Fiber-grade LCP (Liquid Crystal Polymer) continuous flow synthesis system
By combining solution polycondensation and melt polymerization with a fiber-grade LCP continuous flow synthesis system, the problem of low efficiency in traditional batch reactors has been solved, achieving efficient and uniform resin production suitable for large-scale industrial production.
Patent Information
- Application Number
- CN202423100667.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-16
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2034-12-16
AI Technical Summary
Traditional batch reactors are difficult to use for continuous production, resulting in low LCP resin production efficiency, affecting product purity and quality, and making it difficult to precisely control the reaction temperature.
A fiber-grade LCP continuous flow synthesis system is adopted, including a raw material storage system, a prepolymerization system, a separation system, and a polycondensation system. It utilizes equipment such as microchannel mixers, continuous flow microchannel reactors, and continuous polycondensation reactors, combined with solution polycondensation and melt polymerization, to achieve continuous production and efficient control.
It improves the uniformity and purity of resin molecular weight, meets the production requirements of fiber-grade resin, is suitable for large-scale continuous industrial preparation, avoids the scale-up effect of traditional reactors, and improves production efficiency and product quality.
Smart Images
Figure CN223945627U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to LCP resin poly field, concretely relates to a kind of fiber grade LCP continuous flow synthesis system. BACKGROUND
[0002] LCP fiber is mainly prepared by using fiber grade resin through melt extrusion process, which makes molecules orient along the fiber axis, so that the fiber has high toughness, high wear resistance, flame resistance, chemical resistance (acid, alkali, organic solvent) and lower yarn abrasion degree.
[0003] At present, LCP resin polymerization method is mainly melt polycondensation, and high molecular weight products are prepared by solid phase polycondensation for most aromatic LCP, and one-step or two-step melt polymerization is usually used for non-aromatic LCP. Most of the melt polycondensation is carried out in a kettle reactor. The traditional kettle reactor has mature equipment technology, controllable equipment investment, simple operation process and control technology, but it is difficult to realize continuous production, the efficiency is low, and it is difficult to accurately control the reaction temperature during the reaction process, and there are many by-products in the product, which seriously affects the purity and quality of the product. UTILITY MODEL CONTENT
[0004] In order to overcome the above-mentioned shortcomings, the purpose of the utility model is to provide a kind of fiber grade LCP continuous flow synthesis system.
[0005] In order to achieve the above purpose, the utility model adopts the technical scheme at least including raw material storage system, prepolymerization system, separation system and polycondensation system, wherein the raw material storage system, the prepolymerization system and the separation system are connected in sequence, and the separation system is connected with the polycondensation system and the raw material storage system respectively; the raw material storage system includes benzene ring-containing monomer raw material storage tank, naphthalene ring-containing monomer raw material storage tank and esterification reaction catalyst raw material storage tank, and the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification reaction catalyst raw material storage tank are connected with the prepolymerization system through conveying pipeline respectively.
[0006] In the preferred technical scheme of the above fiber grade LCP continuous flow synthesis system, the prepolymerization system includes microchannel mixer and continuous flow microchannel reactor connected in sequence, and the polycondensation system includes continuous polycondensation reaction kettle and storage tank connected in sequence.
[0007] In the preferred technical scheme of the above fiber grade LCP continuous flow synthesis system, the separation system at least includes gas-solid separator connected with the continuous flow microchannel reactor and the continuous polycondensation reaction kettle respectively, and includes solvent storage tank for connecting the gas-solid separator and the raw material storage system.
[0008] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the inner wall of the continuous flow microchannel reactor is provided with an ultrasonic generator.
[0009] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the continuous flow microchannel reactor and the gas-solid separator are both externally provided with a temperature control jacket.
[0010] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the polycondensation system further comprises a material tank connected with the continuous polycondensation reactor, and the material tank is capable of supplying a polycondensation catalyst to the continuous polycondensation reactor.
[0011] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the continuous polycondensation reactor is internally provided with a multi-stage stirring device.
[0012] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification reaction catalyst raw material storage tank are all provided with a liquid level meter.
[0013] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification reaction catalyst raw material storage tank are all provided with a stirring mechanism.
[0014] In the preferred technical scheme of the fibre-grade LCP continuous flow synthesis system, the raw material storage system further comprises a metering pump, and the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification reaction catalyst raw material storage tank are respectively connected with the prepolymerization system through the metering pump and the conveying pipeline.
[0015] The fibre-grade LCP continuous flow synthesis system has the advantages that the fibre-grade LCP continuous flow synthesis system combines the advantages of solution polycondensation and melt polymerization, utilizes solution polymerization to prepare a pre-polymer with uniform molecular weight, and then utilizes solid-phase melt polycondensation, so that the molecular weight of the resin is greatly improved, the molecular weight purity of the synthetic resin is high and uniform, the production requirements of the fibre-grade resin are met, the continuous flow microchannel reactor of the fibre-grade LCP continuous flow synthesis system has no amplification effect, and the fibre-grade LCP resin can be continuously prepared on an industrial scale. BRIEF DESCRIPTION OF DRAWINGS
[0016] Figure 1 The fibre-grade LCP continuous flow synthesis system has the advantages that the fibre-grade LCP continuous flow synthesis system combines the advantages of solution polycondensation and melt polymerization, utilizes solution polymerization to prepare a pre-polymer with uniform molecular weight, and then utilizes solid-phase melt polycondensation, so that the molecular weight of the resin is greatly improved, the molecular weight purity of the synthetic resin is high and uniform, the production requirements of the fibre-grade resin are met, the continuous flow microchannel reactor of the fibre-grade LCP continuous flow synthesis system has no amplification effect, and the fibre-grade LCP resin can be continuously prepared on an industrial scale.
[0017] In the figure: raw material storage system 1, benzene ring containing monomer raw material tank 11, naphthalene ring containing monomer raw material tank 12, esterification reaction catalyst raw material tank 13, stirring mechanism 14, metering pump 15, micro-channel mixer 21, continuous flow micro-channel reactor 22, gas-solid separator 31, solvent tank 32, continuous polycondensation reactor 41, multi-stage stirring device 411, storage tank 42, material tank 43. DETAILED DESCRIPTION
[0018] The preferred embodiments of the present application will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present application, and are not intended to limit the protection scope of the present application.
[0019] It should be noted that in the description of the present application, the terms "upper", "lower", "left", "right", "front", "back" and other terms indicating direction or positional relationship are based on the direction or positional relationship shown in the drawings, which is only for the convenience of description, and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present application. In addition, the terms "first", "second" are only for descriptive purposes and cannot be understood as indicating or implying relative importance.
[0020] In addition, it should also be noted that in the description of the present application, unless otherwise explicitly specified and limited, the terms "provided", "connected", "connected" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or it can be integrally connected. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.
[0021] As Figure 1 shown, the fiber-grade LCP continuous flow synthesis system of the present application at least includes a raw material storage system 1, a prepolymerization system, a separation system and a polycondensation system, wherein the raw material storage system 1, the prepolymerization system and the separation system are connected in sequence, and the separation system is connected with the polycondensation system and the raw material storage system 1 respectively; the raw material storage system 1 includes a benzene ring containing monomer raw material tank 11, a naphthalene ring containing monomer raw material tank 12 and an esterification reaction catalyst raw material tank 13, and the benzene ring containing monomer raw material tank 11, the naphthalene ring containing monomer raw material tank 12 and the esterification reaction catalyst raw material tank 13 are connected with the prepolymerization system through the conveying pipeline respectively.
[0022] Referring to Figure 1The raw material storage system 1 is used for storing raw materials required for LCP synthesis, including benzene ring-containing monomers, naphthalene ring-containing monomers and esterification catalysts, and is used for supplying the raw materials to a prepolymerization system, the prepolymerization system is used for performing prepolymerization on a resin solution, a separation system is used for heating and separating the organic solvent and the prepolymer resin transmitted by the prepolymerization system, and a polycondensation system is used for further performing melt polycondensation reaction on the prepolymer resin separated by the separation system, so as to increase the molecular weight of the resin, and make the synthesized resin have uniform molecular weight, high purity and good quality.
[0023] Specifically, when the fiber-grade LCP resin is prepared, the benzene ring-containing monomers, the naphthalene ring-containing monomers and the esterification catalysts stored in the benzene ring-containing monomer raw material storage tank 11, the naphthalene ring-containing monomer raw material storage tank 12 and the esterification catalyst raw material storage tank 13 are proportionally transported to the prepolymerization system, the prepolymerization system cuts and performs prepolymerization on the resin solution to synthesize a prepolymer mixture with uniform molecular weight, then the prepolymer mixture is pumped into the separation system, the separation system controls the temperature to be above the boiling point of the organic solvent and below the melting point of the LCP prepolymer, so as to evaporate the organic solvent in the prepolymer mixture, the evaporated organic solvent is recycled and stored through condensation reflux, and the unevaporated LCP prepolymer is heated and melted and then pumped into the polycondensation system, the polycondensation system performs polycondensation on the prepolymer to form the fiber-grade LCP resin, and the fiber-grade LCP resin can be stored and preserved after being prepared.
[0024] The fiber-grade LCP continuous flow synthesis system of the present application combines the advantages of solution polycondensation and melt polymerization, utilizes solution polymerization to prepare a prepolymer with uniform molecular weight, and then utilizes solid-phase melt polycondensation, which greatly increases the molecular weight of the resin, so that the synthesized resin has high molecular weight, high purity and uniformity, and meets the production requirements of fiber-grade resin. In addition, compared with the amplification effect of the traditional reaction kettle, the prepolymerization system of the present application has no amplification effect and is suitable for industrialized large-scale continuous preparation of fiber-grade LCP resin.
[0025] In one or more embodiments, the prepolymerization system comprises a microchannel mixer 21 and a continuous flow microchannel reactor 22 connected in sequence, and the polycondensation system comprises a continuous polycondensation kettle 41 and a storage tank 42 connected in sequence.
[0026] Referring to Figure 1 The microchannel mixer 21 has three liquid inlets and one liquid outlet, the three liquid inlets are respectively used for connecting the benzene ring-containing monomer raw material storage tank 11, the naphthalene ring-containing monomer raw material storage tank 12 and the esterification catalyst raw material storage tank 13, and the liquid outlet is used for connecting the continuous flow microchannel reactor 22, and the outlet of the continuous flow microchannel reactor 22 is connected to the separation system.
[0027] Specifically, when the fiber grade LCP resin is prepared, the benzene ring containing monomer, the naphthalene ring containing monomer and the esterification reaction catalyst stored in the benzene ring containing monomer raw material storage tank 11, the naphthalene ring containing monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 are proportionally transported into the micro-channel mixer 21. The micro-structure units of the micro-channel mixer 21 cut the reaction fluid flowing therethrough to realize sufficient mixing and contact between the reactants in a micron or even smaller space, improve the conversion rate of the raw materials, avoid the problems of incomplete dissolution and insufficient mixing of the materials during the synthesis of the LCP resin, and the raw materials after sufficient mixing are transported into the continuous flow micro-channel reactor 22 for resin dissolution and prepolymerization. In the continuous flow micro-channel reactor 22, the raw materials after sufficient mixing are subjected to prepolymerization to synthesize a prepolymer mixture with uniform molecular weight. Then, the prepolymer mixture is pumped into a separation system. The separation system controls the temperature to be above the boiling point of the organic solvent and below the melting point of the LCP prepolymer, so as to evaporate the organic solvent in the prepolymer mixture. The evaporated organic solvent is recycled and stored by condensation reflux. The LCP prepolymer that is not evaporated is heated and melted and then pumped into the continuous polycondensation reactor 41. The polycondensation catalyst is added to the continuous polycondensation reactor 41 and the continuous polycondensation reactor 41 is subjected to vacuum and temperature rising treatment to perform melt polycondensation reaction. The LCP prepolymer is subjected to polycondensation in the continuous polycondensation reactor 41 to obtain the fiber grade LCP resin. Then, the fiber grade LCP resin is pumped into the storage tank 42.
[0028] In one or more embodiments, the separation system at least includes a gas-solid separator 31 connected to the continuous flow micro-channel reactor 22 and the continuous polycondensation reactor 41 respectively, and a solvent storage tank 32 for connecting the gas-solid separator 31 and the raw material storage system 1.
[0029] Referring to Figure 1 , the separation system includes the gas-solid separator 31 and the solvent storage tank 32. The inlet of the gas-solid separator 31 is connected to the outlet of the continuous flow micro-channel reactor 22. The gas-solid separator 31 has two outlets and is connected to the inlet of the continuous polycondensation reactor 41 and the inlet of the solvent storage tank 32 respectively. The solvent storage tank 32 is used to recycle the organic solvent evaporated from the continuous polycondensation reactor 41. The solvent storage tank 32 is connected to the benzene ring containing monomer raw material storage tank 11, the naphthalene ring containing monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 through pipelines respectively, so as to proportionally pump the organic solvent into the benzene ring containing monomer raw material storage tank 11, the naphthalene ring containing monomer raw material storage tank 12 or the esterification reaction catalyst raw material storage tank 13. The gas-solid separator 31 can heat the prepolymer mixture therein. The heating temperature is above the boiling point of the organic solvent and below the melting point of the LCP prepolymer, so as to evaporate the organic solvent in the prepolymer mixture and recycle the evaporated organic solvent to the solvent storage tank 32 by condensation reflux. The organic solvent is recycled, which greatly saves the cost and avoids the problems of waste and pollution caused by the volatilization of the organic solvent.
[0030] In one or more embodiments, the inner wall of the continuous flow microchannel reactor 22 is configured with an ultrasonic generator; both the continuous flow microchannel reactor 22 and the gas-solid separator 31 are externally configured with a temperature control jacket.
[0031] Referring to Figure 1 , the ultrasonic generator can perform ultrasonic mixing on the raw materials in the continuous flow microchannel reactor 22, disperse and stir the raw materials using ultrasonic waves, accelerate the prepolymerization reaction, avoid unnecessary side reactions, and increase the regularity of the resin structure. At the same time, the ultrasonic effect can reduce the adhesion of the raw materials to the wall of the continuous flow microchannel reactor 22, reduce the possibility of raw material blockage of the pipeline, and reduce the maintenance frequency of the continuous flow microchannel reactor 22.
[0032] In addition, the temperature control jacket is configured outside the continuous flow microchannel reactor 22 to control the temperature required for the prepolymerization reaction, so that the molecular weight of the synthesized prepolymer mixture is more uniform; the temperature control jacket is configured outside the gas-solid separator 31 to control the boiling point required for the evaporation of the organic solvent, to ensure the smooth evaporation of the organic solvent in the prepolymer mixture.
[0033] In one or more embodiments, the polycondensation system further comprises a material tank 43 connected to the continuous polycondensation reactor 41, which can supply the polycondensation catalyst to the continuous polycondensation reactor 41.
[0034] Referring to Figure 1 , the material tank 43 is used to store the polycondensation catalyst, that is, the polycondensation catalyst is stored in the material tank 43, the outlet of the material tank 43 is connected to the inlet of the continuous polycondensation reactor 41 through a pipeline, and a pump body is arranged on the pipeline to automatically pump the catalyst into the continuous polycondensation reactor 41, realizing automatic feeding of the catalyst.
[0035] In one or more embodiments, the continuous polycondensation reactor 41 is internally configured with a multi-stage stirring device 411.
[0036] Referring to Figure 1 , the multi-stage stirring device 411 can be a stirring rod and a plurality of blades arranged on the stirring rod in the height direction; the prepolymer mixture in the continuous polycondensation reactor 41 is stirred by the multi-stage stirring device 411 to further break the polymer, avoid the problem of mass transfer after the viscosity of the polymer rises sharply, and ensure uniform molecular weight distribution and high intrinsic viscosity of the polymer.
[0037] In one or more embodiments, liquid level meters are arranged on the benzene ring-containing monomer raw material storage tank 11, the naphthalene ring-containing monomer raw material storage tank 12, and the esterification reaction catalyst raw material storage tank 13.
[0038] The liquid level meter is not shown in the drawings, and the liquid level meters configured on the benzene ring monomer raw material storage tank 11, the naphthalene ring monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 are used to monitor the raw material liquid level in each raw material storage tank, so as to avoid the problem that the raw materials in each raw material storage tank are too much and difficult to stir.
[0039] In one or more embodiments, the benzene ring monomer raw material storage tank 11, the naphthalene ring monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 are each provided with a stirring mechanism 14.
[0040] Referring to Figure 1 The stirring mechanism 14 can be a rotating shaft controlled by a servo motor and stirring blades arranged on the rotating shaft. By arranging the stirring mechanism 14 in the above-mentioned raw material storage tank, the raw materials in each raw material storage tank can be effectively mixed and dissolved.
[0041] In one or more embodiments, the raw material storage system 1 further comprises a metering pump 15, and the benzene ring monomer raw material storage tank 11, the naphthalene ring monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 are respectively connected to the prepolymerization system through the metering pump 15 and the conveying pipeline.
[0042] Referring to Figure 1 When the benzene ring monomer raw material storage tank 11, the naphthalene ring monomer raw material storage tank 12 and the esterification reaction catalyst raw material storage tank 13 are respectively connected to the three liquid inlets of the micro-channel mixer 21 through the conveying pipelines in turn, a metering pump 15 is arranged on each conveying pipeline to control the raw material amount ratio pumped into the micro-channel mixer 21 from each raw material storage tank, so as to ensure the effect of synthesizing the fiber-grade LCP resin.
[0043] The above embodiments are only for illustrating the technical concept and characteristics of the present application, and the purpose is to enable those skilled in the art to understand the content of the present application and implement it, and cannot limit the protection scope of the present application. Any equivalent changes or modifications made according to the spirit and essence of the present application should be covered within the protection scope of the present application.
Claims
1. A continuous flow system for the synthesis of fiber grade LCP, characterized in that, The system comprises a raw material storage system, a prepolymerization system, a separation system and a polycondensation system, wherein the raw material storage system, the prepolymerization system and the separation system are connected in sequence, and the separation system is connected with the polycondensation system and the raw material storage system respectively; The prepolymerization system comprises a microchannel mixer and a continuous flow microchannel reactor connected in sequence, and the polycondensation system comprises a continuous polycondensation reactor and a storage tank connected in sequence; The separation system comprises a gas-solid separator connected with the continuous flow microchannel reactor and the continuous polycondensation reactor respectively, and a solvent storage tank for connecting the gas-solid separator and the raw material storage system; The polycondensation system further comprises a material tank connected with the continuous polycondensation reactor, and the material tank is capable of supplying a polycondensation catalyst to the continuous polycondensation reactor; The raw material storage system comprises a benzene ring-containing monomer raw material storage tank, a naphthalene ring-containing monomer raw material storage tank and an esterification catalyst raw material storage tank, and the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification catalyst raw material storage tank are connected with the prepolymerization system through conveying pipelines respectively.
2. The continuous flow synthesis system of fiber grade LCP according to claim 1, characterized in that: The inner wall of the continuous flow microchannel reactor is provided with an ultrasonic generator.
3. The fiber-grade LCP continuous flow synthesis system of claim 1, wherein: The continuous flow microchannel reactor and the gas-solid separator are both provided with a temperature control jacket outside.
4. The fiber-grade LCP continuous flow synthesis system of claim 1, wherein: The continuous polycondensation reactor is provided with a multi-stage stirring device inside.
5. The fiber-grade LCP continuous flow synthesis system of claim 1, wherein: The benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification catalyst raw material storage tank are all provided with a liquid level meter.
6. The continuous flow synthesis system of fibre grade LCP according to claim 1 or 5, characterized in that: The benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification catalyst raw material storage tank are all provided with a stirring mechanism.
7. The fiber-grade LCP continuous flow synthesis system of claim 1, wherein: The raw material storage system further comprises a metering pump, and the benzene ring-containing monomer raw material storage tank, the naphthalene ring-containing monomer raw material storage tank and the esterification catalyst raw material storage tank are connected with the prepolymerization system through the metering pump and the conveying pipelines respectively.