A carbomer production system and process thereof

Abstract

The present application provides a carbomer production system and process, including raw material mixing mechanism, polymerization reactor, solvent recovery mechanism, product dehydration mechanism and packaging mechanism, the raw material mixing mechanism includes several storage tanks, metering pumps and high-efficiency mixers, the storage tanks are used for storing monomers, crosslinking agents and initiators respectively, a sealing cover and an exhaust port are arranged on the top of each storage tank, and the bottom of the storage tank is connected to the metering pump through a pipeline. The carbomer production system and process have the characteristics of high efficiency, environmental protection, stability and automation, significantly improve the production efficiency of carbomer, ensure the high quality of the product, and greatly reduce the energy consumption and environmental pollution. Through comprehensive sensor monitoring and central control system, the safety and intelligent operation of the production process are ensured. In addition, the modular design of the equipment and the flexibility of the process make the system widely applicable to different production scales and various carbomer product manufacturing needs.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of carbomer preparation, in particular to a carbomer production system and process thereof. BACKGROUND

[0002] Carbomer is a commonly used high molecular polymer, widely used in medical, cosmetic and industrial fields as thickening agent, suspending agent and stabilizer, etc. The basic composition of carbomer is a high molecular network structure formed by acrylic acid as the main monomer and crosslinking agent. Its performance mainly includes good thickening effect, high viscosity, good rheological properties and sensitivity to pH. These properties make it have wide application value in colloidal systems.

[0003] However, there are still some technical problems in the existing carbomer production process and equipment in the industrialization process:

[0004] 1. Inhomogeneous mixing In the traditional production process, the mixing efficiency of acrylic acid, crosslinking agent and initiator is low, which can easily lead to uneven distribution of materials, thereby affecting the stability of the polymerization reaction and the performance of the carbomer product. The existing high-efficiency mixer design is insufficient, and it is difficult to meet the needs of rapid and uniform mixing.

[0005] 2. Unstable reaction condition control The polymerization reaction of carbomer has strict requirements on temperature, pressure and stirring speed, but the temperature control system and stirring device of the existing polymerization equipment often lack precision, making it difficult to adjust the reaction conditions in real time, leading to an increase in side reactions during the polymerization process, and ultimately causing large fluctuations in the quality of the final product.

[0006] 3. Solvent volatilization and environmental pollution The solvents used in the production process (such as isopropyl alcohol and ethanol) have certain volatility. If the solvent recovery equipment is not designed reasonably, it is easy to cause excessive volatilization of the solvent, which not only increases the production cost, but also causes environmental pollution. In addition, solvent volatilization also poses a potential threat to the health of workshop operators.

[0007] 4. Low efficiency of product post-treatment The product dehydration process in the existing technology has low efficiency, and the design of vacuum drying or centrifugal separation equipment has not been fully optimized, often leading to high energy consumption, low production capacity, and affecting the drying quality of the carbomer product.

[0008] 5. Insufficient degree of system modularization Many existing carbomer production equipment lacks modular design, has high equipment maintenance and replacement cost, and is difficult to adapt to the flexible adjustment of different production scales and process requirements, limiting the application range and production efficiency of the equipment.

[0009] In view of the above problems, developing an efficient, stable and environmentally friendly carbomer production system has become an urgent need for the industry development. By optimizing the design of equipment and process flow, not only the production efficiency and product performance of carbomer can be improved, but also the energy consumption and environmental impact in the production process can be reduced. In view of these technical problems, the present application proposes an improved carbomer production system and its production process to solve the defects in the prior art. SUMMARY

[0010] The present application aims to provide a carbomer production system and process to improve production efficiency, stabilize product quality and reduce environmental impact.

[0011] To achieve the above purpose, the present application proposes the following technical scheme: a carbomer production system, comprising:

[0012] A raw material mixing mechanism, comprising a plurality of storage tanks, metering pumps and high-efficiency mixers, the storage tanks are respectively used to store monomers, crosslinking agents and initiators, each storage tank is provided with a sealing cover and an exhaust port at the top, the bottom of the storage tank is connected to the metering pump through a pipeline, the metering pump is connected to the bottom of the storage tank, and is used to deliver the raw materials to the high-efficiency mixer according to the set proportion; the high-efficiency mixer is connected to the metering pump through a feeding pipe, and the high-efficiency mixer is provided with multi-leaf high-speed stirring paddles;

[0013] A polymerization reactor, connected to the outlet of the high-efficiency mixer, provided with a high-precision temperature control system, a stirrer and a gas-tight sealing structure;

[0014] The temperature control system comprises a plurality of temperature sensors, a heating unit and a cooling unit, the temperature in the reactor is adjusted through a jacket structure, the stirrer is located in the reactor, and the stirrer is driven by a variable speed motor, and the stirring speed is adjusted according to the reaction viscosity;

[0015] The sealing structure comprises a sealing ring and an exhaust valve, which are arranged on the cover of the reactor to prevent solvent evaporation;

[0016] A solvent recovery mechanism, connected to the exhaust valve of the polymerization reactor through a pipeline, used to recover the volatile solvent in the production process;

[0017] The solvent recovery mechanism comprises a condenser and an adsorption device, the volatile solvent is condensed into liquid by the condenser, the adsorption device is connected to the outlet of the condenser through a pipeline, and the adsorption device is provided with activated carbon or adsorption resin to further absorb the uncondensed solvent;

[0018] A product dehydration mechanism, connected to the discharge port at the bottom of the polymerization reactor, used to remove the water and solvent in the carbomer reaction product;

[0019] The product dehydration mechanism comprises a vacuum dryer and a centrifugal separation device, the vacuum dryer comprises a heating plate and a vacuum pump, and is used for removing solvent in a low-temperature environment, and the centrifugal separation device separates excess liquid from solid through centrifugal force;

[0020] The packaging mechanism comprises an automatic weighing device and a sealing device, and is used for packaging the dehydrated finished product, the automatic weighing device is connected with the outlet of the dehydration device, is used for accurate weighing, and the sealing device comprises a sealing machine and a vacuum packaging device, and is used for sealing and packaging the finished product.

[0021] Further, in the application, the inner wall of the polymerization reactor is made of corrosion-resistant material, and a jacket heating structure is arranged outside for heating or cooling the reaction liquid.

[0022] Further, in the application, the storage tank, the metering pump and the high-efficiency mixer are connected through quick-assembly pipelines; the polymerization reactor and the solvent recovery mechanism are connected through high-temperature-resistant pipelines, and flow control valves are arranged on the pipelines; the polymerization reactor and the product dehydration mechanism are connected through a delivery pump, and a filter screen is arranged at the inlet of the delivery pump to prevent solid particles from blocking the pipeline; all the equipment is fixed on standardized bases and is uniformly controlled through a central control system.

[0023] Further, in the application, the polymerization reactor is provided with a temperature sensor and a pressure sensor, the temperature sensor and the pressure sensor are respectively used for detecting reaction conditions; the solvent recovery mechanism is provided with a gas concentration sensor, and the gas concentration sensor is used for monitoring solvent evaporation; the dehydration mechanism is provided with a humidity sensor, and the humidity sensor is used for judging whether the dehydration process is completed;

[0024] The polymerization reactor is provided with a pH sensor, a viscometer and a solid content analyzer;

[0025] The polymerization reactor is provided with a heating unit and a pressure control unit, the heating unit is an electric heater, and the pressure control unit is a pressure valve.

[0026] Further, in the application, a control system is included, the control system comprises a PLC, the temperature sensor, the pressure sensor, the pH sensor, the viscometer, the stirrer and the electric heater are connected with the PLC, and the PLC adjusts the temperature of the polymerization reaction through the following process:

[0027] Step one, data acquisition and pretreatment;

[0028] The following variables are collected from the sensor:

[0029] Temperature-T measured (t), pressure Pmeasured (t), viscosity η measured (t), pH value pH measured (t);

[0030] De-noising processing, using the moving average method to smooth the original data collected, filter out noise: Wherein, X(t) is the real-time acquisition value, N is the size of the sliding window;

[0031] Error calculation, error calculation formula as follows:

[0032] e T (t) = T target -T filtered (t);

[0033] e P (t) = P targtet -P filtered (t);

[0034] e S (t) = η target -η fitered (t);

[0035] e T (t): temperature error, temperature error at time t, unit ℃;

[0036] T target : target temperature, the ideal temperature value, unit ℃;

[0037] T measured (t): the current measured temperature value, unit ℃;

[0038] e P (t): pressure error, pressure error at time t, unit: MPa;

[0039] P target : target pressure, the ideal pressure value, unit: Mpa;

[0040] P measured (t): the current measured pressure value, the pressure obtained by real-time monitoring of the system, unit: MPa;

[0041] e S (t): stirring speed error, viscosity error at time t, mPa·s;

[0042] η target : target viscosity, the ideal viscosity value, unit: mPa·s;

[0043] η measured(t): current measured viscosity value, viscosity value obtained by real-time monitoring of the system, unit: mPa·s;

[0044] Step two: fuzzy control rules;

[0045] Define the membership function for input error e T , e P , e S and output adjustment value ΔT, ΔP, ΔS, use triangular distribution: a, b, c are the threshold values of the membership function;

[0046] If e T is "high", increase ΔT; if e P is "low", decrease ΔP; if e S is "high", decrease ΔS;

[0047] Fuzzy control output calculation:

[0048]

[0049] ΔT: temperature adjustment value, adjust the output of the heating or cooling system;

[0050] ΔP: pressure adjustment value, adjust the output of the pressure system;

[0051] ΔS: stirring speed adjustment value, adjust the speed of the stirrer;

[0052] w i : weight value of the ith fuzzy rule, indicating the influence degree of the rule on the final adjustment amount;

[0053] μ(e T ): membership function value of temperature error e T , indicating the fuzzy membership of temperature error;

[0054] μ(e P ): membership function value of pressure error e P , indicating the fuzzy membership of pressure error;

[0055] μ(e S ): membership function value of stirring speed error e S , indicating the fuzzy membership of stirring speed error;

[0056] n: number of fuzzy rules, each rule will give an adjustment value;

[0057] Step three, PID controller parameter self-tuning;

[0058] Each adjustment amount is calculated by PID control, the formula is as follows:

[0059]

[0060] Δu T (t): adjustment amount of temperature control, i.e. adjusting the control output of the heating / cooling system according to the temperature error;

[0061] K pT : proportional gain of temperature control, indicating the weight of the proportional control part;

[0062] K iT : integral gain of temperature control, indicating the weight of the integral control part;

[0063] K dT : differential gain of temperature control, indicating the weight of the differential control part;

[0064] e T (t): temperature error, indicating the difference between the target temperature and the current temperature;

[0065] ∫e T (t): integral part of temperature error, indicating the cumulative value of the error;

[0066] differential part of temperature error, indicating the rate of change of the error;

[0067] PID controller parameters are dynamically adjusted by fuzzy control:

[0068]

[0069] K pT , K iT , K dT are gain parameters of the PID controller, μ(e T ) is the output of the fuzzy controller;

[0070] The PID control parameter adjustment for pressure and stirring speed is the same.

[0071] A carbomer production process, using the above-mentioned carbomer production system, further comprising the following steps:

[0072] Step one: prepare raw materials, including 100 parts of acrylic acid, 0.5-1 parts of crosslinking agent, 0.2-0.5 parts of initiator, 100-150 parts of solvent, appropriate amount of pH regulator, 50-100 parts of water: acrylic acid as the main monomer, providing the basic structure of carbomer, acrylic acid, crosslinking agent, initiator and solvent are weighed according to the proportion and placed in the storage tank respectively; add water in the reaction kettle, start stirring, and maintain uniform liquid environment;

[0073] Step two solution mixing, acrylic acid and crosslinking agent are slowly added into the reaction kettle while stirring; initiator solution is added, stirring speed is controlled at 100-300 rpm, ensuring uniform mixing; temperature is controlled at 25-35℃, avoiding too high reaction rate;

[0074] Step three polymerization reaction, start heating system, increase the temperature of the reaction kettle to 65-80℃; at the beginning of the reaction, observe the viscosity change of the system and adjust the stirring speed; reaction time is 2-4 hours, after the reaction is completed, a transparent gel-like polymer is formed;

[0075] Step four post-treatment, transfer the reaction product to a vacuum drying device, control the temperature below 60℃, remove the solvent and moisture; adjust the pH to the range of 6.0-7.0, ensure that the carbomer has good application performance; if powder carbomer is needed, further crushing and sieving treatment can be carried out;

[0076] Step five packaging, transfer the dried carbomer to the packaging machine, automatically weigh and seal according to the specifications, prevent moisture absorption.

[0077] Further, in the present application, the crosslinking agent is one or both of ethylene glycol diacrylate or pentaerythritol triacrylate, which gives the carbomer gel network structure.

[0078] Further, in the present application, the initiator is one or both of ammonium persulfate or benzoyl peroxide, which is used to initiate the polymerization reaction.

[0079] Further, in the present application, the solvent is isopropyl alcohol or ethanol, which serves as a dispersion medium to reduce by-products during the reaction process.

[0080] Further, in the present application, the pH regulator is selected from sodium hydroxide or triethanolamine.

[0081] Beneficial effects, the technical scheme of the present application has the following technical effects:

[0082] The carbomer production system and process of the present application have the characteristics of high efficiency, environmental protection, stability and automation, significantly improving the production efficiency of carbomer, ensuring the high quality of the product, and greatly reducing energy consumption and environmental pollution. Through comprehensive sensor monitoring and central control system, the safety and intelligent operation of the production process are ensured. In addition, the modular design of the equipment and the flexibility of the process make the system widely applicable to different production scales and the manufacturing needs of various carbomer products.

[0083] It should be understood that all combinations of the aforementioned concepts and additional concepts described in greater detail below can be seen as part of the subject matter of the present disclosure, as long as such concepts are not mutually contradictory.

[0084] The foregoing and other aspects, embodiments and features of the present teachings can be better understood from the following description of the BRIEF DESCRIPTION OF DRAWINGS

[0085] The drawings are not intended to be to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures can be represented by a like numeral. For purposes of clarity, not every component can be called out in every drawing. There is a description of embodiments of various aspects of the present teachings with reference to the attached drawings, in which:

[0086] Figure 1 Schematic diagram of the system of the present application.

[0087] Figure 2 Schematic diagram of the structural arrangement of the present application.

[0088] In the drawings, the following symbols are used: 1: storage tank; 2: metering pump; 3: high-efficiency mixer; 4: material conveying pipe; 5: polymerization reactor; 7: stirrer; 8: air-tight sealing structure; 9: condenser; 10: adsorption device; 11: vacuum dryer; 12: centrifugal separation device; 13: automatic weighing device; 14: sealing device. DETAILED DESCRIPTION

[0089] For a more complete understanding of the technical content of the present application, specific embodiments are described below with reference to the accompanying drawings. Aspects of the present application are described in this disclosure with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. The embodiments of the present disclosure are not necessarily defined by every embodiment described. It is to be understood that various concepts and embodiments introduced above and those described in greater detail below can be implemented in any of numerous ways, as the disclosed concepts and embodiments are not limited to any particular manner of implementation. Additionally, some aspects of the present disclosure can be utilized independently, or in any suitable combination with other aspects of the present disclosure.

[0090] As Figure 1As shown, the present application provides a carbomer production system, which comprises a raw material mixing mechanism, a polymerization reactor 5, a solvent recovery mechanism, a product dehydration mechanism and a packaging mechanism. The raw material mixing mechanism comprises a plurality of storage tanks 1, metering pumps 2 and a high-efficiency mixer 3. The storage tanks 1 are respectively used for storing monomers, crosslinking agents and initiators. Each storage tank 1 is provided with a sealing cover and an exhaust port at the top. The bottom of each storage tank 1 is connected to a metering pump through a pipeline. The metering pumps 2 are connected to the bottoms of the storage tanks and used for conveying raw materials to the high-efficiency mixer 3 according to a set ratio. The high-efficiency mixer 3 is connected to the metering pumps through a feeding pipe 4. The high-efficiency mixer 3 is provided with multi-leaf high-speed stirring paddles.

[0091] The polymerization reactor 5 is connected to the outlet of the high-efficiency mixer 3. The polymerization reactor 5 is provided with a high-precision temperature control system, a stirrer 7 and a gas-tight sealing structure 8.

[0092] The temperature control system comprises a plurality of temperature sensors, a heating unit and a cooling unit. The cooling unit is a fan. The temperature in the reactor is adjusted through a jacket structure. The stirrer 7 is located in the reactor. The stirrer 7 is driven by a variable-speed motor. The stirring speed is adjusted according to the reaction viscosity.

[0093] The sealing structure 8 comprises a sealing ring and an exhaust valve, which are arranged on the cover of the reactor to prevent solvent evaporation.

[0094] The solvent recovery mechanism is connected to the exhaust valve of the polymerization reactor 5 through a pipeline and used for recovering the solvent volatilized in the production process.

[0095] The solvent recovery mechanism comprises a condenser 9 and an adsorption device 10. The condenser 9 condenses the volatile solvent into a liquid. The adsorption device 10 is connected to the outlet of the condenser 9 through a pipeline. The adsorption device 10 is provided with activated carbon or adsorption resin and used for further absorbing the uncondensed solvent.

[0096] The product dehydration mechanism is connected to the discharge port at the bottom of the polymerization reactor 5. The product dehydration mechanism is used for removing the water and solvent in the carbomer reaction product.

[0097] The product dehydration mechanism comprises a vacuum drying machine 11 and a centrifugal separation device 12. The vacuum drying machine 11 comprises a heating plate and a vacuum pump and is used for removing the solvent in a low-temperature environment. The centrifugal separation device 12 separates the excess liquid from the solid through centrifugal force.

[0098] The packaging mechanism comprises an automatic weighing device and a sealing device and is used for packaging the dehydrated product. The packaging mechanism comprises an automatic weighing device 13 and a sealing device 14. The automatic weighing device 13 is connected to the outlet of the dehydration device and used for accurate weighing. The sealing device 14 comprises a sealing machine and a vacuum packaging device and is used for sealing and packaging the product.

[0099] In this embodiment, the inner wall of the polymerization reactor 5 is made of corrosion-resistant material, and a jacket heating structure is provided outside for heating or cooling the reaction liquid.

[0100] In this embodiment, the storage tank 1, the metering pump 2, and the high-efficiency mixer 3 are connected by quick-assembly pipes; the polymerization reactor 5 and the solvent recovery mechanism are connected by high-temperature-resistant pipes, and flow control valves are provided on the pipes; the polymerization reactor 5 and the product dehydration mechanism are connected by a delivery pump, and the inlet of the delivery pump is provided with a filter screen to prevent solid particles from blocking the pipes; all equipment is fixed on standardized bases and is uniformly controlled by a central control system.

[0101] In this embodiment, the polymerization reactor 5 is provided with temperature sensors and pressure sensors for detecting reaction conditions; the solvent recovery mechanism is provided with a gas concentration sensor for monitoring solvent evaporation; and the dehydration mechanism is provided with a humidity sensor for determining whether the dehydration process is complete.

[0102] In this embodiment, the polymerization reactor 5 is provided with pH sensors, viscometers, and solid content analyzers.

[0103] The working principle of this production system can be divided into five main stages: raw material mixing, polymerization reaction, solvent recovery, product dehydration, and product packaging. Specifically, the raw material mixing mechanism is composed of a storage tank 1, a metering pump 2, and a high-efficiency mixer 3, which are used to accurately mix monomers (such as acrylic acid), crosslinking agents (such as ethylene glycol diacrylate), initiators (such as ammonium persulfate), and solvents (such as isopropyl alcohol) in proportion. Each raw material is stored in a different storage tank. The top of the storage tank is provided with a sealed cover and an exhaust port to prevent the raw materials from evaporating and to maintain the system closed. According to the formula proportion, the metering pump delivers each raw material through the pipeline to the high-efficiency mixer 3. The high-efficiency mixer 3 is equipped with multi-blade high-speed stirring paddles, which uniformly mix the materials through high-speed rotation, avoiding local over-concentration or unevenness. The mixed raw materials enter the polymerization reactor 5 through the feed pipe 4.

[0104] After that, the mixed raw materials enter the polymerization reactor 5 to undergo polymerization reaction under the set temperature and pressure conditions, generating carbomer gel. The temperature control system uses a jacket structure and multiple temperature sensors to accurately control the reaction temperature through heating and cooling units, ensuring the stability of the reaction process. The stirrer 7 is driven by a variable speed motor, which automatically adjusts the stirring speed according to the reaction viscosity, ensuring that the materials are fully mixed and preventing local overheating. The sealing ring and exhaust valve of the airtight sealing structure 8 effectively prevent solvent evaporation, ensuring that the reaction conditions are controlled. The temperature sensor, pressure sensor, pH sensor, viscometer, and solid content analyzer inside the reactor monitor the reaction conditions in real time, ensuring product quality and reaction safety.

[0105] After solvent recovery, the volatile solvent in the polymerization process enters the solvent recovery mechanism through the reactor exhaust valve, reducing the emission of volatile organic compounds (VOC). The volatile solvent is cooled to liquid in the condenser 9, and returns to the storage tank for reuse. The condensed solvent is further absorbed by activated carbon or adsorption resin through the adsorption device 10, ensuring that the solvent emission is minimized. The gas concentration sensor monitors the solvent volatilization in real time, and feeds back to the central control system to adjust the recovery parameters.

[0106] The product dehydration process, the carbomer gel generated by the polymerization reaction contains a lot of water and residual solvent, which is post-processed by the product dehydration mechanism. Under the condition of low temperature and low pressure, the solvent and water are removed by heating plate and vacuum pump, avoiding the influence of high temperature on the performance of the product. The excess liquid and solid are further separated by centrifugal force, improving the dehydration efficiency and reducing the subsequent drying burden. The humidity sensor monitors the humidity after dehydration in real time to ensure that the water content of the product meets the requirements.

[0107] Finally, the product packaging is carried out, and the dehydrated carbomer product is weighed and packaged by the packaging mechanism to prepare the final product. The automatic weighing device 13 accurately measures the mass of the dehydrated carbomer to ensure the consistency of the packaging specifications. The sealing machine in the sealing device 14 heat-seals the packaging bag, and the vacuum packaging device is used to prevent the finished product from being damp and contaminated. All equipment is uniformly controlled by the central control system. The parameters include temperature, pressure, stirring speed, flow rate, etc. The system adjusts the operating conditions by monitoring sensor data (such as temperature, pressure, humidity, gas concentration, etc.) in real time. Once an abnormality is detected (such as excessive temperature, excessive pressure, or solvent leakage), the system automatically sends an alarm and takes emergency measures to ensure the safety of the production process.

[0108] In this embodiment, the polymerization reactor (5) is provided with a heating unit and a pressure control unit, the heating unit is an electric heater, and the pressure control unit is a pressure valve.

[0109] The control system is also included in this embodiment, which includes a PLC, and the temperature sensor, pressure sensor, pH sensor, viscometer stirrer and electric heater are connected with the PLC, and the PLC adjusts the temperature of the polymerization reaction by the following process:

[0110] Step one, data acquisition and pretreatment;

[0111] The following variables are collected from the sensor:

[0112] Temperature-T measured (t), pressure P measured (t), viscosity η measured (t), pH value pH measured (t);

[0113] De-noising processing, using the moving average method to smooth the collected raw data, filter out noise: Wherein, X(t) is the real-time acquisition value, N is the size of the sliding window;

[0114] Calculate the error, the error calculation formula is as follows:

[0115] e T (t) = T target -T filtered (t);

[0116] e P (t) = P target -P filtered (t);

[0117] e S (t) = η target -η fitered (t);

[0118] e T (t) : temperature error, temperature error at time t, unit ℃;

[0119] T target : target temperature, the ideal temperature value, unit ℃;

[0120] T measured (t) : the current measured temperature value, unit ℃;

[0121] e P (t) : pressure error, pressure error at time t, unit: MPa;

[0122] P target : target pressure, the ideal pressure value, unit: Mpa;

[0123] P measured (t) : the current measured pressure value, the pressure obtained by real-time monitoring of the system, unit: MPa;

[0124] e s (t) : stirring speed error, viscosity error at time t, mPa·s;

[0125] η target : target viscosity, the ideal viscosity value, unit: mPa·s;

[0126] η measured (t) : the current measured viscosity value, the viscosity obtained by real-time monitoring of the system, unit: mPa·s;

[0127] Step 2: fuzzy control rule;

[0128] The input error e T , e P , e S and the output adjustment value ΔT, ΔP, ΔS define the membership function, using a triangular distribution: a, b, c are the threshold values of the membership function;

[0129] If e T is "high", increase ΔT; if e P is "low", decrease ΔP; if e S is "high", decrease ΔS;

[0130] Fuzzy control output calculation:

[0131]

[0132] ΔT: temperature adjustment value, adjust the output of the heating or cooling system;

[0133] ΔP: pressure adjustment value, adjust the output of the pressure system;

[0134] ΔS: stirring speed adjustment value, adjust the speed of the stirrer;

[0135] w i : weight value of the i-th fuzzy rule, indicating the degree of influence of the rule on the final adjustment amount;

[0136] μ(e T ): membership function value of the temperature error e T , indicating the fuzzy membership of the temperature error;

[0137] μ(e P ): membership function value of the pressure error e P , indicating the fuzzy membership of the pressure error;

[0138] μ(e S ): membership function value of the stirring speed error e S , indicating the fuzzy membership of the stirring speed error;

[0139] n: number of fuzzy rules, each rule gives an adjustment value;

[0140] Step three, PID controller parameter self-tuning;

[0141] Each adjustment amount is calculated by PID control, the formula is as follows:

[0142]

[0143] Δu T(t): the adjustment amount of temperature control, i.e. adjusting the control output of heating / cooling system according to temperature error;

[0144] K pT : the proportional gain of temperature control, representing the weight of proportional control part;

[0145] K iT : the integral gain of temperature control, representing the weight of integral control part;

[0146] K dT : the differential gain of temperature control, representing the weight of differential control part;

[0147] e T (t): temperature error, representing the difference between target temperature and current temperature;

[0148] ∫e T (t): integral part of temperature error, representing the accumulated value of error;

[0149] differential part of temperature error, representing the rate of change of error;

[0150] PID controller parameters are dynamically adjusted by fuzzy control:

[0151]

[0152] K pT , K iT , K dT are gain parameters of PID controller, μ(e T ) is the output of fuzzy controller;

[0153] The adjustment of PID control parameters for pressure and stirring speed is the same.

[0154] Specific operation process initialization: set target value T target , P target , η target , initialize PID parameters K p , K i , K d , real-time data acquisition: collect T measured (t), P measured (t), η measured (t) every second. Calculate error and fuzzy inference: calculate fuzzy adjustment value ΔT, ΔP, ΔS according to e T , e P , e S . Adjust PID parameters according to fuzzy inference results. Apply PID control, use PID control formula to calculate adjustment value Δu T , Δu P , ΔuS The electric heater and the stirring speed of the stirrer are adjusted. The feedback adjustment updates the collected data and the control quantity every second. The loop is executed until the error e T , e P , e S is stabilized within the set threshold range.

[0155] For example, assuming the target temperature T target = 80℃, the target pressure P target = 0.8MPa, and the target viscosity η measured (t) = 2000mPa·s. The current temperature T measured = 75°, and the error e T = 5°. The fuzzy inference gives: ΔT = +10%, and the cooling power ΔP = -5%. The PID adjustment gives: increase the electric heater power by 8%, and decrease the cooling unit power by 3%. Finally, through real-time adjustment, the reaction conditions quickly tend to be stable.

[0156] The present application can efficiently mix and accurately control the reaction: through advanced mixing and temperature control technology, the uniformity of the reaction materials and the stability of the reaction process are ensured. The solvent is effectively recovered, the emission of volatile substances is reduced, and the resource utilization rate is improved. The production process is modularly designed, the central control system is monitored in real time, the production efficiency and product quality are improved. The combination of vacuum drying and centrifugal separation greatly reduces energy consumption while improving dehydration effect. Through the above working principle, the system realizes the goals of efficient, environmentally friendly, safe and high-quality output of carbomer production.

[0157] Example 1: High-efficiency raw material mixing test

[0158] Purpose of the experiment: to verify whether the combination of the storage tank, the metering pump and the high-efficiency mixer can achieve efficient and uniform mixing.

[0159] Experimental conditions:

[0160] Monomer: 100 parts of acrylic acid;

[0161] Crosslinking agent: 0.7 parts of ethylene glycol diacrylate;

[0162] Initiator: 0.3 parts of ammonium persulfate;

[0163] Solvent: 120 parts of isopropyl alcohol;

[0164] Temperature: 30℃;

[0165] Mixing time: 10 minutes;

[0166] Stirring speed: 200RPM;

[0167] Experimental data:

[0168] Viscosity uniformity test (5 samples taken at the outlet of the mixer): viscosity uniformity error less than 2%; composition analysis (determined by GC-MS): deviation of each component in the material within ±1%;

[0169] Conclusion: Through the action of the high-efficiency mixer, the raw material mixing realizes rapid and uniform distribution, ensuring the stability of the subsequent reaction.

[0170] Example 2: Precise reaction control test

[0171] Purpose of the experiment: to verify the influence of the reaction kettle on the stability of the polymerization reaction under different temperature control conditions.

[0172] Experimental conditions:

[0173] The formula is the same as in Example 1;

[0174] The temperature is set to 65°C, 70°C and 75°C;

[0175] Reaction time: 2 hours;

[0176] Stirring speed: 250 RPM;

[0177] Experimental data:

[0178]

[0179] Conclusion: The high-precision temperature control system of the reaction kettle ensures the stability of the reaction, and when the temperature control is at 70°C, the product performance is best.

[0180] Example 3: Solvent recovery efficiency test

[0181] Purpose of the experiment: to verify the recovery efficiency of the condenser and adsorption device for solvent volatiles.

[0182] Experimental conditions:

[0183] Reaction system: same as Example 1;

[0184] Volatile solvent: isopropyl alcohol;

[0185] Condensation temperature: 10°C;

[0186] Adsorption material: activated carbon;

[0187] Recovery time: 30 minutes;

[0188] Experimental data:

[0189] Original volatile amount: 1200g;

[0190] Condensed recovery amount: 1100g;

[0191] Adsorption recovery amount: 85g;

[0192] Total recovery efficiency: 98.1%;

[0193] Conclusion: The combination of condenser and adsorption device can effectively recover volatile solvents and significantly reduce environmental pollution.

[0194] Example 4: Efficiency test of dehydration treatment

[0195] Purpose of the experiment: To verify the improvement effect of vacuum drying machine and centrifugal separation device on dehydration efficiency.

[0196] Experimental conditions:

[0197] Initial moisture content: 45%;

[0198] Vacuum drying temperature: 50°C;

[0199] Centrifugal separation speed: 3000 RPM;

[0200] Treatment time: 60 minutes;

[0201] Experimental data:

[0202] Initial sample weight: 1000g;

[0203] Sample weight after drying: 550g;

[0204] Moisture content decreased to: ≤5%;

[0205] Conclusion: Vacuum drying machine and centrifugal separation device effectively reduce the moisture content in the product, ensuring the drying quality of the final product.

[0206] Example 5: Quality and application performance test of finished product

[0207] Purpose of the experiment: To verify the quality indicators and application performance of the final product.

[0208] Experimental conditions:

[0209] Formula same as Example 1;

[0210] Product form: gel and powder;

[0211] Application test: Test the thickening performance and stability of carbomer under different pH conditions;

[0212] Experimental data:

[0213] Gel transparency: 99%;

[0214] Powder fineness: 120 mesh;

[0215] Thickening performance (solution viscosity):

[0216] pH = 6.0: 27000 mPa s;

[0217] pH = 7.0: 31000 mPa s;

[0218] Conclusion: The finished carbomer has high transparency, excellent thickening performance and stability, meeting the needs of industrial applications.

[0219] Synthesis Conclusion

[0220] The above experimental results fully demonstrate the beneficial effects of the invention:

[0221] 1. The high-efficiency mixing mechanism ensures uniformity and mixing efficiency of the material.

[0222] 2. Precise temperature control and stirring control technology stabilizes the polymerization reaction and improves product quality.

[0223] 3. The solvent recovery system significantly reduces the waste and environmental pollution of volatile solvents.

[0224] 4. Product dehydration technology optimizes drying efficiency and product quality.

[0225] 5. Through standardized processes, the prepared carbomer product has excellent performance and can adapt to different industrial application scenarios.

[0226] Example 6

[0227] A production process for carbomer, the material ratio is as follows: acrylic acid: 100 parts, crosslinking agent (ethylene glycol diacrylate): 0.5 parts; initiator (ammonium persulfate): 0.2 parts; solvent (ethanol): 120 parts; water: 80 parts; pH adjuster (triethanolamine): appropriate amount

[0228] The process steps are as follows

[0229] 1. Raw material preparation: weigh the above raw materials according to the proportion, and place the acrylic acid, crosslinking agent, initiator and solvent in the storage tank respectively.

[0230] 2. Solution mixing: Add 80 parts of water to the reaction kettle and start the stirring device. Slowly add acrylic acid and crosslinking agent, and keep the stirring speed at 150 rpm.

[0231] 3. Polymerization reaction: heat to 70℃, add initiator solution, control the reaction time for 3 hours, and observe the formation of transparent gel.

[0232] 4. Post-processing: Transfer the reaction product to a vacuum drying device, control the temperature at 50℃, dry for 8 hours, and adjust the pH to 6.5.

[0233] 5. Packaging: After drying, the carbomer is processed by a pulverizer, sieved, weighed according to specifications, and sealed and packaged.

[0234] The experimental data are as follows: gel transparency: 96%, viscosity (1% aqueous solution, 25°C): 32000 mPa-s, pH stability: stable for 48 hours within the range of pH 6.0-7.0.

[0235] Example 7

[0236] A production process of carbomer, the material ratio is as follows: acrylic acid: 100 parts, crosslinking agent (pentaerythritol triacrylate): 1 part, initiator (benzoyl peroxide): 0.5 parts; solvent (isopropyl alcohol): 100 parts; water: 70 parts, pH adjuster (sodium hydroxide): appropriate amount

[0237] The process steps are as follows

[0238] 1. Raw material preparation: acrylic acid, crosslinking agent, initiator and solvent are respectively placed in the storage tank, and water is weighed and added to the reaction kettle.

[0239] 2. Solution mixing: slowly add acrylic acid into water, then add crosslinking agent, control the stirring speed at 200 rpm.

[0240] 3. Polymerization: heat to 75°C, gradually add initiator solution, maintain temperature and stir for 2 hours. 4. Post-processing: drying temperature is 55°C, vacuum drying for 10 hours, adjust pH to 6.0.

[0241] 5. Packaging: seal and package after crushing and sieving.

[0242] The experimental data are as follows: gel transparency: 94%, viscosity (1% aqueous solution, 25°C): 30000 mPa-s, water absorption ratio: 250g of water absorption for 1g product, and the water absorption performance is remarkable.

[0243] Example 8

[0244] A production process of carbomer, the material ratio is as follows: acrylic acid: 100 parts, crosslinking agent (ethylene glycol diacrylate and pentaerythritol triacrylate, ratio 1:1): 0.75 parts, initiator (ammonium persulfate and benzoyl peroxide, ratio 1:1): 0.4 parts, solvent (ethanol and isopropyl alcohol, ratio 1:1): 150 parts, water: 100 parts, pH adjuster (triethanolamine and sodium hydroxide, ratio 1:1): appropriate amount

[0245] The process steps are as follows

[0246] 1. Raw material preparation: weigh the raw materials and add them to the storage tank respectively.

[0247] 2. Solution mixing: add water to the reaction kettle, maintain the stirring speed at 300 rpm, and then add acrylic acid, crosslinking agent and initiator in sequence.

[0248] 3. Polymerization: the temperature is raised to 80℃ and maintained for 3 hours, and the viscosity change is monitored.

[0249] 4. Post-treatment: the vacuum drying temperature is 45℃, the time is 12 hours, the pH is adjusted to 7.0, and the dried product is sieved.

[0250] 5. Packaging: the finished product is sealed and packaged.

[0251] Experimental data, gel transparency: 98%, viscosity (1% aqueous solution, 25℃): 35000 mPa·s, water absorption ratio: 270g of water absorption per 1g of product, salt resistance: viscosity retention rate reaches 80% in 0.5mol / L sodium chloride solution.

[0252] Technical effect comparison

[0253]

[0254] From the experimental data, it can be seen that different raw material ratios and process conditions can all prepare carbomers with excellent performance, and the comprehensive performance of Example 8 is the best, especially in terms of viscosity and water absorption ratio, which shows significant technical advantages and meets the demand for high-performance carbomer products.

[0255] Although the present application has been disclosed with the preferred embodiments as above, it is not intended to limit the present application. Those skilled in the art can make various modifications and improvements without departing from the spirit and scope of the present application. Therefore, the protection scope of the present application shall be subject to the scope defined by the claims.

Claims

1. A system for producing carbomer, characterized by: It includes: Raw material mixing mechanism, the raw material mixing mechanism includes several storage tanks (1), metering pump (2) and high efficiency mixer (3), storage tank (1) is used for storing monomer, crosslinking agent and initiator respectively, each storage tank (1) top is equipped with sealing cover and exhaust port, the bottom of the storage tank (1) is connected to metering pump by pipeline, metering pump (2) is connected with the bottom of storage tank, for delivering raw materials to high efficiency mixer (3) according to the set proportion;High efficiency mixer (3) is connected with metering pump through feed pipe (4), the high efficiency mixer (3) is built-in multi-blade high-speed stirring paddle; Polymerization reactor (5), the polymerization reactor (5) is connected with the outlet of high efficiency mixer (3), the polymerization reactor (5) is provided with high-precision temperature control system, stirrer (7) and gas-tight sealing structure (8); The temperature control system includes a plurality of temperature sensors, heating unit and cooling unit, the temperature in the kettle is adjusted by jacket structure, the stirrer (7) is located in the kettle, the stirrer (7) is driven by variable speed motor, and the stirring speed is adjusted according to the reaction viscosity; The sealing structure (8) includes a sealing ring and an exhaust valve, the sealing ring and the exhaust valve are arranged on the kettle cover to prevent solvent evaporation; Solvent recovery mechanism, the solvent recovery mechanism is connected with the exhaust valve of polymerization reactor (5) through pipeline, for recovering the solvent volatilized in the production process; The solvent recovery mechanism includes condenser (9) and adsorption device (10), the volatile solvent is condensed into liquid by the condenser (9), the adsorption device (10) is connected to the outlet of condenser (9) through pipeline, the adsorption device (10) is built-in activated carbon or adsorption resin, for further absorbing uncondensed solvent; Product dehydration mechanism, the product dehydration mechanism is connected with the discharge port at the bottom of polymerization reactor (5), and the product dehydration mechanism is used for removing water and solvent in carbomer reaction product; The product dehydration mechanism includes vacuum drying machine (11) and centrifugal separation device (12), the vacuum drying machine (11) includes a heating plate and a vacuum pump, which is used for removing solvent in low temperature environment, and the centrifugal separation device (12) separates excess liquid from solid by centrifugal force; Packaging mechanism, the packaging mechanism includes automatic weighing device and sealing device, which is used for packaging the dehydrated finished product, the packaging mechanism includes automatic weighing device (13) and sealing device (14), the automatic weighing device (13) is connected with the outlet of dehydration device, which is used for accurate weighing, and the sealing device (14) includes sealing machine and vacuum packaging device, which is used for sealing and packaging the finished product; The polymerization reactor (5) is provided with temperature sensor and pressure sensor, the temperature sensor and pressure sensor are used for detecting reaction conditions respectively;Solvent recovery mechanism is provided with gas concentration sensor, the gas concentration sensor is used for monitoring solvent volatilization;Dehydration mechanism is provided with humidity sensor, the humidity sensor is used for judging whether the dehydration process is completed or not; The polymerization reactor (5) is provided with pH sensor, viscometer and solid content analyzer; The polymerization reactor (5) is provided with a heating unit and a pressure control unit, the heating unit is an electric heater, and the pressure control unit is a pressure valve; The control system comprises a PLC, and the temperature sensor, the pressure sensor, the pH sensor, the viscometer stirrer and the electric heater are connected with the PLC, and the PLC performs temperature adjustment of the polymerization reaction through the following process: Step one, data acquisition and preprocessing; The following variables are collected from the sensor: Temperature - T measured (t), pressure P measured (t), viscosity η measured (t), pH value pH measured (t); De-noising processing, using the moving average method to smooth the original data collected, filter out noise: Wherein, X(t) is the real-time acquisition value, N is the size of the sliding window; Error calculation formula: e T (t) = T target -T filtered (t); e P (t) = P target - P filtered (t); e S (t) = η target -η filtered (t); e T (t): Temperature error, temperature error at time t, unit ℃; T target : target temperature, preset ideal temperature value, unit ℃; T measured (t): current measured temperature value, unit °C; e P (t): pressure error, pressure error at time t, unit: MPa; P target : target pressure, preset ideal pressure value, unit: Mpa; P measured (t): the current measured pressure value, the pressure obtained by real-time monitoring of the system, unit: MPa; e S (t): error in stirring speed, error in viscosity at time t, mPa-s; η target : target viscosity, preset ideal viscosity value, unit: mPa·s; η measured (t): the viscosity value of the current measurement, the viscosity value obtained by real-time monitoring of the system, unit: mPa·s; Step two: fuzzy control rule; The input error e T , e P , e S and the output adjustment value ΔT, ΔP, ΔS define a membership function, which is triangularly distributed: a, b, c are threshold values of the membership function; If e T is "high", increase ΔT; if e P is "low", decrease ΔP; if e S is "high", decrease ΔS; Fuzzy control output calculation: Delta T: temperature adjustment value, adjust the output of the heating or cooling system; Delta P: pressure adjustment value, adjust the output of the pressure system; Delta S: stirring speed adjustment value, adjust the speed of the stirrer; w i : weight value of the ith fuzzy rule, indicating the influence degree of the rule on the final adjustment amount; μ(e T ) : membership function value of temperature error e T , representing fuzzy membership of temperature error; μ(e P ) : membership function value of pressure error e P , representing fuzzy membership of pressure error; μ(e S ) : membership function value of the stirring speed error e S , indicating the fuzzy membership of the stirring speed error; N: the number of fuzzy rules, each rule will give an adjustment value; Step three, PID controller parameter self-tuning; Each adjustment amount is calculated by PID control, and the formula is as follows: Δu T (t): temperature control adjustment, i.e. adjustment of the control output of the heating / cooling system in accordance with the temperature error; K pT : proportional gain of temperature control, indicating the weight of the proportional control part; K iT : integral gain of temperature control, indicating the weight of the integral control part; K dT : temperature control differential gain, indicating the weight of the differential control part; e T (t): temperature error, representing the difference between the target temperature and the current temperature; ∫e T (t): integral part of temperature error, indicating the cumulative value of error; The differential part of the temperature error indicates the rate of change of the error. The PID controller parameters are dynamically adjusted by fuzzy control: K pT , K iT , K dT is a gain parameter of the PID controller, μ(e T ) is the fuzzy controller output; The PID control parameters of the pressure and stirring speed are adjusted in the same way.

2. The carbomer production system of claim 1, wherein: The main body of the polymerization reactor (5) is made of corrosion-resistant material, and a jacket heating structure is arranged outside for heating or cooling the reaction liquid.

3. The carbomer production system of claim 1, wherein: The storage tank (1), the metering pump (2) and the high-efficiency mixer (3) are connected through quick-assembly pipelines; the polymerization reactor (5) and the solvent recovery mechanism are connected through high-temperature-resistant pipelines, and flow control valves are arranged on the pipelines; the polymerization reactor (5) and the product dehydration mechanism are connected through a delivery pump, and a filter screen is arranged at the inlet of the delivery pump to prevent solid particles from blocking the pipeline; all the equipment is fixed on standardized bases, and unified regulation and control is realized through a central control system.

4. A process for the production of carbomer characterized by: The production system of the carbomer according to any one of claims 1-3 further comprises the following steps: Step one, preparing raw materials, the raw materials include 100 parts of acrylic acid, 0.5-1 part of crosslinking agent, 0.2-0.5 part of initiator, 100-150 parts of solvent, appropriate amount of pH regulator, 50-100 parts of water, acrylic acid as the main monomer, providing the basic structure of the carbomer, and the acrylic acid, crosslinking agent, initiator and solvent are weighed according to the proportion and placed in the storage tank respectively; water is added to the reaction kettle, and stirring is started to maintain a uniform liquid environment; Step two, solution mixing, slowly add the acrylic acid and crosslinking agent into the reaction kettle while maintaining stirring; add the initiator solution, and control the stirring speed at 100-300 revolutions per minute to ensure uniform mixing; control the temperature at 25-35 DEG C to avoid excessive reaction rate; Step three, polymerization reaction, start the heating system, and raise the temperature of the reaction kettle to 65-80 DEG C; when the reaction starts, observe the viscosity change of the system and adjust the stirring speed; the reaction time is 2-4 hours, and a transparent gel-like polymer is formed after the reaction is completed; Step four, post-treatment, transfer the reaction product to a vacuum drying device, control the temperature below 60 DEG C, and remove the solvent and moisture; adjust the pH to the range of 6.0-7.0 to ensure that the carbomer has good application performance; if powder carbomer is needed, further crushing and sieving treatment is needed. Step five packaging, after drying the carbomer transfer to the packaging machine, according to the specification automatic weighing and sealing package, prevent moisture absorption.

5. The process for the production of carbomer according to claim 4, characterized in that: The crosslinking agent is one or both of ethylene glycol diacrylate or pentaerythritol triacrylate, which gives the carbomer gel network structure.

6. The process for the production of carbomer according to claim 4, characterized in that: The initiator is one or both of ammonium persulfate or benzoyl peroxide, which is used to initiate the polymerization reaction.

7. The process for production of carbomer as claimed in claim 4 wherein: The solvent is isopropyl alcohol or ethanol, which is used as a dispersion medium to reduce the by-products during the reaction process.

8. The process for production of carbomer as claimed in claim 4 wherein: The pH regulator is selected from sodium hydroxide or triethanolamine.

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