Method and system for controlling vacuum degree of glue mixing and preparing reaction kettle

Abstract

The invention discloses a method and a system for controlling the vacuum degree of a glue mixing and preparing reaction kettle, and relates to the technical field of reaction equipment. Comprising the following steps: S1, acquiring global viscosity distribution, axial / radial temperature gradient and a filler phase separation critical point, and monitoring a colloid rheological-dielectric-thermodynamic state in real time; s2, establishing a colloidal state coupling model, and determining a target vacuum degree; and S3, according to the vacuum degree deviation, the axial temperature gradient of the reaction kettle and the dielectric change rate, the opening degree of the magnetic suspension valve, the stirring rotating speed and the flow of the regulator are cooperatively adjusted. According to the method, global viscosity distribution is monitored in real time through the shear wave-ultrasonic wave combined viscometer and is combined with the temperature gradient and the dielectric change rate, so that the vacuum degree is dynamically adjusted, the vacuum degree can be adaptively adjusted according to the colloid state, local excessive air exhaust is avoided, the solvent evaporation rate balance is maintained, and the product quality is improved. And the surface layer curing risk is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction equipment, and specifically provides a method and system for controlling the vacuum degree of a glue mixing and glue making reaction kettle. Background Art

[0002] In the preparation process of materials such as adhesives and resins, the glue mixing and glue making reaction kettle is one of the core equipment, and its process conditions directly affect the performance and quality of the final product. As a key link of the reaction kettle, vacuum degree control is mainly applied to processes such as dehydration, impurity removal, and maintaining a pure reaction environment, and is of great significance for shortening the production cycle, improving the purity and stability of products.

[0003] Chinese invention patent with the publication number of CN114870761A discloses an intelligent safety temperature control method applied to a calorimetric reaction kettle. The invention collects the sample temperature through a double-branch platinum resistance, calculates the oil bath feedforward quantity at the target temperature, and outputs the oil bath target temperature; determines whether the temperature difference between the sample temperature and the target temperature exceeds a predetermined deviation, and if it exceeds, the maximum value of the temperature difference between the sample temperature and the target temperature is updated in real time; when the temperature difference is less than 60% of the maximum temperature difference, the oil bath temperature is dynamically adjusted according to the proportion of the temperature difference to the maximum temperature difference; when the temperature difference is less than 30% of the maximum temperature difference, self-learning is carried out by using a BP neural network according to the temperature difference between the sample temperature and the sample target temperature, the oil bath target temperature, and the sample temperature, and the optimal control parameters are output. The invention gives full play to the advantages of each control strategy and realizes intelligent, safe, and precise temperature control of the reaction kettle.

[0004] However, during the vacuum degassing process of the glue mixing and glue making reaction kettle, high-viscosity colloids (such as epoxy resin, polyurethane, etc.) in a vacuum environment will cause local concentration increase on the surface layer of the colloid due to the too fast solvent evaporation rate, resulting in the phenomenon of pre-curing. At the same time, under the action of negative pressure, components with large density differences inside the colloid (such as fillers, thickeners) will undergo phase separation to form stratification. For the existing reaction kettle vacuum degree control methods, when pumping air with a fixed vacuum degree, there is a lack of real-time viscosity monitoring. Therefore, not only can it not inhibit the curing defects caused by the solvent evaporation gradient, but it is also difficult to eliminate the stratification phenomenon through equipment structure optimization. Summary of the Invention

[0005] The purpose of the present invention is to provide a method and system for controlling the vacuum degree of a glue mixing and glue making reaction kettle to solve the problems raised in the above background art.

[0006] To achieve the above purpose, the present invention provides the following technical solution: A method for controlling the vacuum degree of a glue mixing and glue making reaction kettle includes:

[0007] S1: Obtain the rheological-dielectric-thermodynamic composite parameters of the colloid: Through a shear wave-ultrasonic combined viscometer, a distributed optical fiber temperature measurement network, and a broadband dielectric spectrometer, obtain the global viscosity distribution, axial / radial temperature gradient, and the critical point of filler phase separation, and monitor the rheological-dielectric-thermodynamic state of the colloid in real time;

[0008] S2: Determine the compensation vacuum degree: According to the rheological-dielectric-thermodynamic state of the colloid, establish a colloid state coupling model to determine the target vacuum degree;

[0009] S3: Coordinated adjustment: According to the target vacuum degree and the current vacuum degree, obtain the vacuum degree deviation. At the same time, according to the vacuum degree deviation, the axial temperature gradient of the reaction kettle, and the dielectric change rate, coordinately adjust the opening degree of the magnetic suspension valve, the stirring speed, and the flow rate of the regulator, including:

[0010] S3.1: Normalization processing: According to the set vacuum degree deviation threshold, maximum temperature gradient threshold, and the critical value of the dielectric change rate, perform normalization processing on the vacuum degree deviation magnitude, temperature gradient, and dielectric change rate. Specifically:

[0011]

[0012] Among them: is the normalized vacuum deviation, is the vacuum degree deviation, is the vacuum deviation threshold, is the normalized temperature gradient, is the axial temperature gradient of the reaction kettle, is the maximum temperature gradient threshold, is the normalized dielectric change rate, is the change rate of the loss tangent value, is the critical value of the dielectric change rate;

[0013] S3.2: Determine the adjustment amount: According to the vacuum degree deviation magnitude, temperature gradient, and dielectric change rate after normalization processing, determine the adjustment amount of the magnetic suspension valve opening degree, the stirring speed adjustment amount, and the regulator flow rate adjustment amount, and through the PLC controller, adjust and control the valve current, the output frequency of the frequency converter, and the peristaltic pump speed;

[0014] S3.3: Real-time adjustment: According to the adjusted valve current, the output frequency of the frequency converter, and the peristaltic pump speed, coordinately perform vacuum adjustment, mechanical stirring, and chemical injection.

[0015] Furthermore, real-time monitoring of the rheological-dielectric-thermodynamic state of the colloid includes:

[0016] S1.1: Measurement by shear wave - ultrasonic combined viscometer: Electromagnetic exciters are symmetrically installed on the side wall of the reaction kettle, and ultrasonic probes are arranged at the top and bottom of the reaction kettle. Through the electromagnetic exciters and ultrasonic probes, the storage modulus and dynamic viscosity are obtained, specifically as follows:

[0017]

[0018] Among them: is the storage modulus, is the colloid density, is the shear wave velocity, is the dynamic viscosity, is the ultrasonic propagation time difference, is the material acoustic impedance constant, is the ultrasonic probe spacing;

[0019] S1.2: Monitoring by distributed optical fiber temperature measurement network: The optical fiber is wound in a spiral along the axis of the reaction kettle, covering the height and radius of the reaction kettle, and the optical fiber is connected to the input port of the OFRD demodulator through a splitter to obtain the axial / radial temperature gradient of the reaction kettle, specifically as follows:

[0020]

[0021] Among them: is the axial temperature gradient of the reaction kettle, is the top temperature of the reaction kettle, is the bottom temperature of the reaction kettle, is the height of the reaction kettle, is the radial temperature gradient of the reaction kettle, is the temperature in the central area of the reaction kettle, is the wall temperature of the reaction kettle, is the radius of the reaction kettle;

[0022] S1.3: Identification by broadband dielectric spectrometer: An electrode assembly is vertically inserted in the middle inside the reaction kettle, and through the electrode assembly, the dielectric constant and loss factor corresponding to different packing states are obtained, and the tangent value of the loss angle is determined, specifically as follows:

[0023]

[0024] Among them: is the tangent value of the loss angle, is the dielectric constant, is the loss factor.

[0025] Further, the electrode assembly is arranged as a coaxial annular electrode structure, and the distance between the inner electrode diameter and the outer electrode inner diameter is set to 2 mm. Meanwhile, there is a distance between the bottom end of the electrode assembly and the inner bottom end of the reactor.

[0026] Further, determining the target vacuum degree includes:

[0027] S2.1: Determine the comprehensive compensation vacuum degree: According to the rheological-dielectric-thermodynamic state of the colloid, establish a colloid state coupling model, specifically:

[0028]

[0029] Where: is the compensation vacuum degree after comprehensive compensation, is the viscosity compensation coefficient, is the modulus compensation coefficient, is the dielectric loss compensation coefficient, is the dynamic viscosity, is the storage modulus, is the change rate of the loss tangent value, is the reference value of the storage modulus, is the reference value of the dynamic viscosity;

[0030] S2.2: Perform temperature gradient correction: Compare the axial temperature gradient of the reactor with the preset temperature gradient threshold, and according to the comparison result, perform temperature gradient correction to obtain the compensation vacuum degree of temperature gradient correction, specifically:

[0031]

[0032] Where: is the compensation vacuum degree of temperature gradient correction, is the axial temperature gradient of the reactor;

[0033] S2.3: Obtain the target vacuum degree: According to the compensation vacuum degree after comprehensive compensation and the compensation vacuum degree of temperature gradient correction, obtain the final compensation vacuum degree, and through the initial setting value of the vacuum degree, obtain the target vacuum degree, specifically:

[0034]

[0035] Where: is the target vacuum degree, is the compensation vacuum degree after comprehensive compensation, is the compensation vacuum degree of temperature gradient correction, is the initial setting value of the vacuum degree.

[0036] Furthermore, according to the comparison result, temperature gradient correction is performed, specifically as follows:

[0037] When the axial temperature gradient of the reactor is greater than the preset temperature gradient threshold, temperature gradient correction is performed; otherwise, no temperature gradient correction is performed.

[0038] Furthermore, adjustment control is performed on the valve current, the output frequency of the frequency converter, and the rotation speed of the peristaltic pump, including:

[0039] S3.2.1: Determine the valve current: Determine the opening adjustment amount according to the normalized vacuum degree deviation and the vacuum adjustment coefficient, and obtain the adjusted valve current value according to the opening adjustment amount and the initial current value, specifically as follows:

[0040]

[0041] Where: is the adjusted valve current value, is the initial current value, is the opening adjustment amount, is the current-opening conversion coefficient;

[0042] S3.2.2: Determine the output frequency of the frequency converter: Determine the stirring speed adjustment amount according to the normalized temperature gradient and the temperature gradient coefficient, and obtain the output frequency of the frequency converter according to the stirring speed adjustment amount and the current stirring speed, specifically as follows:

[0043]

[0044] Where: is the output frequency of the frequency converter, is the current stirring speed, is the stirring speed adjustment amount;

[0045] S3.2.3: Determine the rotation speed of the peristaltic pump: Determine the regulator flow adjustment amount according to the normalized dielectric change rate and the dielectric sensitivity coefficient, and obtain the rotation speed of the peristaltic pump according to the regulator flow adjustment amount and the current regulator flow rate, specifically as follows:

[0046]

[0047] Where: is the rotation speed of the peristaltic pump, is the current regulator flow rate, is the regulator flow adjustment amount.

[0048] Furthermore, the acquisition formulas for the opening adjustment amount, the stirring speed adjustment amount, and the regulator flow adjustment amount are specifically as follows:

[0049]

[0050] Wherein: is the opening adjustment amount, is the vacuum adjustment coefficient, is the normalized vacuum deviation, is the vacuum weight factor, is the stirring speed adjustment amount, is the temperature gradient coefficient, is the normalized temperature gradient, is the temperature weight factor, is the regulator flow rate adjustment amount, is the dielectric sensitivity coefficient, is the normalized dielectric change rate, is the dielectric weight factor.

[0051] Furthermore, during the co-regulation process in step S3, the state of phase separation and the change state of the temperature gradient are monitored, and according to the abnormal state corresponding to the monitoring result, abnormal coordination processing is performed, including:

[0052] W1: Abnormal state diagnosis: Through a dielectric spectrometer, laser backscattering, and multimode quartz optical fiber, the dielectric loss change rate, phase separation index, and temperature change amount at the axial position are obtained. At the same time, the dielectric loss change rate, phase separation index, and temperature change amount at the axial position are compared with the set change rate threshold, phase separation threshold, and temperature change threshold, and according to the comparison result, the abnormal state is determined, specifically:

[0053] When the dielectric loss change rate is greater than the change rate threshold and the frequency peak of the tangent value of the loss angle decreases, the abnormal state is filler agglomeration. When the dielectric loss change rate is greater than the change rate threshold and the frequency peak of the tangent value of the loss angle increases, the abnormal state is phase separation. Otherwise, there is no abnormal state;

[0054] When the phase separation index is greater than the phase separation threshold, the abnormal state is phase separation. Otherwise, there is no abnormal state;

[0055] When the temperature change amount is greater than the temperature change threshold, the abnormal state is local overheating. Otherwise, there is no abnormal state;

[0056] W2: Co-processing: According to the abnormal state, the anti-stratification pulse sequence, curing inhibition, and lining self-repair are started co-ordinately at intervals.

[0057] Furthermore, starting the anti-stratification pulse sequence, curing inhibition, and lining self-repair co-ordinately at intervals includes:

[0058] W2.1: Implement an anti-stratification pulse sequence: Determine the agglomeration area in the reaction kettle through laser backscattering, and focus ultrasonic waves on the agglomeration area;

[0059] W2.2: Carry out curing inhibition: Spray an ethanol solution into the high-temperature area determined in the reaction kettle through a two-fluid atomizing nozzle;

[0060] W2.3: Carry out self-repair of the inner lining: Prepare microcapsules from polydimethylsiloxane, platinum catalyst and urea-formaldehyde resin, and disperse the microcapsules in an epoxy resin-based coating.

[0061] A vacuum degree control system for an adhesive mixing and making reaction kettle uses the vacuum degree control method for an adhesive mixing and making reaction kettle described in any one of the above.

[0062] Compared with the prior art, the beneficial effects of the present invention are:

[0063] Firstly: The present invention monitors the global viscosity distribution in real time through a shear wave-ultrasonic viscometer, combines it with the temperature gradient and the dielectric change rate, and thus dynamically adjusts the vacuum degree, enabling the vacuum degree to be adaptively adjusted according to the colloid state, avoiding local over-pumping, maintaining the balance of the solvent evaporation rate, and reducing the risk of surface curing;

[0064] Secondly: The present invention balances multiple variables of vacuum regulation, mechanical stirring and chemical injection through the set normalization weight factor, shortening the process cycle;

[0065] Thirdly: The present invention identifies abnormal states such as agglomeration and overheating through dielectric spectroscopy, laser backscattering, and optical fiber temperature measurement, and focuses ultrasonic waves to break agglomerates, atomize ethanol for cooling, and automatically repair the damage to the inner wall of the reaction kettle with a microcapsule coating for corresponding treatment, which can not only shorten the abnormal response time, but also extend the equipment life. Description of the Drawings

[0066] Figure 1 It is a schematic flow chart of the vacuum degree control method for the adhesive mixing and making reaction kettle of the present invention;

[0067] Figure 2 It is a schematic flow chart of obtaining the target vacuum degree of the present invention;

[0068] Figure 3 It is a comparative analysis chart of the energy consumption of the solution of the present invention;

[0069] Figure 4 It is a comparative chart of the response time of the solution of the present invention;

[0070] Figure 5 It is a comparative chart of the recovery rate of the solution of the present invention. Detailed Embodiments

[0071] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0072] During the vacuum degassing process of the existing glue mixing and making reaction kettle, for high-viscosity colloids (such as epoxy resin, polyurethane, etc.) in a vacuum environment, due to the too fast solvent evaporation rate, the local concentration on the surface layer of the colloid will increase, resulting in the phenomenon of pre-curing. At the same time, under the action of negative pressure, components with large density differences inside the colloid (such as fillers, thickeners) will undergo phase separation to form stratification. For the existing reaction kettle vacuum degree control method, when using a fixed vacuum degree for pumping, there is a lack of real-time viscosity monitoring. Therefore, it is not only impossible to inhibit the curing defects caused by the solvent evaporation gradient, but also difficult to eliminate the stratification phenomenon through equipment structure optimization. The technical solution of this application obtains the global viscosity distribution, axial / radial temperature gradient, and the critical point of filler phase separation, monitors the rheological-dielectric-thermodynamic state of the colloid in real time, and based on this, establishes a colloid state coupling model, obtains the comprehensive compensation vacuum degree, and combines it with the temperature compensation vacuum degree to dynamically adjust the vacuum degree. At the same time, according to the obtained vacuum degree, the axial temperature gradient of the reaction kettle, and the dielectric change rate, the opening degree of the magnetic suspension valve, the stirring speed, and the flow rate of the regulator are synergistically adjusted, thereby not only avoiding local over-pumping, maintaining the balance of the solvent evaporation rate, reducing the surface curing risk, but also shortening the process cycle.

[0073] Embodiment 1

[0074] Reference Figure 1 And Figure 2 This embodiment provides a method for controlling the vacuum degree of a glue mixing and making reaction kettle. The method for controlling the vacuum degree of the glue mixing and making reaction kettle includes the following steps:

[0075] Step S1: Obtain the rheological-dielectric-thermodynamic composite parameters of the colloid. That is, measure the global viscosity distribution through a shear wave-ultrasonic combined viscometer, monitor the axial / radial temperature gradient through a distributed optical fiber temperature measurement network, and identify the critical point of filler phase separation through a broadband dielectric spectrometer. At the same time, according to the obtained global viscosity distribution, axial / radial temperature gradient, and the critical point of filler phase separation, monitor the rheological-dielectric-thermodynamic state of the colloid in real time. Specifically as follows:

[0076] Step S1.1: Measurement by shear wave - ultrasonic combined viscometer. That is, install the same number of electromagnetic exciters symmetrically on the side wall of the reaction kettle, and the distance between adjacent two electromagnetic exciters is not less than 30 cm to avoid standing wave interference. At the same time, set the same number of ultrasonic probes at the top and bottom of the reaction kettle respectively, and form a cross - measurement path.

[0077] Furthermore, adjust the amplitude of the electromagnetic exciter through current, and synchronize the electromagnetic exciter with the clock of the data acquisition card. At the same time, apply shear waves in the state of an empty kettle to measure the background vibration noise, and inject standard silicone oil into the reaction kettle. Adjust the shear wave velocity by adjusting the excitation current. And obtain the propagation waveform of the electromagnetic exciter through a piezoelectric accelerometer, and obtain the corresponding storage modulus, specifically:

[0078]

[0079] Where: is the storage modulus, is the colloid density, is the shear wave velocity.

[0080] Furthermore, through the pulse wave signal emitted by the ultrasonic probe and the received echo signal, obtain the time difference of ultrasonic wave propagation in different colloids, and obtain the corresponding dynamic viscosity, specifically:

[0081]

[0082] Where: is the dynamic viscosity, is the ultrasonic wave propagation time difference, is the material acoustic impedance constant, is the ultrasonic probe spacing.

[0083] During the specific implementation process, install 4 groups of electromagnetic exciters symmetrically on the side wall of the reaction kettle, and set the distance between adjacent two electromagnetic exciters to 30 cm. Set a pair of 5 MHz ultrasonic probes at the top and bottom of the reaction kettle respectively. At the same time, set the incident angle to 30°, set the distance between adjacent two ultrasonic probes to 10 cm, and use a high - temperature silicone grease couplant to form a 0.2 mm thick acoustic guide layer on the surface of the ultrasonic probe.

[0084] Furthermore, at a temperature of 25 °C, the shear wave velocity of epoxy resin is 2.1 m / s, and its corresponding storage modulus is 1.2*10 6 Pa. Furthermore, when the ultrasonic probe spacing is set to 10 cm, the time difference of ultrasonic wave propagation in epoxy resin is 28 μs, and the dynamic viscosity is 12500 cP.

[0085] Step S1.2: Distributed optical fiber temperature measurement network monitoring. That is, along the axis of the reactor, multiple optical fibers are spirally wound to cover the height and radius of the reactor. In this embodiment, 8 optical fibers are spirally wound along the axis of the reactor, and the starting point and ending point of each optical fiber are marked with different color rings. Further, each optical fiber is connected to the input port of the OFRD demodulator through a splitter to obtain the temperature at each optical fiber position, so as to determine the axial / radial temperature gradient of the reactor. Specifically:

[0086]

[0087] Where: is the axial temperature gradient of the reactor, is the top temperature of the reactor, is the bottom temperature of the reactor, is the height of the reactor, is the radial temperature gradient of the reactor, is the temperature in the central area of the reactor, is the wall temperature of the reactor, is the radius of the reactor.

[0088] In the process of specific implementation, the average temperature corresponding to the first optical fiber channel and the second optical fiber channel is set as the top temperature of the reactor, which is 85 °C. The average temperature corresponding to the seventh optical fiber channel and the eighth optical fiber channel is set as the bottom temperature of the reactor, which is 78 °C. At the same time, the height of the reactor is 1.2 m, so the axial temperature gradient of the reactor is 5.8 °C / m.

[0089] Further, the average temperature corresponding to the third optical fiber channel and the fourth optical fiber channel is set as the central temperature of the reactor, which is 82 °C. At the same time, the wall temperature of the reactor is 80 °C, and the radius of the reactor is 0.3 m, so the radial temperature gradient of the reactor is 6.7 °C / m.

[0090] Step S1.3: Broadband dielectric spectrometer identification. That is, an electrode assembly is vertically inserted in the middle inside the reactor, and the end of the electrode assembly does not contact the bottom of the reactor. Through the set electrode assembly, the dielectric spectrum data of the filler in different states is obtained.

[0091] Further, the electrode assembly in this embodiment is a coaxial ring electrode structure, and the distance between the inner electrode diameter and the outer electrode inner diameter is set to 2 mm. Specifically, the inner electrode diameter in this embodiment is set to 8 mm, the outer electrode inner diameter is set to 10 mm, and the effective area is set to 4 cm 2 . And the distance between the bottom of the electrode assembly and the inner bottom end of the reactor is set to 0.5 m to avoid stirring interference.

[0092] In the process of specific implementation, a sinusoidal swept-frequency signal of 1 V is applied to the coaxial annular electrode, and dielectric spectrum data is collected every 5 seconds. Specifically, when the peak frequency of the tangent of the loss angle is at a high frequency, the filler is dispersed and in the normal state. Conversely, when the peak frequency of the tangent of the loss angle is at a low frequency, the filler agglomerates and is in the phase separation state.

[0093] Furthermore, when the peak frequency of the tangent of the loss angle is 1 MHz, the filler is dispersed and in the normal state. At the same time, the corresponding dielectric constant is 3.2 and the loss factor is 0.15. Furthermore, when the peak frequency of the tangent of the loss angle is 10 kHz, the filler agglomerates and is in the phase separation state. At the same time, the corresponding dielectric constant is 2.9, a decrease of 9.4%, and the loss factor is 0.22, an increase of 46.7%.

[0094] In this embodiment, the acquisition formula for the tangent value of the loss angle is specifically:

[0095]

[0096] Where: is the tangent value of the loss angle, is the dielectric constant, is the loss factor.

[0097] Step S2: Determine the compensation vacuum degree. That is, according to the rheological-dielectric-thermodynamic state of the colloid obtained in step S1, a colloid state coupling model is established. That is to say, through the established colloid state coupling model, the target compensation vacuum degree is determined. Specifically as follows:

[0098] Step S2.1: Determine the comprehensive compensation vacuum degree. That is, according to the rheological-dielectric-thermodynamic state of the colloid obtained in step S1, a colloid state coupling model is established, specifically:

[0099]

[0100] Where: is the compensation vacuum degree after comprehensive compensation, is the viscosity compensation coefficient, is the modulus compensation coefficient, is the dielectric loss compensation coefficient, is the dynamic viscosity, is the storage modulus, is the change rate of the tangent value of the loss angle, is the reference value of the storage modulus, is the reference value of the dynamic viscosity.

[0101] In the process of specific implementation, the currently obtained dynamic viscosity value is 19200 cP, the reference value of the dynamic viscosity is set to 15000 cP, and the viscosity compensation coefficient is 0.2 * 10 -3 kPa / cP, so the corresponding viscosity compensation term is 0.84 kPa. Further, the currently obtained storage modulus value is 1.8 * 10 6 Pa, the reference value of the storage modulus is set to 1.2 * 10 6 Pa, and the modulus compensation coefficient is 0.05 kPa / MPa, so the corresponding modulus compensation term is 0.03 kPa. Further, the change rate of the currently obtained loss tangent value is -0.025 / min, and the dielectric loss compensation coefficient is 10 kPa, so the corresponding dielectric compensation term is -0.25 kPa. That is to say, through the obtained viscosity compensation term, modulus compensation term and dielectric compensation term, the compensated vacuum degree after comprehensive compensation can be determined, which is: 0.84 + 0.03 - 0.25 = 0.62 kPa.

[0102] Step S2.2: Perform temperature gradient correction. That is, according to the axial temperature gradient of the reaction kettle obtained in step S1.2, compare the obtained axial temperature gradient with a preset temperature gradient threshold (which can be specifically set according to actual needs, so it is not specifically described in this embodiment). When the obtained axial temperature gradient is greater than the preset temperature gradient threshold, temperature gradient correction is required; otherwise, temperature gradient correction is not required.

[0103] In this embodiment, when performing temperature gradient correction, the compensated vacuum degree of the corresponding temperature gradient correction is specifically:

[0104]

[0105] Where: is the compensated vacuum degree of temperature gradient correction, is the axial temperature gradient of the reaction kettle.

[0106] In the process of specific implementation, the axial temperature gradient of the reaction kettle is 5.8 °C / m, and the preset temperature gradient threshold in this embodiment is set to 3 °C / m, that is, the obtained axial temperature gradient is greater than the preset temperature gradient threshold, so temperature gradient correction is required. That is to say, the compensated vacuum degree of the corresponding temperature gradient correction is -0.58 kPa.

[0107] Step S2.3: Obtain the target vacuum degree. That is, according to the compensated vacuum degree after comprehensive compensation obtained in step S2.1 and the compensated vacuum degree of temperature gradient correction obtained in step S2.2, obtain the final compensated vacuum degree. At the same time, according to the finally obtained compensated vacuum degree and the initial set value of the vacuum degree, specifically:

[0108]

[0109] Wherein: is the target vacuum degree, is the compensated vacuum degree after comprehensive compensation, is the compensated vacuum degree corrected by the temperature gradient, is the initial set value of the vacuum degree.

[0110] In the process of specific implementation, the compensated vacuum degree after comprehensive compensation is 0.62 kPa, and the compensated vacuum degree corrected by the temperature gradient is -0.58 kPa. Then the corresponding final compensated vacuum degree is: 0.62 - 0.58 = 0.04 kPa. At the same time, the initial set value of the vacuum degree is 80 kPa, so the target vacuum degree is 80.04 kPa.

[0111] Step S3: Coordinated adjustment. That is, according to the target vacuum degree obtained in step S2.3 and the currently monitored actual vacuum degree, and at the same time according to the actually obtained axial temperature gradient and dielectric change rate of the reaction kettle, the opening degree of the magnetic suspension valve, the stirring speed and the flow rate of the regulator are coordinately adjusted. Specifically as follows:

[0112] Step S3.1: Normalization processing. That is, according to the finally compensated vacuum degree obtained in step S2.3 and the currently monitored actual vacuum degree, the vacuum degree deviation between the two is obtained. Specifically:

[0113]

[0114] Wherein: is the vacuum degree deviation, is the actually monitored vacuum degree, is the target vacuum degree.

[0115] Furthermore, according to the set vacuum degree deviation threshold, maximum temperature gradient threshold and critical value of the dielectric change rate, the vacuum degree deviation, temperature gradient and dielectric change rate are normalized. Specifically:

[0116]

[0117] Wherein: is the normalized vacuum deviation, is the vacuum degree deviation, is the vacuum deviation threshold, is the normalized temperature gradient, is the axial temperature gradient of the reaction kettle, is the maximum temperature gradient threshold, is the normalized dielectric change rate, is the rate of change of the loss tangent value, is the critical value of the dielectric change rate.

[0118] In the process of specific implementation, the target vacuum degree is 80.04 kPa, and the actually monitored vacuum degree is 80 kPa, so the vacuum degree deviation is 0.04 kPa. At the same time, the vacuum deviation threshold is set to 0.5 kPa, so the corresponding normalized vacuum deviation is 0.08. Further, the axial temperature gradient of the reaction kettle is 5.8 °C / m, and the maximum temperature gradient threshold is set to 10 °C / m, so the corresponding normalized temperature gradient is 0.58. Further, the rate of change of the loss tangent value is -0.02 / min, and the critical value of the dielectric change rate is 0.05 / min, so the corresponding normalized dielectric change rate is -0.4.

[0119] Step S3.2: Determine the adjustment amount. That is, through the normalized vacuum deviation, normalized temperature gradient, and normalized dielectric change rate obtained in step S3.1, determine the corresponding adjustment amounts of the magnetic suspension valve opening, stirring speed, and regulator flow rate. Further, according to the obtained adjustment amounts of the magnetic suspension valve opening, stirring speed, and regulator flow rate, determine the corresponding valve current, frequency converter output frequency, and peristaltic pump speed, and perform corresponding adjustment control through the PLC controller. Specifically as follows:

[0120] Step S3.2.1: Determine the valve current. That is, according to the magnitude of the normalized vacuum degree deviation and the vacuum adjustment coefficient obtained in step S3.1, determine the corresponding opening adjustment amount, specifically:

[0121]

[0122] Where: is the opening adjustment amount, is the vacuum adjustment coefficient, is the normalized vacuum deviation, is the vacuum weight factor.

[0123] In the process of specific implementation, the vacuum adjustment coefficient is set to 15%, the normalized vacuum deviation is 0.08, and the vacuum weight factor is 1.0, so the corresponding opening adjustment amount is 1.2%.

[0124] Further, according to the determined opening adjustment amount and the magnitude of the initial current value, combine them with the current-opening conversion coefficient to obtain the corresponding adjusted valve current magnitude, specifically:

[0125]

[0126] Where: is the adjusted valve current magnitude, is the initial current value, is the opening adjustment amount, is the current-opening conversion coefficient.

[0127] In the process of specific implementation, the initial current value is set to 4.2 A, and the current-opening conversion coefficient is set to 0.1 A / %. Then the adjusted valve current value is: 4.2 A + 3% * 0.1 A / % = 7.8 A.

[0128] Specifically, through the PLC controller, a current signal of 7.8 A is sent to the proportional valve.

[0129] Step S3.2.2: Determine the output frequency of the frequency converter. That is, according to the normalized temperature gradient and the temperature gradient coefficient obtained in step S3.1, determine the corresponding stirring speed adjustment amount, specifically:

[0130]

[0131] Where: is the stirring speed adjustment amount, is the temperature gradient coefficient, is the normalized temperature gradient, is the temperature weight factor.

[0132] In the process of specific implementation, the normalized temperature gradient is 0.58, the temperature gradient coefficient is set to 5 rpm, and the temperature weight factor is set to 0.8. Then the corresponding stirring speed adjustment amount is: 5 * 0.58 * 0.8 = 2.3 rpm.

[0133] Furthermore, according to the currently set stirring speed and the obtained stirring speed adjustment amount, determine the target stirring speed, and according to the target stirring speed, determine the corresponding output frequency value of the frequency converter, specifically:

[0134]

[0135] Where: is the output frequency of the frequency converter, is the current stirring speed, is the stirring speed adjustment amount.

[0136] In the process of specific implementation, the current stirring speed is 65 rpm, and the stirring speed adjustment amount is set to 2.3 rpm. Then the corresponding target stirring speed is 67.5 rpm, that is, the corresponding output frequency value of the frequency converter is: 67.5 / 1.2 = 56.25 Hz.

[0137] Specifically, through the PLC controller, a frequency set value of 56.25 Hz is sent to the frequency converter.

[0138] Step S3.2.3: Determine the peristaltic pump speed. That is, according to the normalized dielectric change rate and dielectric sensitivity coefficient obtained in Step S3.1, determine the size of the regulator flow rate adjustment amount, specifically:

[0139]

[0140] Where: is the regulator flow rate adjustment amount, is the dielectric sensitivity coefficient, is the normalized dielectric change rate, is the dielectric weight factor.

[0141] In the process of specific implementation, the normalized dielectric change rate is -0.4, the dielectric sensitivity coefficient is set to 5 mL / min, and the dielectric weight factor is set to 0.5. Then the corresponding regulator flow rate adjustment amount is: 5 * 0.4 * 0.5 = 1 mL / min.

[0142] Furthermore, according to the determined size of the regulator flow rate adjustment amount and the currently set size of the regulator flow rate, obtain the target regulator flow rate. At the same time, according to the target regulator flow rate, determine the corresponding peristaltic pump speed size, specifically:

[0143]

[0144] Where: is the peristaltic pump speed, is the current regulator flow rate, is the regulator flow rate adjustment amount.

[0145] In the process of specific implementation, the current regulator flow rate is set to 6 mL / min. Since the regulator flow rate adjustment amount is 1 mL / min, the corresponding target regulator flow rate is 7 mL / min. That is to say, the corresponding peristaltic pump speed is: 20 * 7 = 140 rpm.

[0146] Specifically, send a pulse signal corresponding to a speed of 140 rpm to the peristaltic pump through the PLC controller. Among them, the speed of 140 rpm corresponds to a frequency of 466.7 Hz in a 2000 PPR encoder and can be set to 1600 pulses / revolution in the stepper motor driver.

[0147] Step S3.3: Real-time adjustment. That is, according to the sizes of the respective adjustment amounts determined in Step S3.2, cooperate to perform vacuum adjustment, mechanical stirring, and chemical injection. It should be noted that during the cooperative operation, the vacuum adjustment, mechanical stirring, and chemical injection are set in sequence.

[0148] In the process of specific implementation, at the initial moment, a current signal of 7.8 A is sent to the proportional valve through the PLC controller to adjust the spool position of the proportional valve for vacuum compensation. Further, a frequency set value of 56.25 Hz is sent to the frequency converter through the PLC controller to adjust the stirring speed. Further, a pulse signal corresponding to a rotational speed of 140 rpm is sent to the peristaltic pump through the PLC controller to adjust the target regulator flow rate.

[0149] Reference Figure 3 , Figure 3 is the energy consumption comparison analysis chart of the solution in this embodiment. It can be seen from Figure 3 that the energy consumption of the traditional solution is between 90 and 110 kWh, while the energy consumption of this solution is between 80 and 90 kWh. That is to say, the peak energy consumption has dropped from 110 kWh to 90 kWh, a decrease of 18%. At the same time, the average energy consumption has dropped from 100 kWh to 85 kWh, a decrease of 15%.

[0150] Reference Figure 4 , Figure 4 is the response time comparison chart of the solution in this embodiment. It can be seen from Figure 4 that the vacuum control of the traditional solution relies on manual inspection or a single sensor, resulting in a delay in fault identification, and its response time is 30 seconds. While this solution conducts real-time monitoring through laser backscattering and multimode optical fiber temperature measurement to quickly capture anomalies such as agglomeration and overheating, and combines it with the automated diagnosis of the PLC, shortening its response time to 10 seconds and increasing the response speed by 67%.

[0151] This embodiment also provides a vacuum degree control system for a glue mixing and glue making reactor, and this vacuum degree control system for a glue mixing and glue making reactor uses the vacuum degree control method for a glue mixing and glue making reactor described in the above embodiment.

[0152] Embodiment 2

[0153] This embodiment provides a vacuum degree control method for a glue mixing and glue making reactor. The specific implementation method is the same as that of Embodiment 1, and the difference is that during the coordinated operation of vacuum regulation, mechanical stirring, and chemical injection, the state of phase separation and the change state of the temperature gradient are monitored, and corresponding processing is performed according to the monitoring results. The present invention will be illustrated below in conjunction with the specific implementation manners of this embodiment.

[0154] In this embodiment, during the coordinated operation of vacuum regulation, mechanical stirring, and chemical injection, the state of phase separation and the change state of the temperature gradient are monitored in real time. When the state of phase separation and the change state of the temperature gradient are abnormal, an anti-stratification pulse sequence and a curing inhibition strategy are triggered through a self-repairing reactor lining and a surface regulator atomization system. It includes the following steps:

[0155] Step W1: Abnormal state diagnosis. That is, through a dielectric spectrometer, obtain the moving state of the peak frequency of the loss tangent value, and based on the obtained peak frequency of the loss tangent value, obtain the corresponding dielectric loss change rate, specifically:

[0156]

[0157] Where: is the dielectric loss change rate, is the peak frequency of the current loss tangent value, is the peak frequency of the initial loss tangent value, is the detection time interval.

[0158] Furthermore, through laser backscattering, detect the change in particle size distribution and obtain the phase separation index, specifically:

[0159]

[0160] Where: is the phase separation index, is the current average particle size, is the initial average particle size.

[0161] Furthermore, through a multimode quartz fiber, obtain the axial temperature of the reactor and obtain the temperature change at the axial position, specifically:

[0162]

[0163] Where: is the temperature change, is the anti-Stokes light intensity, is the Stokes light intensity, is the calibration constant, is the temperature coefficient.

[0164] Specifically, according to the obtained dielectric loss change rate, phase separation index, and temperature change, compare them with the set change rate threshold, phase separation threshold, and temperature change threshold (not specifically set in this embodiment, and the threshold size can be specifically set according to specific data), and based on the comparison results, determine the abnormal state. Specifically:

[0165] When the obtained dielectric loss change is greater than the change rate threshold and the frequency peak of the loss tangent value decreases, the abnormal state at this time is filler agglomeration. When the obtained dielectric loss change rate is greater than the change rate threshold and the frequency peak of the loss tangent value increases, the abnormal state at this time is phase separation. Otherwise, there is no abnormal state.

[0166] When the obtained phase separation index is greater than the phase separation threshold, the abnormal state at this time is phase separation; otherwise, there is no abnormal state.

[0167] When the obtained temperature change amount is greater than the temperature change threshold, the abnormal state at this time is local overheating; otherwise, there is no abnormal state.

[0168] In the process of specific implementation, the peak frequency of the current loss tangent value is 980 kHz, the peak frequency of the initial loss tangent value is 1 MHz, and the detection time interval is 1 minute, then the corresponding dielectric loss change rate is 2% / min. Further, the current average particle size is 48 μm, the initial average particle size is 30 μm, then the corresponding phase separation index is 60%. Further, the ratio between the anti-Stokes light intensity and the Stokes light intensity is 1.12, the calibration constant is 1.02, and the temperature coefficient is 0.05, then the temperature change amount is 2°C.

[0169] Specifically, the change rate threshold in this embodiment is set to 0.05 / min, and the obtained dielectric loss change is less than the change rate threshold. At the same time, the phase separation threshold in this embodiment is set to 30%, and the obtained phase separation index is greater than the phase separation threshold, that is, the abnormal state at this time is phase separation. At the same time, the temperature change threshold in this embodiment is set to 5°C, and the obtained temperature change amount is less than the temperature change threshold.

[0170] Step W2: Collaborative processing. That is, according to the abnormal state determined in step W1, perform lining self-repair, anti-stratification pulse sequence, and curing inhibition collaboratively. That is, start the anti-stratification pulse sequence, curing inhibition, and lining self-repair intermittently in coordination. Specifically as follows:

[0171] Step W2.1: Implement the anti-stratification pulse sequence. That is, determine the agglomeration area in the reaction kettle through laser backscattering. At the same time, according to the determined agglomeration area, focus the ultrasonic wave on this agglomeration area and trigger intermittent adjustment through a hydrogen bubble sensor.

[0172] Step W2.2: Perform curing inhibition. That is, determine the high-temperature area in the reaction kettle through an optical fiber, and spray an ethanol solution into the high-temperature area in the reaction kettle through a two-fluid atomizing nozzle.

[0173] Step W2.3: Perform lining self-repair. That is, prepare microcapsules from polydimethylsiloxane, platinum catalyst, and urea formaldehyde resin, and disperse the prepared microcapsules in an epoxy resin-based coating. Further, perform high-pressure airless spraying, and the thickness after the dry film is set to 300 ± 20 μm.

[0174] Reference Figure 5 , Figure 5 is the comparison chart of the recovery rate of the solution in this embodiment. FromFigure 5 It can be seen that the recovery rate of the traditional solution is only 50%, making it difficult to accurately intervene in complex anomalies. However, through the collaborative treatment mechanism of ultrasonic focusing to break up aggregates, two-fluid atomization to spray ethanol solution for rapid cooling, and microcapsules to automatically repair the damage to the inner wall of the reaction kettle, the recovery rate of this solution reaches 95%. That is to say, compared with the traditional solution, the recovery rate is increased by 45%, significantly reducing the scrap rate.

[0175] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended embodiments and their equivalents.

Claims

1. A method for controlling the vacuum degree of a glue mixing and making reaction kettle, characterized in that: Included are: S1: Obtain rheological-dielectric-thermodynamic composite parameters of colloids: Obtain global viscosity distribution, axial / radial temperature gradient and filler phase separation critical point through shear wave-ultrasonic viscometer, distributed optical fiber temperature measurement network and broadband dielectric spectrometer, and monitor the rheological-dielectric-thermodynamic state of colloids in real time; S2: Determine the compensation vacuum degree: establish a colloid state coupling model according to the rheological-dielectric-thermodynamic state of the colloid, and determine the target vacuum degree; S3: Coordinated adjustment: According to the target vacuum degree and the current vacuum degree, the vacuum degree deviation is obtained, and according to the vacuum degree deviation, the axial temperature gradient of the reactor and the dielectric change rate, the magnetic suspension valve opening, the stirring speed and the regulator flow rate are coordinated and adjusted, including: S3.1: Normalization: According to the set vacuum deviation threshold, maximum temperature gradient threshold and dielectric change rate critical value, the vacuum deviation, temperature gradient and dielectric change rate are normalized, specifically: ； in: is the normalized vacuum deviation, is the vacuum degree deviation, is the vacuum deviation threshold, is the normalized temperature gradient, is the axial temperature gradient of the reactor, is the maximum temperature gradient threshold, is the normalized dielectric change rate, is the rate of change of the loss tangent, is the critical value of dielectric change rate; S3.2: Determine the adjustment amount: According to the normalized vacuum deviation, temperature gradient and dielectric change rate, determine the magnetic suspension valve opening adjustment amount, stirring speed adjustment amount and regulator flow adjustment amount, and adjust and control the valve current, inverter output frequency and peristaltic pump speed through the PLC controller; S3.3: Real-time regulation: vacuum regulation, mechanical stirring and chemical injection are coordinated according to the adjusted valve current, inverter output frequency and peristaltic pump speed.

2. A method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 1, characterized in that: Real-time monitoring of colloid rheological-dielectric-thermodynamic states, including: S1.1: Shear wave-ultrasonic viscometer measurement: Electromagnetic exciters are symmetrically installed on the side walls of the reactor, and ultrasonic probes are set on the top and bottom of the reactor. The storage modulus and dynamic viscosity are obtained through the electromagnetic exciter and ultrasonic probe, specifically: ； in: is the storage modulus, is the colloid density, is the shear wave velocity, is the dynamic viscosity, is the ultrasonic propagation time difference, is the material acoustic impedance constant, is the ultrasonic probe spacing; S1.2: Distributed optical fiber temperature measurement network monitoring: The optical fiber is spirally wound along the axial direction of the reactor to cover the height and radius of the reactor, and the optical fiber is connected to the input port of the OFRD demodulator through a splitter to obtain the axial / radial temperature gradient of the reactor, specifically: ； in: is the axial temperature gradient of the reactor, is the top temperature of the reactor, is the bottom temperature of the reactor, is the height of the reactor, is the radial temperature gradient of the reactor, is the temperature of the center area of ​​the reactor, is the wall temperature of the reactor, is the radius of the reactor; S1.3: Broadband dielectric spectrometer identification: Insert the electrode assembly vertically into the middle of the reactor, and obtain the dielectric constant and loss factor corresponding to different filler states through the electrode assembly to determine the loss tangent value, specifically: ； in: is the loss tangent value, is the dielectric constant, is the loss factor.

3. A method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 2, characterized in that: The electrode assembly is configured as a coaxial annular electrode structure, and the spacing between the inner electrode diameter and the outer electrode inner diameter is configured to be 2 mm, and a spacing is configured between the bottom end of the electrode assembly and the inner bottom end of the reactor.

4. The method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 1, characterized in that: Determine the target vacuum level, including: S2.1: Determine the comprehensive compensation vacuum degree: According to the rheological-dielectric-thermodynamic state of the colloid, establish a colloid state coupling model, specifically: ； in: is the compensation vacuum degree after comprehensive compensation, is the viscosity compensation coefficient, is the modulus compensation coefficient, is the dielectric loss compensation coefficient, is the dynamic viscosity, is the storage modulus, is the rate of change of the loss tangent, is the reference value of storage modulus, is the reference value of dynamic viscosity; S2.2: Perform temperature gradient correction: compare the axial temperature gradient of the reactor with the preset temperature gradient threshold, and perform temperature gradient correction based on the comparison result to obtain the compensation vacuum degree of the temperature gradient correction, specifically: ； in: is the compensation vacuum degree corrected for the temperature gradient, is the axial temperature gradient of the reactor; S2.3: Obtaining the target vacuum degree: Obtaining the final compensation vacuum degree according to the compensation vacuum degree after comprehensive compensation and the compensation vacuum degree corrected by the temperature gradient, and obtaining the target vacuum degree through the initial setting value of the vacuum degree, specifically: ； in: is the target vacuum degree, is the compensation vacuum degree after comprehensive compensation, is the compensation vacuum degree corrected for the temperature gradient, is the initial setting value of vacuum degree.

5. A method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 4, characterized in that: According to the comparison results, the temperature gradient correction is performed, specifically: When the axial temperature gradient of the reactor is greater than a preset temperature gradient threshold, the temperature gradient correction is performed; otherwise, the temperature gradient correction is not performed.

6. The method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 1, characterized in that: Adjust and control the valve current, inverter output frequency and peristaltic pump speed, including: S3.2.1: Determine valve current: Determine the opening adjustment amount according to the normalized vacuum deviation and the vacuum adjustment coefficient, and obtain the adjusted valve current according to the opening adjustment amount and the initial current value, specifically: ； in: To adjust the rear valve current, is the initial current value, is the opening adjustment amount, is the current-opening conversion coefficient; S3.2.2: Determine the inverter output frequency: Determine the stirring speed adjustment amount according to the normalized temperature gradient and the temperature gradient coefficient, and obtain the inverter output frequency according to the stirring speed adjustment amount and the current stirring speed, specifically: ； in: is the output frequency of the inverter, is the current stirring speed, is the stirring speed adjustment amount; S3.2.3: Determine the peristaltic pump speed: Determine the regulator flow adjustment amount according to the normalized dielectric change rate and the dielectric sensitivity coefficient, and obtain the peristaltic pump speed according to the regulator flow adjustment amount and the current regulator flow, specifically: ； in: is the peristaltic pump speed, is the current regulator flow rate, It is the regulator flow adjustment amount.

7. A method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 6, characterized in that: The formulas for obtaining the opening adjustment amount, the stirring speed adjustment amount and the regulator flow adjustment amount are as follows: ； in: is the opening adjustment amount, is the vacuum adjustment factor, is the normalized vacuum deviation, is the vacuum weight factor, is the stirring speed adjustment amount, is the temperature gradient coefficient, is the normalized temperature gradient, is the temperature weight factor, is the regulator flow adjustment amount, is the dielectric sensitivity coefficient, is the normalized dielectric change rate, is the dielectric weight factor.

8. The method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 1, characterized in that: During the coordinated adjustment in step S3, the phase separation state and the temperature gradient change state are monitored, and abnormal coordination processing is performed according to the abnormal state corresponding to the monitoring result, including: W1: Abnormal state diagnosis: The dielectric loss change rate, phase separation index and temperature change at the axial position are obtained through a dielectric spectrometer, laser backscattering and multimode quartz optical fiber. At the same time, the dielectric loss change rate, phase separation index and temperature change at the axial position are compared with the set change rate threshold, phase separation threshold and temperature change threshold, and the abnormal state is determined according to the comparison result, specifically: When the dielectric loss change rate is greater than the change rate threshold and the frequency peak of the loss tangent value decreases, the abnormal state is filler agglomeration; when the dielectric loss change rate is greater than the change rate threshold and the frequency peak of the loss tangent value increases, the abnormal state is phase separation; otherwise, there is no abnormal state; When the phase separation index is greater than the phase separation threshold, the abnormal state is phase separation, otherwise, there is no abnormal state; When the temperature change is greater than the temperature change threshold, the abnormal state is local overheating, otherwise, there is no abnormal state; W2: Cooperative processing: According to the abnormal state, the anti-delamination pulse sequence, curing inhibition and lining self-repair are initiated in an interval and coordinated manner.

9. A method for controlling the vacuum degree of a glue mixing and making reaction kettle according to claim 8, characterized in that: Interval synergistically initiates anti-delamination pulse sequences, cure inhibition and liner self-repair, including: W2.1: Implement anti-stratification pulse sequence: determine the agglomeration area in the reactor through laser backscattering and focus the ultrasound on the agglomeration area; W2.2: Perform solidification inhibition: spray ethanol solution to the high temperature area determined in the reactor through a two-fluid atomizing nozzle; W2.3: Perform lining self-repair: prepare microcapsules using polydimethylsiloxane, platinum catalyst and urea-formaldehyde resin, and disperse the microcapsules in an epoxy resin-based coating.

10. A vacuum control system for a glue mixing and making reaction kettle, characterized in that: A vacuum degree control method for a glue mixing and making reaction kettle as described in any one of claims 1 to 9 is used.

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