient and safe cyanate ester polymerization equipment according to claim 1, wherein the cooling flow channel (42) and the material flow channel (41) are spiral, and the cooling flow channel (42) and the material flow channel (41) are alternately distributed, the side wall of the cooling tank (31) where the cooling flow channel (42) is located is respectively communicated with a cooling inlet pipe (36) and a cooling outlet pipe (33), and the side wall of the cooling tank (31) where the material flow channel (41) is located is respectively communicated with a second feeding pipe (35) and a second discharging pipe (39).
3. The efficient and safe cyanate ester polymerization equipment according to claim 2, wherein the width-to-depth ratio of the material flow channel (41) is 0.5-0.7:1, and the width-to-depth ratio of the cooling flow channel (42) is 0.13-0.2: 1.
4. The efficient and safe cyanate ester polymerization equipment according to claim 2, wherein the number of spiral turns of the material flow passage (41) and the cooling flow passage (42) is 4-7.
5. The efficient and safe cyanate ester polymerization equipment according to claim 2, wherein one end of the cooling inlet pipe (36) is connected with a throttle valve (37), and the cooling outlet pipe (33) is connected with a gas collecting pipe (32).
6. The efficient and safe cyanate ester polymerization equipment according to claim 1, wherein said polymerization device (12) comprises a reaction tube (21) and a heater disposed inside the reaction tube (21), a driving shaft (24) rotatably mounted with the reaction tube (21) is fixed on top of the heater, and the driving shaft (24) is driven to rotate by a first motor (13) fixed on the top surface of the steel platform (11).
7. The efficient and safe cyanate ester polymerization equipment according to claim 6, wherein the circumferential side surface of the driving shaft (24) is fixed with a carbon brush (25) electrically connected with the heater, and the steel platform (11) is provided with an electrode (23) matched with the carbon brush (25).
8. The efficient and safe cyanate ester polymerization equipment according to claim 1, wherein the extruding device (16) comprises an extruding pipe (51), one end of the extruding pipe (51) is provided with a screw extruder (62), and the extruding end of the screw extruder (62) is communicated with a tubular heat exchanger (64).
9. An efficient and safe cyanate ester polymerization process is characterized by comprising the following steps:
firstly, conveying a polymerization monomer raw material into a preheating tank (14) of polymerization equipment, heating to a temperature 4-7 ℃ higher than the melting temperature of the polymerization monomer, and stirring until the polymerization monomer is completely melted to obtain a molten material;
secondly, pumping the molten material into a polymerization device (12), driving a heater by a first motor (13) to stir the molten material and heat the molten material to a polymerization temperature, carrying out polymerization reaction by heat preservation and stirring, stopping heating when the polymerization degree is lower than a target value of 0.02-0.05/105 ℃, pumping a solvent and stirring to obtain a mixture;
thirdly, discharging the mixture into a quenching tank, releasing a coolant into a cooling flow channel (42), rapidly cooling the mixture, and terminating the polymerization reaction;
and fourthly, sucking the mixture subjected to rapid temperature reduction into an extrusion device (16), slowly cooling to a collection temperature, extruding and storing.
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