Control system for continuous production of methacrylic acid series polymer

By combining a DCS controller and a group of sensors, the problem of controlling the reaction heat in the production of methacrylic polymers was solved, achieving automated production and dynamic equilibrium, and improving production efficiency and product quality.

CN223875023UActive Publication Date: 2026-02-06CHINA BLUESTAR CHENGRAND CO LTD +1
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Patent Information

Application Number
CN202520339243.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-02-28
Publication Date
2026-02-06
Estimated Expiration
2035-02-28

AI Technical Summary

Technical Problem

In existing methacrylic acid polymer production processes, the molecular weight and regularity of the polymerized raw material monomers cannot be effectively controlled, and the heat of reaction cannot be removed precisely, efficiently, and quickly. This results in the degree of polymerization and the heat of reaction influencing each other, affecting the conversion rate and production efficiency.

Method used

By employing a combination of DCS controller, sensor group, and equipment group, and through temperature sensor and heat transfer oil control loop, the reaction heat is accurately and efficiently removed. A temperature control loop is formed through electrical signal interlocking, which, together with the fully mixed reactor and segmented tubular reactor, controls the dynamic balance between polymerization conversion rate and reaction heat.

Benefits of technology

It has achieved automated control of the production of methacrylic polymers, reduced labor intensity, ensured production stability and controllability, maintained a dynamic balance between conversion rate and reaction heat, and improved production efficiency and product quality.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The utility model discloses a control system for continuous production of methacrylic acid polymers, and belongs to the technical field of production of methacrylic acid polymers. According to the control system, through the arrangement of the DCS controller, the sensor group, the equipment group and the like, automation of a methacrylic acid polymer production process is realized, the labor intensity is effectively reduced, and meanwhile, the stability, controllability and traceability of the methacrylic acid polymer production process are ensured; the systematic control and management are realized, so as to be matched with a methacrylic acid polymer production process; in particular, reaction heat is controlled to be moved out accurately, efficiently and quickly, and dynamic balance between the conversion rate and the reaction heat is ensured, so that continuous production of the methacrylic acid series polymer is matched.
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Description

TECHNICAL FIELD

[0001] The utility model relates to a control system of polymer production, especially to a control system of methacrylic polymer continuous production belongs to methacrylic polymer production technical field. BACKGROUND

[0002] ‌Methacrylic polymer is a kind of high molecular material with wide application prospect, is the high molecular compound formed by methacrylic acid or its derivative monomer through polymerization reaction. Methacrylic polymer has uniqueness in chemical structure, and the alkyl side chain is methyl instead of hydrogen atom, and the polymer usually has higher transparency, good weathering resistance and other characteristics. Among them, polymethyl methacrylate (PMMA) is an important member of methacrylic polymer, and polymethyl methacrylate is also called organic glass or acrylic, which is a kind of high transparent, amorphous high molecular polymer.

[0003] At present, polymerization process mainly includes:

[0004] I. Suspension polymerization method, with water as continuous phase, the viscosity of polymerization system is low, the viscosity of material changes little in the reaction process, has the advantages of easy removal of polymerization heat, easy control of temperature, safe production operation, short process flow etc. But due to the use of a large amount of water phase, the production capacity of suspension polymerization is low, which is not suitable for large-scale continuous production, and the preparation process needs filtering, washing, drying and other complicated procedures, so that the production efficiency is reduced, and there are problems of poor product purity and large amount of sewage etc.;

[0005] II. Solution polymerization method, the viscosity of polymerization system is low, and the mass transfer and heat transfer are easy to control, the operation condition control is stable, large-scale, continuous production can be carried out, and there is no sewage treatment problem. But there are problems of complex recovery and treatment process of organic solvent, high cost and possible environmental pollution.

[0006] Third, the bulk polymerization method is suitable for continuous production, the product has high purity and transparency, the polymerization conversion rate is high, only a small amount of unreacted monomer needs to be recovered, and the energy consumption is low. However, due to the high viscosity of the polymerization system, the mass transfer and heat transfer control is difficult, and the equipment and process operation process are harsh, therefore, a large amount of research has been carried out, such as: the prior art CN102933610A discloses a "methyl methacrylate polymer production method", which is mainly based on the bulk polymerization process, and the final product is obtained by multi-stage series connection of a complete mixing reactor and a pipeline reactor; the prior art CN104955853A discloses a "method for producing a methyl methacrylate polymer composition and a molded product", first, the polymerization monomer and the auxiliary agent are supplied into the first complete mixing type reactor through the supply port of the reactor, then the reaction is carried out, and the obtained methyl methacrylate polymer composition is taken out through the discharge port of the second complete mixing type reactor; the prior art CN101338001A discloses a "continuous solution polymerization process for optical grade polymethyl methacrylate and the equipment used", wherein the equipment is composed of a refining distillation device, a polymerization reaction device, a two-stage devolatilization device and a wire drawing and granulation device; CN103130945A and CN103130946A both provide a PMMA continuous polymerization method, which adopts a three-completely-mixed-reactor series connection mode, and realizes the continuous production of polymethyl methacrylate by pre-polymerization, secondary polymerization and tertiary polymerization in turn.

[0007] Although the above-mentioned prior art all adopts the bulk polymerization method to produce the methyl methacrylate polymer, realizes the innovation and optimization of the polymerization process, but for the control of the conversion rate and the reaction heat in the polymerization process, generally, the reaction section or the equipment is increased to control the conversion rate in each section or equipment, and finally the reaction heat is reduced, that is, there is still a technical problem:

[0008] The molecular weight and regularity of the raw material monomer after polymerization cannot be effectively controlled, the reaction heat cannot be accurately, efficiently and quickly removed, and the polymerization degree and the reaction heat are mutually influenced, that is, the higher the reaction polymerization conversion rate is, the higher the reaction heat is; on the contrary, if the reaction heat is not removed in time, the polymerization rate will be accelerated and the conversion rate will be increased, and finally the effective production of the methyl methacrylate polymer cannot be realized; in addition, in the current methyl methacrylate polymer production process, the heat cannot be dynamically and controllably removed quickly, and the reaction rate cannot be maintained in the opposite direction, that is, the automatic control technology is still blank.

[0009] Therefore, a control system for the production of the methyl methacrylate polymer, which can control the rapid heat removal, regulate the dynamic balance between the polymerization conversion rate and the reaction heat, and can be better matched with the methyl methacrylate polymer production process, is needed. SUMMARY

[0010] In order to overcome the deficiencies of the prior art, a control system for continuous production of methacrylic polymers is proposed. In the technical solution, through the setting of a DCS controller, a sensor group and a device group, not only is the automation of the methacrylic polymer production process realized, effectively reducing labor intensity, but also the stability, controllability and traceability of the methacrylic polymer production process are ensured; and systematic control and management are realized to cooperate with the methacrylic polymer production process; among them, especially the precise, efficient and rapid removal of reaction heat is controlled, and the dynamic balance between conversion rate and reaction heat is ensured to cooperate with the continuous production of methacrylic polymers.

[0011] In order to achieve the above technical purpose, the following technical solution is proposed:

[0012] The technical solution aims to provide a control system for continuous preparation of methacrylic polymers, which is arranged in a production system of methacrylic polymers, and comprises a DCS controller, a human-machine interface connected to the DCS controller through a data input interface, a data acquisition unit connected to the DCS controller through a data feedback interface, and an execution unit connected to the DCS controller through a data output interface.

[0013] The DCS controller comprises a batching control module, a prepolymerization control module and a polymerization control module.

[0014] The data acquisition unit is arranged in the production system of methacrylic polymers, and comprises a sensor group for data acquisition and transmission in the production process of methacrylic polymers.

[0015] The execution unit is arranged in the production system of methacrylic polymers, and comprises a device group for preparation and regulation of methacrylic polymers.

[0016] The DCS controller receives information of batching process and its regulation, information of prepolymerization process and its regulation, information of polymerization process and its regulation, information of waste treatment process and its regulation, and safety warning information from the human-machine interface, and receives batching process information, prepolymerization process information, polymerization process information, waste treatment process information and safety warning information from the data acquisition unit, completes information analysis, comparison and judgment, issues data acquisition instructions through the data acquisition unit, and issues execution instructions through the execution unit.

[0017] Human-machine interface: input information of completing the ingredient process and its regulation, the prepolymerization process and its regulation, the polymerization process and its regulation, the waste treatment process and its regulation, and safety warning information. For the arrangement on the human-machine interface, multifunctional tables, corresponding identification icons, switch control keys, regulation control keys, etc. can be provided;

[0018] Data acquisition unit: receive data acquisition instructions issued by the DCS controller, complete the collection and transmission of the ingredient process and its regulation information, the prepolymerization process and its regulation information, the polymerization process and its regulation information, the waste treatment process and its regulation information, and safety warning information, and feedback to the DCS controller;

[0019] Execution unit: complete the instructions issued by the DCS controller.

[0020] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0021] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0022] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0023] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0024] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0025] Further, the sensor group includes a methyl alkyl acrylate monomer metering pump, an alkyl acrylate monomer metering pump, a (methyl) cyclic acrylate monomer metering pump, and an oxygen content analyzer connected with the ingredient control module;

[0026] The alkyl methacrylate monomer metering pump and the alkyl methacrylate monomer feeding control valve are interlocked by electric signals, and the alkyl methacrylate monomer metering pump, the feeding control module and the alkyl methacrylate monomer feeding control valve form an alkyl methacrylate monomer feeding control loop by electric signals;

[0027] The alkyl acrylate monomer metering pump and the alkyl acrylate monomer feeding control valve are interlocked by electric signals, and the alkyl acrylate monomer metering pump, the feeding control module and the alkyl acrylate monomer feeding control valve form an alkyl acrylate monomer feeding control loop by electric signals;

[0028] The (methyl) cyclic acrylate monomer metering pump and the (methyl) cyclic acrylate monomer feeding control valve are interlocked by electric signals, and the (methyl) cyclic acrylate monomer metering pump, the feeding control module and the (methyl) cyclic acrylate monomer feeding control valve form a (methyl) cyclic acrylate monomer feeding control loop by electric signals;

[0029] The solvent metering pump and the solvent feeding control valve are interlocked by electric signals, and the solvent metering pump, the feeding control module, the prepolymerization control module and the solvent feeding control valve form a solvent feeding control loop by electric signals;

[0030] The auxiliary agent metering pump I and the auxiliary agent feeding control valve I are interlocked by electric signals, and the auxiliary agent metering pump I, the feeding control module, the prepolymerization control module and the auxiliary agent feeding control valve I form an auxiliary agent feeding control loop in the prepolymerization process by electric signals;

[0031] The auxiliary agent metering pump II and the auxiliary agent feeding control valve II are interlocked by electric signals, and the auxiliary agent metering pump II, the feeding control module, the polymerization control module and the auxiliary agent feeding control valve II form an auxiliary agent feeding control loop in the polymerization process by electric signals;

[0032] The temperature sensor I, the temperature sensor II, the heat transfer material feeding control valve, the heat transfer material discharge control valve, the heat conducting oil feeding control valve I and the heat conducting oil discharge control valve I are interlocked by electric signals, and the temperature sensor I, the temperature sensor II, the prepolymerization control module, the heat transfer material feeding control valve, the heat transfer material discharge control valve, the heat conducting oil feeding control valve I and the heat conducting oil discharge control valve I form a prepolymerization temperature control loop by electric signals;

[0033] The temperature sensor III, the temperature sensor IV, the heat conducting oil feeding control valve II, the heat conducting oil discharge control valve II and the cold oil feeding control valve are interlocked by electric signals, and the temperature sensor III, the temperature sensor IV, the polymerization control module, the heat conducting oil feeding control valve II, the heat conducting oil discharge control valve II and the cold oil feeding control valve form a polymerization temperature control loop by electric signals.

[0034] Further, the equipment group further comprises a mixture delivery pump, a prepolymerization reaction system delivery pump and a reactant delivery pump, all of which are connected with the DCS controller.

[0035] Further, the equipment group further comprises a frequency converter arranged on the stirring device, and the stirring device is connected with the stirring motor through the frequency converter.

[0036] In addition, the DCS controller further comprises a deashing separation control module, a waste treatment module and an alarm control module, the deashing separation control module is connected with the polymerization control module, the waste treatment module is connected with the deashing separation control module, and the alarm control module is connected with the batching control module, the prepolymerization control module, the polymerization control module, the deashing separation control template and the waste treatment module.

[0037] In the technical solution, the number and more specific positions of the metering pumps, sensors, control valves and the like on the corresponding pipelines and / or equipment can be further limited according to actual requirements.

[0038] In the technical solution, the positional relationships such as "rear side of the station", "between", "on", "in", "above", "below", "bottom", "top", "from bottom to top", "one end", "the other end", "lower part" and the like are defined according to the actual use state, are conventional terms in the technical field, and are also conventional terms used by persons skilled in the art in the actual use process.

[0039] In the description of the technical solution, it should be noted that, unless otherwise explicitly specified and limited, the "arrangement" and "connection" should be understood in a broad sense, for example, can be fixedly connected, can be detachably connected, or integrally connected; can be mechanically connected, can be electrically connected; can be directly connected, can be indirectly connected through an intermediate medium, or can be connected inside two elements. For those skilled in the art, the specific meaning of the above terms in the utility model can be understood according to the specific circumstances.

[0040] By adopting the technical solution, the following beneficial technical effects are brought:

[0041] The utility model is set in the production system of methacrylic acid polymer, through the setting of DCS controller, sensor group and equipment group etc., can better cooperate with the continuous production process of methacrylic acid polymer ( for the production process of methacrylic acid polymer, the molecular weight and regularity of raw material monomer after polymerization cannot realize effective control, reaction heat cannot realize accurate, efficient and fast removal, and the polymerization degree and reaction heat are mutually influenced, the higher the reaction polymerization conversion rate is, the higher the reaction heat is, on the contrary, if reaction heat is not removed in time, it will accelerate the polymerization rate, increase the conversion rate, and finally cannot realize effective production of methacrylic acid polymer), not only guarantee the high degree of automation control of methacrylic acid polymer production system, low labor intensity, can effectively control manpower and other costs, guarantee the stability, controllability and traceability of methacrylic acid polymer preparation process, and through the accurate, efficient and fast removal of reaction heat, guarantee the dynamic balance between conversion rate and reaction heat, realize effective control to pre-polymerization reaction temperature and polymerization reaction temperature, cooperate with the continuous production of methacrylic acid polymer,

[0042] In the utility model, through the setting of temperature sensor I, temperature sensor II, heat removal material feeding control valve, heat removal material discharge control valve, heat conducting oil feeding control valve I and heat conducting oil discharge control valve I, temperature sensor I, temperature sensor II, pre-polymerization control module, heat removal material feeding control valve, heat removal material discharge control valve, heat conducting oil feeding control valve I and heat conducting oil discharge control valve I form pre-polymerization temperature control loop through electric signal between them;Among them, cooperate with the full-mixing reaction kettle, the temperature control coil of full-mixing reaction kettle realizes accurate, efficient and fast removal of reaction heat according to the mechanism of heat removal of heat removal material vaporization, finally, maintains the balance of polymerization conversion rate and reaction heat, guarantees the polymerization conversion rate in the control range, realizes the effective production of methacrylic acid polymer;

[0043] In the utility model, through the setting of temperature sensor III, temperature sensor IV, heat conducting oil feeding control valve II, heat conducting oil discharge control valve II and cold oil feeding control valve, temperature sensor III, temperature sensor IV, polymerization control module, heat conducting oil feeding control valve II, heat conducting oil discharge control valve II and cold oil feeding control valve form polymerization temperature control loop through electric signal between them;Among them, cooperate with the sectional type column reactor, concentrate multiple reaction sections in column reactor, realize concentrated efficient heat exchange through column heat exchanger structure, and control the conversion rate and polymerization degree of each polymerization reaction node in a relatively narrow range, realize accurate control, thereby realize effective control to the temperature of entire polymerization reaction node, guarantee the safety and reliability, continuous controllability of reaction process;

[0044] The methacrylic acid polymer production system can realize systematic control and management, fills the gap of the automatic control technology in the methacrylic acid polymer production process, and meets the industrialized mass production requirement. BRIEF DESCRIPTION OF DRAWINGS

[0045] Figure 1 The utility model relates to the working principle schematic diagram of production system,

[0046] Figure 2 The utility model relates to the equipment structure block diagram of production system,

[0047] Figure 3 The utility model relates to the structure schematic diagram of sectional type column pipe type reactor in production system,

[0048] Figure 4 The utility model is the control principle schematic diagram of control system,

[0049] Figure 5 It is the logic connection block diagram of control system in the utility model,

[0050] Figure 6 It is the working principle schematic diagram of control system in the utility model,

[0051] In the drawing, 1, mixed buffer tank, 100, alkyl methacrylate monomer feed pipe, 101, alkyl methacrylate monomer metering tank, 102, alkyl acrylate monomer feed pipe, 103, alkyl acrylate monomer metering tank, 104, (Meth) acrylic cyclic ester monomer feed pipe, 105, (Meth) acrylic cyclic ester monomer metering tank, 1066, protective gas inlet pipe I, 107, displacement gas outlet pipe, 108, mixed material conveying pipe,

[0052] 2, all mixed reaction kettle, 200, solvent feed pipe, 201, solvent metering tank, 202, additive feed pipe I, 203, additive metering tank, 204, protective gas inlet pipe II, 205, three-paddle stirring mechanism, 206, temperature control coil, 207, heat removal object inlet pipe, 208, heat removal object outlet pipe, 209, prepolymerization reaction system conveying pipe, 210, heating jacket, 211, heat conducting oil inlet pipe I, 212, heat conducting oil outlet pipe I,

[0053] 3, sectional type column pipe type reactor, 300, shell, 301, mixed flow unit, 302, column pipe reaction unit, 303, mixed flow cavity, 304, column pipe, 305, temperature control cavity, 306, additive feed pipe II, 307, heat conducting oil inlet pipe II, 308, heat conducting oil outlet pipe II, 309, heat conducting oil communication pipe, 310, reactant conveying pipe, 311, cold oil feed pipe,

[0054] 4, dehydrated and extruded integrated machine,

[0055] 5, protective gas storage tank;

[0056] 6, methacrylic polymer storage tank;

[0057] 7, monomer recovery device, 700, recycling pipe;

[0058] 8, DCS controller, 81, batch control module, 82, prepolymerization control module, 83, polymerization control module, 84, waste treatment module, 85, alarm control module, 86, ash separation control template;

[0059] 9, alkyl methacrylate monomer feed control valve, 10, alkyl methacrylate monomer metering pump, 11, alkyl acrylate monomer feed control valve, 12, alkyl acrylate monomer metering pump, 13, (Meth) acrylic acid cyclic ester monomer feed control valve, 14, (Meth) acrylic acid cyclic ester monomer metering pump, 15, protective gas feed control valve I, 16, oxygen content analyzer, 17, pressure sensor I, 18, temperature sensor I, 19, mixed material delivery pump, 20, solvent feed control valve, 22, solvent metering pump, 23, auxiliary feed control valve I, 24, auxiliary metering pump I, 25, protective gas feed control valve II, 26, heat transfer material feed control valve, 27, heat transfer material discharge control valve, 28, pressure sensor II, 29, temperature sensor II, 30, prepolymerization reaction system delivery pump, 31, heat transfer oil feed control valve I, 32, heat transfer oil discharge control valve I, 33, auxiliary feed control valve II, 34, auxiliary metering pump II, 35, heat transfer oil feed control valve II, 36, heat transfer oil discharge control valve II, 37, cold oil feed control valve, 38, reactant delivery pump, 39, pressure sensor III, 40, temperature sensor III, 41, pressure sensor IV, 42, temperature sensor IV. DETAILED DESCRIPTION

[0060] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0061] Embodiment 1

[0062] The present embodiment provides: a control system for continuous production of methacrylic polymers, such as Figure 2As shown, the production system for methacrylic acid polymers includes a mixing buffer tank 1, a fully mixed reactor 2, a segmented tubular reactor 3, and a deashing and extrusion machine 4 arranged in sequence. The mixing buffer tank 1, the fully mixed reactor 2, the segmented tubular reactor 3, and the deashing and extrusion machine 4 form a continuous pathway for the production of methacrylic acid polymers.

[0063] like Figure 4 As shown, the control system includes a DCS controller 8, which is connected to a human-machine interface through a data input interface, a data acquisition unit through a data feedback interface, and an execution unit through a data output interface.

[0064] The DCS controller 8 includes a batching control module 81, a pre-polymerization control module 82, and a polymerization control module 83 (e.g., ...). Figure 5 (as shown)

[0065] The data acquisition unit is installed in the production system of methacrylic polymers, and the data acquisition unit includes a group of sensors for data acquisition and transmission in the production process of methacrylic polymers.

[0066] The execution unit is located in the production system of methacrylic polymers, and the execution unit includes a group of equipment for the preparation and control of methacrylic polymers.

[0067] Example 2

[0068] Based on Example 1, this example further defines the sensor group and equipment group in order to better control the prepolymerization temperature in the fully mixed reactor 2 and ensure the dynamic balance between the prepolymerization conversion rate and the heat of reaction, and proposes a compatible fully mixed reactor 2 to further illustrate this technical solution.

[0069] like Figure 6 As shown, firstly, the total mixing reactor 2 is equipped with a stirring device, and a temperature control coil 206 is fitted on the stirring device. One end of the temperature control coil 206 is connected to a heat transfer material inlet pipe 207, and the other end is connected to a heat transfer material outlet pipe 208. The total mixing reactor 2 is fitted with a heating jacket 210 on the outside. The heat source in the heating jacket 210 is heat transfer oil. The inlet of the heating jacket 210 is connected to a heat transfer oil inlet pipe I 211, and the outlet of the heating jacket 210 is connected to a heat transfer oil outlet pipe I 212.

[0070] Secondly, sensor group: including pressure sensor I 117 and temperature sensor I 118 arranged on the mixing buffer tank 1, and pressure sensor II 228 and temperature sensor II 229 arranged on the full-mixing reactor 2, the pressure sensor I 117, the temperature sensor I 118, the pressure sensor II 228 and the temperature sensor II 229 are connected with the prepolymerization control module 82.

[0071] Device group: including heat transfer material feeding control valve 26 arranged on the heat transfer material inlet pipe 207, heat transfer material discharging control valve 27 arranged on the heat transfer material outlet pipe 208, heat transfer oil feeding control valve I 31 arranged on the heat transfer oil inlet pipe I 211, and heat transfer oil discharging control valve I 32 arranged on the heat transfer oil outlet pipe I 212, the heat transfer material feeding control valve 26, the heat transfer material discharging control valve 27, the heat transfer oil feeding control valve I 31 and the heat transfer oil discharging control valve I 32 are connected with the prepolymerization control module 82.

[0072] Finally, the temperature sensor I 118, the temperature sensor II 229, the heat transfer material feeding control valve 26, the heat transfer material discharging control valve 27, the heat transfer oil feeding control valve I 31 and the heat transfer oil discharging control valve I 32 are connected through electrical signals, and the temperature sensor I 118, the temperature sensor II 229, the prepolymerization control module 82, the heat transfer material feeding control valve 26, the heat transfer material discharging control valve 27, the heat transfer oil feeding control valve I 31 and the heat transfer oil discharging control valve I 32 form a prepolymerization temperature control loop through electrical signals.

[0073] Example 3

[0074] On the basis of example 1, in order to better control the polymerization temperature in the sectionalized column reactor 3, ensure the dynamic balance of polymerization conversion rate and reaction heat, the sensor group and the device group are further limited, and a suitable sectionalized column reactor 3 is proposed to further illustrate the technical solution.

[0075] As shown in Figure 6 , first, the sectionalized column reactor 3: as shown in Figure 3 , includes a shell 300 and at least two mixing units 301 and at least two column reactor units 302 arranged in the shell 300, the mixing units 301 and the column reactor units 302 are arranged at intervals and are distributed upwards in sequence; the lowermost mixing unit 301 is provided with a feeding port, and the uppermost column reactor unit 302 is provided with a discharging port, and a continuous passage for polymerization reaction is formed between the feeding port, the mixing unit 301, the column reactor unit 302 and the discharging port. The bottom column reactor unit 302 is connected with a heat transfer oil inlet pipe II 307, the top column reactor unit 302 is connected with a heat transfer oil outlet pipe II 308, and the upper column reactor unit 302 and the lower column reactor unit 302 are connected through a heat transfer oil communication pipe 309; and the column reactor unit 302 is further connected with a cold oil feeding pipe 311;

[0076] Secondly, sensor group: including pressure sensor III 39 and temperature sensor III 40 distributed on the mixed flow unit 301, and pressure sensor IV 41 and temperature sensor IV 42 distributed on the column reactor unit 302, the pressure sensor III 39, the temperature sensor III 40, the pressure sensor IV 41 and the temperature sensor IV 42 are connected with the polymerization control module 83.

[0077] Device group: including the heat conducting oil inlet control valve II 35 provided on the heat conducting oil inlet pipe II 307, the heat conducting oil discharge control valve II 36 provided on the heat conducting oil outlet pipe II 308 and the cold oil inlet control valve 37 provided on the cold oil inlet pipe 311, the heat conducting oil inlet control valve II 35, the heat conducting oil discharge control valve II 36 and the cold oil inlet control valve 37 are connected with the polymerization control module 83.

[0078] Finally, the temperature sensor III 40, the temperature sensor IV 42, the heat conducting oil inlet control valve II 35, the heat conducting oil discharge control valve II 36 and the cold oil inlet control valve 37 are connected through electrical signals, and the temperature sensor III 40, the temperature sensor IV 42, the polymerization control module 83, the heat conducting oil inlet control valve II 35, the heat conducting oil discharge control valve II 36 and the cold oil inlet control valve 37 form a polymerization temperature control loop through electrical signals.

[0079] Example 4

[0080] On the basis of examples 1-3, in order to better dosing, ensure the effective progress of subsequent reaction, and improve product quality, the sensor group and the device group are further limited, and the mixing buffer tank 1, the full-mixing reactor 2 and the sectional column reactor 3 are arranged to adapt, so as to further illustrate the technical scheme.

[0081] As shown in Figure 6 Firstly, the mixing buffer tank 1: the alkyl methacrylate monomer metering tank 101 is connected through the alkyl methacrylate monomer feeding pipe 100, the alkyl acrylate monomer metering tank 103 is connected through the alkyl acrylate monomer feeding pipe 102, the cyclic (meth) acrylate monomer metering tank 105 is connected through the cyclic (meth) acrylate monomer feeding pipe 104, and the protective gas storage tank 5 is connected through the protective gas inlet pipe I 106; the displacement gas outlet of the mixing buffer tank 1 is connected with the displacement gas outlet pipe 107;

[0082] The full-mixing reactor 2: the solvent metering tank 201 is connected through the solvent feeding pipe 200, the auxiliary agent metering tank 203 is connected through the auxiliary agent feeding pipe I 202, and the protective gas storage tank 5 is connected through the protective gas inlet pipe II 204;

[0083] The segmented tubular reactor 3: the mixing unit 301 is connected with the auxiliary agent feeding pipe II 306, the mixing unit 301 comprises a mixing cavity 303 which is communicated with the auxiliary agent feeding pipe II 306; the tubular reaction unit 302 in the segmented tubular reactor 3 comprises a tubular 304 which is arranged longitudinally, and a temperature control cavity 305 between the tubular 304 and the shell 300 is used for containing heat conducting oil, and a cold oil feeding pipe 311 is connected with the temperature control cavity 305;

[0084] Secondly, the sensor group: further comprising a methyl alkyl acrylate monomer metering pump 10 arranged on the methyl alkyl acrylate monomer feeding pipe 100, an alkyl acrylate monomer metering pump 12 arranged on the alkyl acrylate monomer feeding pipe 102, a (meth) cyclic acrylate monomer metering pump 14 arranged on the (meth) cyclic acrylate monomer feeding pipe 104, an oxygen content analyzer 16 arranged on the displacement gas outlet pipe 107, a solvent metering pump 22 arranged on the solvent feeding pipe 200, an auxiliary agent metering pump I 24 arranged on the auxiliary agent feeding pipe I 202, and an auxiliary agent metering pump II 34 arranged on the auxiliary agent feeding pipe II 306, the methyl alkyl acrylate monomer metering pump 10, the alkyl acrylate monomer metering pump 12, the (meth) cyclic acrylate monomer metering pump 14, the oxygen content analyzer 16, the solvent metering pump 22, the auxiliary agent metering pump I 24 and the auxiliary agent metering pump II 34 are all connected with the batching control module 81;

[0085] The solvent metering pump 22 and the auxiliary agent metering pump I 24 are connected with the prepolymerization control module 82;

[0086] The auxiliary agent metering pump II 34 is connected with the polymerization control module 83.

[0087] The equipment group: further comprising a methyl alkyl acrylate monomer feeding control valve 9 arranged on the methyl alkyl acrylate monomer feeding pipe 100, an alkyl acrylate monomer feeding control valve 11 arranged on the alkyl acrylate monomer feeding pipe 102, a (meth) cyclic acrylate monomer feeding control valve 13 arranged on the (meth) cyclic acrylate monomer feeding pipe 104, a protective gas feeding control valve I 15 arranged on the protective gas inlet pipe I 1066, a solvent feeding control valve 20 arranged on the solvent feeding pipe 200, an auxiliary agent feeding control valve I 23 arranged on the auxiliary agent feeding pipe I 202, a protective gas feeding control valve II 25 arranged on the protective gas inlet pipe II 204, and an auxiliary agent feeding control valve II 33 arranged on the auxiliary agent feeding pipe II 306, the methyl alkyl acrylate monomer feeding control valve 9, the alkyl acrylate monomer feeding control valve 11, the (meth) cyclic acrylate monomer feeding control valve 13, the protective gas feeding control valve I 15, the solvent feeding control valve 20, the auxiliary agent feeding control valve I 23 and the auxiliary agent feeding control valve II 33 are all connected with the batching control module 81;

[0088] The solvent feed control valve 20, the auxiliary agent feed control valve I 23 and the protective gas feed control valve II 25 are connected with the prepolymerization control module 82;

[0089] The auxiliary agent feed control valve II 33 is connected with the polymerization control module 83;

[0090] The alkyl methacrylate monomer metering pump 10 and the alkyl methacrylate monomer feed control valve 9 are connected through electrical signals, and the alkyl methacrylate monomer metering pump 10, the batching control module 81 and the alkyl methacrylate monomer feed control valve 9 form an alkyl methacrylate monomer feed control loop through electrical signals;

[0091] The alkyl acrylate monomer metering pump 12 and the alkyl acrylate monomer feed control valve 11 are connected through electrical signals, and the alkyl acrylate monomer metering pump 12, the batching control module 81 and the alkyl acrylate monomer feed control valve 11 form an alkyl acrylate monomer feed control loop through electrical signals;

[0092] The (methyl) cyclic acrylate monomer metering pump 14 and the (methyl) cyclic acrylate monomer feed control valve 13 are connected through electrical signals, and the (methyl) cyclic acrylate monomer metering pump 14, the batching control module 81 and the (methyl) cyclic acrylate monomer feed control valve 13 form a (methyl) cyclic acrylate monomer feed control loop through electrical signals;

[0093] The solvent metering pump 22 and the solvent feed control valve 20 are connected through electrical signals, and the solvent metering pump 22, the batching control module 81, the prepolymerization control module 82 and the solvent feed control valve 20 form a solvent feed control loop through electrical signals;

[0094] The auxiliary agent metering pump I 24 and the auxiliary agent feed control valve I 23 are connected through electrical signals, and the auxiliary agent metering pump I 24, the batching control module 81, the prepolymerization control module 82 and the auxiliary agent feed control valve I 23 form an auxiliary agent feed control loop in the prepolymerization process through electrical signals;

[0095] The auxiliary agent metering pump II 34 and the auxiliary agent feed control valve II 33 are connected through electrical signals, and the auxiliary agent metering pump II 34, the batching control module 81, the polymerization control module 83 and the auxiliary agent feed control valve II 33 form an auxiliary agent feed control loop in the polymerization process through electrical signals.

[0096] In addition, for the full-mixing reaction kettle 2, the equipment group further includes a frequency converter 43 arranged on the stirring device, and the stirring device is connected with a stirring motor 44 through the frequency converter 43. The frequency converter 43 is connected with the prepolymerization control module 82, and through the frequency converter 43, the DCS controller 8 controls the rotation frequency of the stirring motor 44, and further controls the rotation speed of the stirring device.

[0097] Embodiment 5

[0098] On the basis of Embodiments 1-4, in order to ensure effective, orderly and controllable conveying of materials in the production line, the present embodiment is further limited as follows:

[0099] The outflow port of the mixed buffer tank 1 is connected with the full-mixing reaction kettle 2 through a mixed material conveying pipe 108, the outflow port of the full-mixing reaction kettle 2 is connected with the sectional column reactor 3 through a prepolymerization reaction system conveying pipe 209, and the outflow port of the sectional column reactor 3 is connected with the deashing and extruding integrated machine 4 through a reaction material conveying pipe 310;

[0100] The equipment group further comprises a mixed material conveying pump 19 arranged on the mixed material conveying pipe 108, a prepolymerization reaction system conveying pump 30 arranged on the prepolymerization reaction system conveying pipe 209, and a reaction material conveying pump 38 arranged on the reaction material conveying pipe 310;

[0101] The mixed material conveying pump 19, the prepolymerization reaction system conveying pump 30 and the reaction material conveying pump 38 are all connected with the DCS controller 8.

[0102] Embodiment 6

[0103] On the basis of Embodiments 1-5, the present embodiment further limits the DCS controller 8 to further illustrate the technical solution.

[0104] As shown in Figure 5 , the DCS controller 8 further comprises a deashing and separating control module 86, a waste treatment module 84 and an alarm control module 85. The deashing and separating control module is connected with the polymerization control module 83, the waste treatment module 84 is connected with the deashing and separating control module, and the alarm control module 85 is connected with the batching control module 81, the prepolymerization control module 82, the polymerization control module 83, the deashing and separating control template 86 and the waste treatment module 84.

[0105] Embodiment 7

[0106] On the basis of Embodiments 1-6, the present embodiment provides a production system of a methacrylic polymer, as shown in Figures 1-2 , comprising a mixed buffer tank 1, a full-mixing reaction kettle 2, a sectional column reactor 3 and a deashing and extruding integrated machine 4.

[0107] The mixed buffer tank 1 is connected with the alkyl methacrylate monomer metering tank 101 through the alkyl methacrylate monomer feeding pipe 100, connected with the alkyl acrylate monomer metering tank 103 through the alkyl acrylate monomer feeding pipe 102, connected with the (meth) cyclic acrylate monomer metering tank 105 through the (meth) cyclic acrylate monomer feeding pipe 104, and connected with the protective gas storage tank 5 through the protective gas inlet pipe I 1066; the mixed buffer tank 1 is connected with the displacement gas outlet pipe 107; the mixed buffer tank 1 is connected with the full-mixing reaction kettle 2 through the mixed material conveying pipe 108.

[0108] The alkyl methacrylate monomer feeding pipe 100 is provided with the alkyl methacrylate monomer feeding control valve 9 and the alkyl methacrylate monomer metering pump 10, the alkyl acrylate monomer feeding pipe 102 is provided with the alkyl acrylate monomer feeding control valve 11 and the alkyl acrylate monomer metering pump 12, the (meth) cyclic acrylate monomer feeding pipe 104 is provided with the (meth) cyclic acrylate monomer feeding control valve 13 and the (meth) cyclic acrylate monomer metering pump 14; the protective gas inlet pipe I 1066 is provided with the protective gas feeding control valve I 15, the displacement gas outlet pipe 107 is provided with the oxygen content analyzer 16, the mixed buffer tank 1 is provided with the pressure sensor I 17 and the temperature sensor I 18, and the mixed material conveying pipe 108 is provided with the mixed material conveying pump 19.

[0109] The full-mixing reaction kettle 2 is provided on the back side of the working position of the mixed buffer tank 1, and is connected with the solvent metering tank 201 through the solvent feeding pipe 200, connected with the auxiliary agent metering tank 203 through the auxiliary agent feeding pipe I 202, and connected with the protective gas storage tank 5 through the protective gas inlet pipe II 204.

[0110] The full-mixing reaction kettle 2 is provided on the back side of the working position of the mixed buffer tank 1, and is connected with the solvent metering tank 201 through the solvent feeding pipe 200, connected with the auxiliary agent metering tank 203 through the auxiliary agent feeding pipe I 202, and connected with the protective gas storage tank 5 through the protective gas inlet pipe II 204.

[0111] The solvent feeding pipe 200 is provided with a solvent feeding control valve 20 and a solvent metering pump 22, the auxiliary agent feeding pipe I 202 is provided with an auxiliary agent feeding control valve I 23 and an auxiliary agent metering pump I 24; the protective gas feeding pipe II is provided with a protective gas feeding control valve II 25, the heat transfer material feeding pipe 207 is provided with a heat transfer material feeding control valve 26, and the heat transfer material discharging pipe 208 is provided with a heat transfer material discharging control valve 27; the full-mixing reaction kettle 2 is provided with a pressure sensor II 28 and a temperature sensor II 29; the prepolymerization reaction system conveying pipe 209 is provided with a prepolymerization reaction system conveying pump 30;

[0112] In addition, the full-mixing reaction kettle 2 is externally sleeved with a heating jacket 210, the heat source in the heating jacket 210 is high-temperature heat-conducting oil, the heating jacket 210 is connected with a heat-conducting oil feeding pipe I 211 at the inlet and connected with a heat-conducting oil discharging pipe I 212 at the outlet; the heat transfer material in the temperature control coil 206 is liquid feed, the gasification temperature of the heat transfer material at normal pressure is 5-10 ℃ higher than the set reaction temperature in the full-mixing reaction kettle 2, and the feeding temperature of the heat transfer material is 5-10 ℃ lower than the set reaction temperature, for example, when the set reaction temperature in the full-mixing reaction kettle 2 is 120 ℃, isopentyl alcohol with a boiling point of 131-132 ℃ can be selected; when the set reaction temperature in the full-mixing reaction kettle 2 is 132 ℃, isopentyl acetate with a boiling point of 142 ℃ can be selected; the heat-conducting oil feeding pipe I 211 is provided with a heat-conducting oil feeding control valve I 31, and the heat-conducting oil discharging pipe I 212 is provided with a heat-conducting oil discharging control valve I 32;

[0113] The sectional column-tube reactor 3 is arranged at the rear side of the working position of the full-mixing reaction kettle 2, and includes a shell 300 and at least two mixed-flow units 301 and at least two column-tube reaction units 302 arranged in the shell 300, the mixed-flow units 301 and the column-tube reaction units 302 are arranged in intervals and distributed upwards in sequence; the lowermost mixed-flow unit 301 is provided with a feeding port, and the uppermost column-tube reaction unit 302 is provided with a discharging port, and the continuous passage for polymerization reaction is formed between the feeding port, the mixed-flow unit 301, the column-tube reaction unit 302 and the discharging port;

[0114] Each mixed-flow unit 301 is connected with an auxiliary agent feeding pipe II 306, the bottom column-tube reaction unit 302 is connected with a heat-conducting oil feeding pipe II 307, the top column-tube reaction unit 302 is connected with a heat-conducting oil discharging pipe II 308, and the upper column-tube reaction unit 302 and the lower column-tube reaction unit 302 are connected through a heat-conducting oil communication pipe 309; the discharging port of the sectional column-tube reactor 3 is connected with the deashing and extruding integrated machine 4 through a reaction material conveying pipe 310;

[0115] The mixed-flow unit 301 includes a mixed-flow cavity 303 in communication with the auxiliary agent feeding pipe II 306, and the column-tube reaction unit 302 includes column tubes 304 arranged longitudinally, and a temperature control cavity 305 between the column tubes 304 and the shell 300 is used for containing heat-conducting oil;

[0116] Preferably, the temperature control cavity 305 is also connected with a cold oil feeding pipe 311, that is, both the heat conducting oil and the cold oil are integrated to comprehensively adjust the problems of the temperature control cavity 305, thereby effectively controlling the temperature in the tube 304 and ensuring the controllable performance of the reaction system;

[0117] The auxiliary feeding pipe II 306 is provided with an auxiliary feeding control valve II 33 and an auxiliary metering pump II 34, the heat conducting oil feeding pipe II 307 is provided with a heat conducting oil feeding control valve II 35, the heat conducting oil discharging pipe II 308 is provided with a heat conducting oil discharging control valve II 36, the cold oil feeding pipe 311 is provided with a cold oil feeding control valve 37, and the reactant conveying pipe 310 is provided with a reactant conveying pump 38; each mixing unit 301 is distributed with a pressure sensor III 39 and a temperature sensor III 40, and the tube reaction unit 302 is distributed with a pressure sensor IV 41 and a temperature sensor IV 42;

[0118] The deashing and extruding integrated machine 4 is arranged at the rear side of the work station of the sectional tube reaction device 3, the polymer outlet of the deashing and extruding integrated machine 4 is connected with the methacrylic polymer storage tank 6, the waste outlet of the deashing and extruding integrated machine 4 is connected with the monomer recycling device 7, and the monomer outlet of the monomer recycling device 7 is connected with the mixing buffer tank 1 through the recycling pipe 700.

[0119] The mixing buffer tank 1, the full-mixing reaction kettle 2, the sectional tube reaction device 3, the deashing and extruding integrated machine 4, and the methacrylic polymer storage tank 6 form a continuous path for the production of the methacrylic polymer.

[0120] Example 8

[0121] Based on the examples 1-7, the present example provides a production process of a methacrylic polymer, which comprises the following steps:

[0122] S1: feeding: the raw materials of the alkyl methacrylate monomer, the alkyl acrylate monomer, and the (methyl) cyclic acrylate monomer are added into the mixing buffer tank until the total volume of the raw materials accounts for 2 / 3-4 / 5 of the content volume of the mixing buffer tank, and then the feeding is stopped;

[0123] The raw materials are uniformly mixed to obtain a mixture; then, high-purity Ar or N2 is introduced into the mixing buffer tank to replace the gas in the mixing buffer tank;

[0124] In the mixing buffer tank, the oxygen content in each monomer raw material is ≤1 ppm; the alkyl methacrylate monomer accounts for 68-95% of the total mass of the monomer raw materials, the alkyl acrylate monomer accounts for 3-30%, and the (methyl) cyclic acrylate monomer accounts for 2-15%; the pressure is 20-50 KPa (gauge pressure), and the temperature is 20-50℃;

[0125] S2 prepolymerization: the gaseous displacement mixture, solvent and additives obtained from step S1 are added to a full-mixing reactor, which is heated to 90-140°C at a rate of 1-3°C / min; then, the mixture is left to react for 30-240 min to obtain a prepolymerization system;

[0126] wherein the full-mixing reactor is controlled to have: the solvent added in an amount of 1-10% of the total monomer raw material, the additive added in an amount of 0.05-0.3% of the total monomer raw material, the actual maximum temperature of the prepolymerization reaction not higher than 10°C from the set temperature, the pressure of 0.5-2.0 MPa, the oxygen content of ≤2 ppm, and the conversion rate of the alkyl methacrylate monomer of 30-50%;

[0127] S3 polymerization: the prepolymerization system obtained from step S2 is introduced into a staged column reactor, which is controlled to have: the temperature of the polymerization reaction of 140-200°C, the pressure of 1.5-3.5 MPa, the additive added again in an amount of 0.04-0.55%, and the moving speed of the material in the column of 0.001-0.1 m / s, and finally, a slurry product is obtained;

[0128] Further, in the staged column reactor, the temperature of each stage gradually increases along the direction of the material flow;

[0129] As a preferred embodiment, the staged column reactor comprises a first stage reaction zone, a second stage reaction zone and a third stage reaction zone arranged in sequence from bottom to top, and the first stage reaction zone is controlled to have: the additive added again in an amount of 0.02-0.2% of the total monomer raw material, the material left to react for 20-100 min, the temperature of 140-155°C, and the total conversion rate of the alkyl methacrylate monomer accumulated to 40-55%;

[0130] The second stage reaction zone is controlled to have: the additive added again in an amount of 0.01-0.2% of the total monomer raw material, the material left to react for 10-80 min, the temperature of 155-175°C, and the total conversion rate of the alkyl methacrylate monomer accumulated to 50-65%;

[0131] The third stage reaction zone is controlled to have: the additive added again in an amount of 0.01-0.15% of the total monomer raw material, the material left to react for 5-60 min, the temperature of 175-200°C, and the total conversion rate of the alkyl methacrylate monomer accumulated to 60-75%;

[0132] Meanwhile, the temperature relationship among the three stage reaction zones is: 7°C≤temperature of the second stage reaction zone - temperature of the first stage reaction zone = temperature of the third stage reaction zone - temperature of the second stage reaction zone≤20°C, that is, the temperature difference between adjacent reaction zones is equal, and 7°C≤temperature difference≤20°C;

[0133] S4: Deashing: The slurry obtained in step S3 is introduced into a deashing extruder, and deashing is performed at a temperature of 200-280°C and an absolute pressure of 10-40 KPa for 10-30 min to obtain a polymer material and waste material (waste material is gas. In the deashing extruder, the waste material is separated from the polymer material after being gasified);

[0134] The polymer material is subjected to subsequent granulation, packaging, etc.

[0135] The waste material including unreacted monomers, solvents, oligomers and additives is introduced into a monomer recovery device, and after separation, waste liquid, waste gas, unreacted monomers and solvents are obtained, and the recovered unreacted monomers can be recycled and used in the batching process.

[0136] Further, before batching, the alkyl methacrylate monomer, the alkyl acrylate monomer and the cyclic (meth)acrylate monomer are each refined to remove the polymerization inhibitor, and then introduced into a mixing buffer tank under the action of a pipeline mixed gas.

[0137] Among them, for each monomer raw material:

[0138] The alkyl methacrylate monomer includes one or a combination of two or more of methyl methacrylate, ethyl methacrylate, propyl methacrylate and (meth)acrylic acid isooctyl ester;

[0139] The alkyl acrylate monomer includes one or a combination of two or more of methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate and isooctyl acrylate;

[0140] The cyclic (meth)acrylate monomer includes one or a combination of two or more of cyclohexyl methacrylate, isobornyl acrylate, isobornyl methacrylate and benzyl methacrylate;

[0141] For the solvent: including one or a combination of two or more of methanol, ethanol, benzene, toluene, methyl acetate and ethyl acetate;

[0142] As a preferred embodiment, the material includes 80-97% of methyl methacrylate, 1-10% of methyl acrylate, 1-8% of isobornyl acrylate and 1-5% of methanol;

[0143] As another preferred embodiment, the material includes 80-97% of methyl methacrylate, 1-10% of ethyl acrylate, 1-7% of isobornyl methacrylate and 1-5% of methanol;

[0144] As another preferred, the material comprises 80-97% of methyl methacrylate, 1-5% of isooctyl acrylate, 1-5% of benzyl methacrylate and 1-5% of ethanol;

[0145] As another preferred, the material comprises 80-95% of methyl methacrylate, 5-10% of propyl acrylate, 2-7% of cyclohexyl methacrylate and 2-5% of ethanol;

[0146] As another preferred, the material comprises 75-95% of methyl methacrylate, 2-5% of isooctyl methacrylate, 1-3% of isobornyl acrylate and 2-5% of methyl acetate;

[0147] For the auxiliary agent: comprising initiator and chain transfer agent;

[0148] The initiator is azo compound or organic peroxide compound. The azo compound is preferably one or a combination of two of azobisisobutyronitrile and azobisisoheptyl nitrile;

[0149] The organic peroxide compound is preferably one or a combination of two or more of dibenzoyl peroxide, dodecanoyl peroxide, di-t-butyl peroxide, dicumyl peroxide and diisopropyl peroxydicarbonate;

[0150] In the full-mixing reaction kettle, the initiator is preferably one or a combination of two or more of azobisisobutyronitrile, dibenzoyl peroxide, di-t-butyl peroxide and azobisisoheptyl nitrile, and the initiator is added in an amount of 0.005-0.03% of the total amount of monomer raw materials; in the staged tubular reactor, the initiator in the first reaction zone and the second reaction zone is preferably one or a combination of two or more of dodecanoyl peroxide, dicumyl peroxide and diisopropyl peroxydicarbonate, and the initiator is added in an amount of 0.005-0.02% of the total amount of monomer raw materials; the initiator in the third reaction zone is preferably one or a combination of two of azobisisoheptyl nitrile and azobisisobutyronitrile, and the initiator is added in an amount of 0.001-0.01% of the total amount of monomer raw materials;

[0151] The chain transfer agent is one or a combination of two or more of benzyl dithiobenzoate, isopropyl phenyl dithiobenzoate, phenethyl dithiobenzoate and 2,4-diphenyl-4-methyl-1-pentene;

[0152] The chain transfer agent is preferably added in an amount of 0.05-0.3% of the total monomer raw material in a full-mixing reaction kettle; in a sectional column reactor, the chain transfer agent is added in an amount of 0.02-0.2% of the total monomer raw material in the first reaction zone, 0.01-0.2% of the total monomer raw material in the second reaction zone, and 0.01-0.15% of the total monomer raw material in the third reaction zone.

[0153] The total amount of initiator added is 0.01-0.1% and the total amount of chain transfer agent added is 0.01-1.0%, based on the total amount of the three monomer esters being 100%. In actual production, the (meth) alkyl acrylate, initiator and transfer agent can be mixed in an air-tight manner and then injected into the material through the feeding port.

[0154] The above is only a preferred embodiment of the present application, and does not limit the present application in any form. Any simple modification or equivalent change made according to the technical essence of the present application falls within the scope of protection of the present application.

Claims

1. A control system for the continuous production of methacrylic polymers, characterized by: The application relates to a control system for a methacrylic polymer production system. The control system comprises a DCS controller (8), which is connected with a man-machine interface through a data input interface, connected with a data acquisition unit through a data feedback interface, and connected with an execution unit through a data output interface. The DCS controller (8) comprises a dosing control module (81), a prepolymerization control module (82) and a polymerization control module (83). The data acquisition unit is arranged in the methacrylic polymer production system, and comprises a sensor group for data acquisition and transmission in the production process of the methacrylic polymer. The execution unit is arranged in the methacrylic polymer production system, and comprises a device group for preparation and regulation of the methacrylic polymer.

2. The control system for continuous production of methacrylic polymers according to claim 1, characterized in that: The sensor group comprises a pressure sensor I (17) and a temperature sensor I (18) arranged on the mixing buffer tank (1), and a pressure sensor II (28) and a temperature sensor II (29) arranged on the full-mixing reaction kettle (2), wherein the pressure sensor I (17), the temperature sensor I (18), the pressure sensor II (28) and the temperature sensor II (29) are connected with the prepolymerization control module (82).

3. The control system for the continuous production of methacrylic polymers according to claim 2, characterized in that: The full-mixing reaction kettle (2) is provided with a stirring device, the stirring device is sleeved with a temperature control coil pipe (206), one end of the temperature control coil pipe (206) is connected with a heat transfer material inlet pipe (207), and the other end is connected with a heat transfer material outlet pipe (208); the full-mixing reaction kettle (2) is sleeved with a heating jacket (210) on the outside, a heat source in the heating jacket (210) is heat conducting oil, an inlet of the heating jacket (210) is connected with a heat conducting oil inlet pipe I (211), and an outlet of the heating jacket (210) is connected with a heat conducting oil outlet pipe I (212); The device group comprises a heat transfer material feeding control valve (26) arranged on the heat transfer material inlet pipe (207), a heat transfer material discharging control valve (27) arranged on the heat transfer material outlet pipe (208), a heat conducting oil feeding control valve I (31) arranged on the heat conducting oil inlet pipe I (211) and a heat conducting oil discharging control valve I (32) arranged on the heat conducting oil outlet pipe I (212), wherein the heat transfer material feeding control valve (26), the heat transfer material discharging control valve (27), the heat conducting oil feeding control valve I (31) and the heat conducting oil discharging control valve I (32) are connected with the prepolymerization control module (82). The temperature sensor I (18), the temperature sensor II (29), the heat-removing material feeding control valve (26), the heat-removing material discharging control valve (27), the heat-conducting oil feeding control valve I (31) and the heat-conducting oil discharging control valve I (32) are connected through electric signals, and the temperature sensor I (18), the temperature sensor II (29), the prepolymerization control module (82), the heat-removing material feeding control valve (26), the heat-removing material discharging control valve (27), the heat-conducting oil feeding control valve I (31) and the heat-conducting oil discharging control valve I (32) form a prepolymerization temperature control loop through electric signals.

4. The control system for continuous production of methacrylic polymers according to claim 1, characterized in that: The sectionalized column reactor (3) comprises a shell (300) and at least two mixed flow units (301) and at least two column reactor units (302) arranged in the shell (300), the mixed flow units (301) and the column reactor units (302) are arranged in intervals and are distributed upwards in sequence; a feeding port is arranged on the lowermost mixed flow unit (301), and a discharging port is arranged on the uppermost column reactor unit (302), and a continuous passage for polymerization reaction is formed between the feeding port, the mixed flow unit (301), the column reactor unit (302) and the discharging port; The sensor group comprises pressure sensor III (39) and temperature sensor III (40) distributed on the mixed flow unit (301), and pressure sensor IV (41) and temperature sensor IV (42) distributed on the column reactor unit (302), and the pressure sensor III (39), the temperature sensor III (40), the pressure sensor IV (41) and the temperature sensor IV (42) are connected with the polymerization control module (83).

5. The control system for the continuous production of methacrylic polymers according to claim 4, characterized in that: The bottom column reactor unit (302) is connected with a heat-conducting oil inlet pipe II (307), the top column reactor unit (302) is connected with a heat-conducting oil outlet pipe II (308), and the upper column reactor unit (302) and the lower column reactor unit (302) are connected through a heat-conducting oil communication pipe (309); and the column reactor unit (302) is further connected with a cold oil feeding pipe (311); The equipment group comprises a heat-conducting oil feeding control valve II (35) arranged on the heat-conducting oil inlet pipe II (307), a heat-conducting oil discharging control valve II (36) arranged on the heat-conducting oil outlet pipe II (308) and a cold oil feeding control valve (37) arranged on the cold oil feeding pipe (311), and the heat-conducting oil feeding control valve II (35), the heat-conducting oil discharging control valve II (36) and the cold oil feeding control valve (37) are connected with the polymerization control module (83); The temperature sensor III (40), the temperature sensor IV (42), the heat-conducting oil feeding control valve II (35), the heat-conducting oil discharging control valve II (36) and the cold oil feeding control valve (37) are connected through electric signals, and the temperature sensor III (40), the temperature sensor IV (42), the polymerization control module (83), the heat-conducting oil feeding control valve II (35), the heat-conducting oil discharging control valve II (36) and the cold oil feeding control valve (37) form a polymerization temperature control loop through electric signals.

6. The control system for the continuous production of methacrylic polymers according to any of claims 1-5, characterized in that: The mixed buffer tank (1) is connected with an alkyl methacrylate monomer metering tank (101) through an alkyl methacrylate monomer feeding pipe (100), is also connected with an alkyl acrylate monomer metering tank (103) through an alkyl acrylate monomer feeding pipe (102), is also connected with a (methyl) cyclic acrylate monomer metering tank (105) through a (methyl) cyclic acrylate monomer feeding pipe (104), and is also connected with a protective gas storage tank (5) through a protective gas inlet pipe I (1066); a displacement gas outlet pipe (107) is connected to the mixed buffer tank (1); The full-mixing reaction kettle (2) is connected with a solvent metering tank (201) through a solvent feeding pipe (200), is also connected with a solvent metering tank (203) through an additive feeding pipe I (202), and is connected with the protective gas storage tank (5) through a protective gas inlet pipe II (204); The mixed flow unit (301) in the sectional tubular reactor (3) is connected with an additive feeding pipe II (306), and the mixed flow unit (301) comprises a mixed flow cavity (303) in communication with the additive feeding pipe II (306); the tubular reaction unit (302) in the sectional tubular reactor (3) comprises a tubular column (304) arranged in a longitudinal direction, and a temperature control cavity (305) between the tubular column (304) and a shell (300) is used for containing heat conducting oil, and a cold oil feeding pipe (311) is connected with the temperature control cavity (305); The sensor group further comprises an alkyl methacrylate monomer metering pump (10) arranged on the alkyl methacrylate monomer feeding pipe (100), an alkyl acrylate monomer metering pump (12) arranged on the alkyl acrylate monomer feeding pipe (102), a (methyl) cyclic acrylate monomer metering pump (14) arranged on the (methyl) cyclic acrylate monomer feeding pipe (104), an oxygen content analyzer (16) arranged on the displacement gas outlet pipe (107), a solvent metering pump (22) arranged on the solvent feeding pipe (200), an additive metering pump I (24) arranged on the additive feeding pipe I (202), and an additive metering pump II (34) arranged on the additive feeding pipe II (306), and the alkyl methacrylate monomer metering pump (10), the alkyl acrylate monomer metering pump (12), the (methyl) cyclic acrylate monomer metering pump (14), the oxygen content analyzer (16), the solvent metering pump (22), the additive metering pump I (24), and the additive metering pump II (34) are connected with the batching control module (81); The solvent metering pump (22) and the additive metering pump I (24) are connected with the prepolymerization control module (82); The additive metering pump II (34) is connected with the polymerization control module (83).

7. The control system for the continuous production of methacrylic polymers according to claim 6, characterized in that: The device group further comprises an alkyl methacrylate monomer feed control valve (9) arranged on an alkyl methacrylate monomer feed pipe (100), an alkyl acrylate monomer feed control valve (11) arranged on an alkyl acrylate monomer feed pipe (102), a (meth) cyclic acrylate monomer feed control valve (13) arranged on a (meth) cyclic acrylate monomer feed pipe (104), a protective gas feed control valve I (15) arranged on a protective gas inlet pipe I (1066), a solvent feed control valve (20) arranged on a solvent feed pipe (200), an auxiliary agent feed control valve I (23) arranged on an auxiliary agent feed pipe I (202), a protective gas feed control valve II (25) arranged on a protective gas inlet pipe II (204), and an auxiliary agent feed control valve II (33) arranged on an auxiliary agent feed pipe II (306), and the alkyl methacrylate monomer feed control valve (9), the alkyl acrylate monomer feed control valve (11), the (meth) cyclic acrylate monomer feed control valve (13), the protective gas feed control valve I (15), the solvent feed control valve (20), the auxiliary agent feed control valve I (23), and the auxiliary agent feed control valve II (33) are connected with the batching control module (81); The solvent feed control valve (20), the auxiliary agent feed control valve I (23), and the protective gas feed control valve II (25) are connected with the prepolymerization control module (82); The auxiliary agent feed control valve II (33) is connected with the polymerization control module (83); The alkyl methacrylate monomer metering pump (10) and the alkyl methacrylate monomer feed control valve (9) are connected through electrical signals, the alkyl methacrylate monomer metering pump (10), the batching control module (81), and the alkyl methacrylate monomer feed control valve (9) form an alkyl methacrylate monomer feed control loop through electrical signals; The alkyl acrylate monomer metering pump (12) and the alkyl acrylate monomer feed control valve (11) are connected through electrical signals, the alkyl acrylate monomer metering pump (12), the batching control module (81), and the alkyl acrylate monomer feed control valve (11) form an alkyl acrylate monomer feed control loop through electrical signals; The (meth) cyclic acrylate monomer metering pump (14) and the (meth) cyclic acrylate monomer feed control valve (13) are connected through electrical signals, the (meth) cyclic acrylate monomer metering pump (14), the batching control module (81), and the (meth) cyclic acrylate monomer feed control valve (13) form a (meth) cyclic acrylate monomer feed control loop through electrical signals; The solvent metering pump (22) and the solvent feed control valve (20) are connected through electrical signals, the solvent metering pump (22), the batching control module (81), the prepolymerization control module (82), and the solvent feed control valve (20) form a solvent feed control loop through electrical signals; The auxiliary agent metering pump I (24) and the auxiliary agent feeding control valve I (23) are connected through electrical signal interlocking, and the auxiliary agent metering pump I (24), the batching control module (81), the prepolymerization control module (82) and the auxiliary agent feeding control valve I (23) form an auxiliary agent feeding control loop in the prepolymerization process through electrical signals. The auxiliary agent metering pump II (34) and the auxiliary agent feeding control valve II (33) are connected through electrical signal interlocking, and the auxiliary agent metering pump II (34), the batching control module (81), the polymerization control module (83) and the auxiliary agent feeding control valve II (33) form an auxiliary agent feeding control loop in the polymerization process through electrical signals.

8. The control system for continuous production of methacrylic polymers according to claim 1, characterized in that: The mixed material delivery pipe (108) is connected to the full-mixing reaction kettle (2) through the discharge port of the mixing buffer tank (1), the full-mixing reaction kettle (2) is connected to the sectional column reactor (3) through the prepolymerization reaction system delivery pipe (209) through the discharge port, and the sectional column reactor (3) is connected to the deashing and extruding integrated machine (4) through the reactant delivery pipe (310) through the discharge port. The device group further comprises a mixed material delivery pump (19) arranged on the mixed material delivery pipe (108), a prepolymerization reaction system delivery pump (30) arranged on the prepolymerization reaction system delivery pipe (209) and a reactant delivery pump (38) arranged on the reactant delivery pipe (310). The mixed material delivery pump (19), the prepolymerization reaction system delivery pump (30) and the reactant delivery pump (38) are connected to the DCS controller (8).

9. The control system for continuous production of methacrylic polymers according to claim 1, characterized in that: The device group further comprises a frequency converter arranged on the stirring device, and the stirring device is connected to the stirring motor through the frequency converter; the frequency converter is connected to the prepolymerization control module (82).

10. The control system for continuous production of methacrylic polymers according to claim 1, characterized in that: The DCS controller (8) further comprises a deashing separation control template (86), a waste treatment module (84) and an alarm control module (85), the deashing separation control module is connected to the polymerization control module (83), the waste treatment module (84) is connected to the deashing separation control module, and the alarm control module (85) is connected to the batching control module (81), the prepolymerization control module (82), the polymerization control module (83), the deashing separation control template (86) and the waste treatment module (84).

Citation Information

Patent Citations

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