Intelligent control system for methyltris (methylethylketoximino) silane production equipment

Abstract

The invention discloses an intelligent control system for methyltris (methylethylketoximino) silane production equipment, which relates to the field of intelligent control of production equipment and comprises a data acquisition module, an analysis module and a control adjustment module. The method comprises the following steps: evaluating an edge three-dimensional structure shape, paddle material characteristics, paddle surface fluctuation characteristics and working motion characteristics in paddle shapes and motion forms to obtain a thermal increase state value, judging and analyzing agglomeration, crystallization, impurities and purity states of raw materials to obtain a raw material increase state value, judging and analyzing a compound reaction speed, and determining and analyzing a compound reaction speed. The method comprises the following steps of: obtaining a compound reaction speed comprehensive value, analyzing to obtain a production estimated temperature value, and performing temperature control on production equipment, so as to analyze components in a product by verifying an adjustment strategy after the temperature control on the production equipment is completed, and obtain different adjustment schemes; the temperature of production equipment can be intelligently controlled in a high-quality and multi-angle mode, and the purity of products can be guaranteed.

Description

Technical Field

[0001] The present invention relates to the field of intelligent control of production equipment, in particular to an intelligent control system for methyl tributylanoxime silane production equipment. Background Art

[0002] With the continuous development of the construction, automotive, and electronics industries, the demand for crosslinking agents and adhesives is increasing. The production of methyl tributylanoxime silane is even more critical, and controlling the temperature of methyl tributylanoxime silane production equipment is particularly important. Traditional control methods rely heavily on manual labor, which is subject to high subjectivity and low accuracy. Therefore, intelligent control systems for methyl tributylanoxime silane production equipment have emerged.

[0003] In the intelligent control process of methyltributylanoximesilane production equipment, it is difficult to perform high-quality and multi-angle intelligent temperature control of the production equipment, resulting in the frequent production of by-products and insufficient production of reactants, and the inability to guarantee product purity. Therefore, how to perform multi-angle intelligent temperature control of production equipment and improve product purity through temperature control are technical problems that need to be solved.

[0004] In order to solve the above-mentioned defects, a technical solution is now provided. Summary of the Invention

[0005] In order to solve the technical problems raised by the above background technology, the present invention is proposed. The embodiments of the present invention provide an intelligent control system for a methyl tributylanoxime silane production device.

[0006] The purpose of the present invention can be achieved through the following technical solution: an intelligent control system for methyl tributylanoxime silane production equipment, including a data acquisition module, an analysis module and a control and adjustment module.

[0007] The data acquisition module is used to collect blade information, raw material information, catalyst carrier information and production reaction information, and transmit it to the analysis module; The analysis module includes a paddle-shaped transport unit, a raw material analysis unit, and a reaction analysis unit; The blade shape and motion unit evaluates the blade's edge three-dimensional structure, blade material properties, blade surface undulation characteristics, and working motion characteristics to obtain thermal gain values. The raw material analysis unit determines and analyzes the agglomeration, crystallization, impurities and purity of the raw materials to obtain the raw material state value; Reaction analysis unit, which determines and analyzes the reaction rate of the compound and obtains the compound reaction rate summary value; The control and adjustment module includes a control unit and an adjustment unit.

[0008] Furthermore, the specific analysis steps of the thermal state value are as follows: The rotational acceleration, oscillation amplitude-frequency value, and eccentric velocity value of the blade during working motion are analyzed. After normalization, a cube is constructed by taking the rotational acceleration as the side length of the cube, and the center point of the cube's upper surface as the vertex of the cone. The sum of the rotational acceleration and the oscillation amplitude-frequency value is the height, and the eccentric velocity value is the diameter of the cone base to construct a cone. The volume of the irregular shape formed by the cube and cone is used as the standard for measuring the working motion state of the blade; The blade edge complexity value, blade material thermal conductivity value, blade surface undulation value and irregular body volume are calculated to obtain the blade thermal increase value jrz.

[0009] Furthermore, the specific analysis steps of the blade edge clutter value, blade material thermal conductivity value and blade surface undulation value are as follows: The three-dimensional structural shape of the blade edge is divided into several facets for analysis, and the solid angle of each facet in space is calculated. The solid angles of each facet of the blade are integrated and summed to obtain the edge clutter value of the blade; the blade material characteristics refer to the thermal conductivity of the blade material and the specific heat capacity of the material, and the sum is used to obtain the thermal conductivity value of the blade material; the blade surface undulation feature refers to when the light beam is focused on the blade surface through the optical lens, the spot diameter increment, spot ellipticity and light intensity contrast are obtained, and their weighted calculations are multiplied by the corresponding weight factor coefficients to obtain the blade surface undulation value. The spot ellipticity refers to the ratio of the major axis to the minor axis of the ellipse, and the light intensity contrast refers to the ratio of the maximum intensity to the minimum intensity.

[0010] Furthermore, the specific analysis steps of the raw material state-added value are as follows: The raw material agglomeration value, raw material crystallinity value, raw material impurity concentration value and raw material purity value are calculated to obtain the raw material state value yrz.

[0011] Furthermore, the specific analysis steps of the raw material agglomeration value, raw material crystallinity value, raw material impurity concentration value and raw material purity value are as follows: Obtaining the particle size of the methyl tributylidene monoxime silane raw material using a laser particle size analyzer, subtracting the minimum particle size of the raw material from the maximum particle size of the raw material to obtain a particle size distribution value of the raw material, placing a solution containing the raw material in an electric field environment, obtaining the distance and time interval of movement of the raw material agglomerates using an optical microscope, and dividing the two to obtain a migration speed ys of the raw material agglomerates, obtaining the viscosity value rn of the solution using a viscometer, calculating a surface potential value bd of the raw material agglomerates, multiplying the particle size distribution value and the surface potential value of the raw material agglomerates by correction factor coefficients h1 and h2, respectively, and summing the products to obtain an agglomeration value of the raw material; The X-ray diffraction pattern of the raw material is obtained by an X-ray diffractometer, and the background curve is fitted by a polynomial, and the background curve is subtracted from the original X-ray diffraction pattern to remove the instrument noise and the background signal of the sample scattering to obtain the diffraction peak. The peak shape is fitted by a combination of Gaussian function and Lorentz function, and the area of ​​each diffraction peak is calculated by integration, marked as the diffraction peak intensity, and the peak intensity of each diffraction peak is obtained. The area of ​​each diffraction peak is divided by the peak intensity of each diffraction peak to obtain the integral width of each diffraction peak. The peak intensity of each diffraction peak and the integral width of each diffraction peak are compared and analyzed with the set reference peak intensity and integral width. When each diffraction peak The peak intensity of the diffraction peak is less than or equal to the set reference peak intensity, and the integral width of each diffraction peak is greater than or equal to the set reference integral width, then the corresponding diffraction peak is a non-crystalline phase; when the peak intensity of each diffraction peak is greater than the set reference peak intensity, and the integral width of each diffraction peak is less than the set reference integral width, then the corresponding diffraction peak is a crystalline phase, the diffraction peak area of ​​the non-crystalline phase and the diffraction peak area of ​​the crystalline phase are counted, and the summation is performed to obtain the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase, and the diffraction peak intensity of the crystalline phase is divided by the sum of the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase to obtain the crystallinity value of the raw material; The methyl tributylan oxime silane raw material is prepared into a series of impurity standard solutions with different concentrations, and the absorbance of the impurity solutions with different concentrations is measured by a spectrometer. A standard absorbance versus concentration variation curve is established with the concentration of the impurity standard solution as the horizontal axis and the obtained absorbance as the vertical axis. The variation curve is fitted by the least squares method to obtain Equation 1. The absorbance of the raw material and the standard solution is measured under the same measurement conditions. The concentration value of the raw material impurity is obtained from Equation 1. The acidic impurity of the methyl tributylan oxime silane raw material is titrated with a standard alkali solution with a molar concentration of b1 and a volume of b2. The amount of the acidic impurity substance is obtained according to the reaction chemical formula. The mass sz of the acidic impurity is calculated by the formula. Specifically, the molar mass of the impurity is obtained through a database. The mass of the acidic impurity is subtracted from the mass of the measured total mass of the raw material to obtain the mass of the effective component. The mass of the effective component is divided by the total mass of the raw material to obtain the purity value of the raw material.

[0012] Furthermore, the specific analysis steps of the compound reaction rate value are as follows: Multiply the average reactant conversion rate by the weight factor coefficient p1 to obtain the product value one, multiply the dielectric constant by the weight factor coefficient p2 to obtain the product value two, multiply the catalyst carrier effective rate value xs by the weight factor coefficient p3 to obtain the product value three, multiply the product value one by the product value three and divide it by the product value two to obtain the overall reaction rate value hhz of the compound.

[0013] Furthermore, the specific analysis steps of the reactant conversion rate mean, dielectric constant and catalyst support effective rate value are as follows: The test liquid is dripped onto the surface of the raw catalyst carrier through a micro syringe. The contact angle meter identifies the outline of the droplet through the optical system and calculates the contact angle jθ of the carrier based on the shape of the droplet and the geometric equation of the ellipse. The specific surface area and pore size of the carrier are obtained and combined with the contact angle jθ of the carrier to calculate the catalyst carrier efficiency value xs. In the methyl tributylanoxime silane production reaction system, gas chromatography is used to measure the different retention times of different compounds in the chromatographic column, and compare them with the retention times of standards in the database to obtain the compound components corresponding to the chromatographic peaks. The types of compounds are determined, and the peak areas of the compounds are summed to obtain the peak area values ​​of the compounds, which are multiplied by the adjustment factor coefficient value to obtain the concentration values ​​of the compounds. The concentration values ​​of the compounds are sorted according to the reaction time, and the concentration values ​​of the compounds in the later order are subtracted from the concentration values ​​of the compounds in the earlier order to obtain the compound increase values, which are multiplied by the time interval between adjacent order values ​​to obtain the reactant conversion rate values. The reactant conversion rate values ​​at each time point are summed and divided by the number of time points to obtain the reactant conversion rate average. During the methyl tributylanoxime silane production reaction process, the dielectric constant of the reaction system is measured by a dielectric constant tester.

[0014] Furthermore, the control unit and the adjustment unit specifically analyze the steps as follows: The control unit is used to obtain the production temperature value based on the blade thermal state value, the raw material thermal state value and the compound reaction rate value sent by the analysis module, and to control the temperature of the production equipment according to the obtained production equipment temperature; The adjustment unit is used to analyze the components in the product by verifying the adjustment strategy after completing the temperature control of the production equipment, and obtain different adjustment plans.

[0015] Furthermore, the specific analysis steps for the temperature control and verification adjustment strategy of the production equipment are as follows: The blade thermal expansion value, the raw material expansion value, and the compound reaction rate are combined to calculate the production temperature estimate; the production temperature estimate is compared with the temperature ranges of several preset production equipment. Each temperature range of the production equipment is set to a corresponding production temperature estimate, and the corresponding production equipment temperature is obtained. The temperature of the production equipment is controlled according to the obtained production equipment temperature; After the temperature control of the production equipment is completed, the product is vaporized by gas chromatography and then enters the chromatographic column under the push of carrier gas. According to the distribution coefficient and retention time, it is analyzed to obtain the by-product content ratio and the unreacted content ratio; When the by-product content ratio in the product content is less than or equal to the set by-product content ratio threshold and the unreacted content ratio is less than or equal to the set unreacted content ratio threshold, the production equipment temperature is determined to be executed according to the control unit setting; When the by-product content ratio in the product content is greater than the set by-product content ratio threshold, the control temperature set by the control unit is lowered in a certain range until the by-product content ratio in the product content is less than the set by-product content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the production equipment temperature control; When the unreacted content ratio is greater than the set unreacted content ratio threshold, the control temperature set by the control unit is increased in sequence according to a certain amplitude until the unreacted content ratio is less than the set unreacted content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the production equipment temperature control.

[0016] Compared with the prior art, the present invention has the following beneficial effects: 1. The present invention evaluates the blade shape and the three-dimensional structural shape of the edge in the motion form, the blade material properties, the blade surface undulation characteristics and the working motion characteristics to obtain the thermal state value, and makes judgment and analysis on the agglomeration, crystallization, impurities and purity state of the raw materials to obtain the agglomeration value of the raw materials, the crystallinity value of the raw materials, the concentration value of the raw material impurities and the purity value of the raw materials, and then calculates and obtains the raw material state value, and makes judgment and analysis on the reaction rate of the compound to obtain the compound reaction rate comprehensive value. It can take into account the blade shape and running state, the characteristics of the raw materials, and the reaction state of the compound, so as to achieve multi-angle intelligent temperature control of the production equipment and improve the accuracy of the intelligent temperature control.

[0017] 2. The present invention is used to obtain the production temperature estimate value based on the blade thermal expansion value, raw material expansion value and compound reaction rate comprehensive value sent by the analysis module, and temperature control the production equipment according to the obtained production equipment temperature. After completing the temperature control of the production equipment, it is used to analyze the components in the product by verifying the adjustment strategy and obtain different adjustment schemes. It can monitor the generation of by-products and insufficient production of reactants, and make timely adjustments to ensure the purity of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. The following drawings are not intentionally scaled to the actual size, and the focus is on illustrating the main purpose of the present invention.

[0019] Figure 1 This is a system block diagram of the present invention. DETAILED DESCRIPTION

[0020] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts also fall within the scope of protection of the present invention.

[0021] like Figure 1 As shown, the intelligent control system for methyl tributylanoxime silane production equipment includes a data acquisition module, an analysis module and a control and adjustment module.

[0022] The data acquisition module collects blade information, raw material information, catalyst carrier information and production reaction information, and sends it to the analysis module.

[0023] The analysis module includes a paddle-shaped transport unit, a raw material analysis unit, and a reaction analysis unit; The blade shape and motion form of the blade are evaluated by the blade shape unit. The three-dimensional structure of the edge, the blade material properties, the blade surface undulation characteristics and the working motion characteristics are evaluated to obtain the thermal state value. The specific analysis steps are as follows: The thermal increase value of the blade shape and motion form is evaluated by the blade's edge three-dimensional structural shape, blade material properties, blade surface undulation characteristics and working motion characteristics. The blade's edge three-dimensional structural shape is divided into several patches, and the solid angle of each patch in space is calculated. The solid angles of each patch of the blade are integrated and summed to obtain the blade's edge clutter value; the blade material property refers to the thermal conductivity of the blade material and the specific heat capacity of the material, and the sum is used to obtain the blade material thermal conductivity value; the blade surface undulation feature refers to the spot diameter increment, spot ellipticity and light intensity contrast obtained when the light beam is focused on the blade surface through the optical lens, and their weighted calculation and multiplication by the corresponding weight factor coefficient are used to obtain the blade surface undulation feature. Volt value, where the spot ellipticity refers to the ratio of the major axis to the minor axis of the ellipse. The larger the ellipticity, the greater the surface undulation. The light intensity contrast refers to the ratio of the maximum light intensity to the minimum light intensity. The rotational acceleration, swing amplitude-frequency value and eccentric velocity value in the working motion of the blade are analyzed. After normalization, a cube is established by taking the rotational acceleration as the side length of the cube, and the position of the center point of the upper surface of the cube as the vertex of the cone. The sum of the rotational acceleration and the swing amplitude-frequency value is the height, and the eccentric velocity value is the diameter of the bottom circle of the cone to establish a cone. The volume of the irregular body formed by the cube and the cone is used as the standard for measuring the working motion state of the blade. The swing amplitude-frequency value is the sum of the swing amplitude and frequency of the blade, and the eccentric velocity value is the sum of the eccentricity and eccentric velocity of the blade. The obtained blade edge clutter value, blade material thermal conductivity value, blade surface undulation value and irregular body volume are marked as jb, jr, jq and yx, respectively, and normalized. The blade thermal increase value jrz is calculated according to the set formula jrz=(tox1×jb+tox3×jq+tox4×yx) / (tox2×jr), where tox1, tox2, tox3 and tox4 are the set weight factor coefficients of the blade edge clutter value, blade material thermal conductivity value, blade surface undulation value and irregular body volume, and their values ​​are 1.121, 1.926, 1.924 and 0.954, respectively.

[0024] The raw material analysis unit is used to determine and analyze the agglomeration, crystallization, impurities and purity of the raw materials to obtain the raw material state value. The specific analysis steps are as follows: Obtaining the particle size of the methyl tributylidene oxime silane raw material using a laser particle size analyzer, subtracting the minimum particle size of the raw material from the maximum particle size of the raw material to obtain the particle size distribution value of the raw material, placing a solution containing the raw material in an electric field environment, obtaining the distance and time interval of movement of the raw material agglomerates using an optical microscope, and dividing the two to obtain the migration speed ys of the raw material agglomerates, obtaining the viscosity value rn of the solution using a viscometer, and calculating the surface potential value bd of the raw material agglomerates according to the set formula bd=4×π×rn×ys / Φ, where Φ is the dielectric constant value of the solution, obtained using a capacitive dielectric constant meter, multiplying the particle size distribution value of the raw material and the surface potential value of the raw material agglomerates by correction factor coefficients h1 and h2, respectively, and summing the products to obtain the agglomeration value of the raw material; The X-ray diffraction pattern of the raw material is obtained by an X-ray diffractometer, and the background curve is fitted by a polynomial, and the background curve is subtracted from the original X-ray diffraction pattern to remove the instrument noise and the background signal of the sample scattering to obtain the diffraction peak. The peak shape is fitted by a combination of Gaussian function and Lorentz function, and the area of ​​each diffraction peak is calculated by integration, marked as the diffraction peak intensity, and the peak intensity of each diffraction peak is obtained. The area of ​​each diffraction peak is divided by the peak intensity of each diffraction peak to obtain the integral width of each diffraction peak. The peak intensity of each diffraction peak and the integral width of each diffraction peak are compared and analyzed with the set reference peak intensity and integral width. When each diffraction peak The peak intensity of the diffraction peak is less than or equal to the set reference peak intensity, and the integral width of each diffraction peak is greater than or equal to the set reference integral width, then the corresponding diffraction peak is a non-crystalline phase; when the peak intensity of each diffraction peak is greater than the set reference peak intensity, and the integral width of each diffraction peak is less than the set reference integral width, then the corresponding diffraction peak is a crystalline phase, the diffraction peak area of ​​the non-crystalline phase and the diffraction peak area of ​​the crystalline phase are counted, and the summation is performed to obtain the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase, and the diffraction peak intensity of the crystalline phase is divided by the sum of the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase to obtain the crystallinity value of the raw material; The methyl tributylanoxime silane raw material is made into a series of impurity standard solutions with concentrations of 0.1 mol / L, 0.2 mol / L, ..., n1 mol / L, and the absorbance of the impurity solutions of each concentration is measured by a spectrometer. The concentration of the impurity standard solution is used as the horizontal axis and the obtained absorbance is used as the vertical axis to establish a standard absorbance versus concentration curve. The curve is fitted by the least squares method to obtain the equation y=a1×x+a2, where x represents the concentration and y represents the absorbance. The absorbance of the raw material and the standard solution is measured under the same conditions. The concentration value of the raw material impurity is obtained from the above equation. The standard base is used to measure the impurity concentration. The acidic impurities of the methyl tributylanoxime silane raw material are titrated with a solution using a standard alkaline solution with a molar concentration of b1 and a volume of b2. The amount of the acidic impurity substance is obtained according to the reaction chemical formula: zw=d1×b1×b2 / d2, where d1 is the alkali stoichiometric coefficient of the alkaline solution and d2 is the stoichiometric coefficient of the acidic impurity. The mass sz of the acidic impurity is obtained according to the formula sz=zw×mz, where mz is the molar mass value of the acidic impurity. Specifically, the molar mass of the impurity is obtained from a database. The mass of the acidic impurity is subtracted from the total mass of the measured raw material to obtain the mass of the active ingredient. The mass of the active ingredient is divided by the total mass of the raw material to obtain the purity value of the raw material. The agglomeration value, crystallinity value, impurity concentration value and purity value of the raw material are marked as tj, jj, zn and cd respectively, and normalized and substituted into the set formula , the raw material enhancement value yrz is obtained, where f1, f2, f3, f4, f5, f6, f7, f8, f9, f10, f11, and f12 are all set weight factor coefficients used to promote the accuracy of calculation. f1 < f5 < f9, f2 < f6 < f10, f3 < f7 < f11, f12 < f8 < f4, and e is the natural constant with a value of 2.718. It should be noted that when the agglomeration phenomenon of the raw material is greater, the crystallinity is greater, the concentration of impurities is greater, the purity of the raw material is smaller, and the heat generated during the production process is less, the raw material enhancement value is smaller.

[0025] The reaction analysis unit is used to judge and analyze the reaction rate of the compound to obtain the compound reaction rate comprehensive state value. The specific analysis steps are as follows: A test liquid is dropped on the surface of the carrier of the raw material catalyst through a micro syringe. The contact angle measuring instrument identifies the contour of the liquid droplet through the optical system, and calculates the contact angle jθ of the carrier according to the shape of the liquid droplet, combined with the geometric equation of the ellipse, obtains the specific surface area and pore size of the carrier, and marks them as bm and kj, and normalizes them with the contact angle jθ of the carrier, according to the set formula The catalyst carrier efficiency rate value xs is obtained, where coc1, coc2, coc3, coc4, coc5, and coc6 are all set weight factor coefficients. coc1 > coc3, coc2 > coc4, coc6 > coc5, and A1 is the set reference carrier pore size. It should be noted that the methyltributanone oxime silane raw material is a hydrophobic reactant. When the contact angle of the carrier is larger, the effect of the catalyst is better; In the production reaction system of methyltributanone oxime silane, the different retention times of different compounds in the chromatographic column are measured by gas chromatography and compared with the retention times of the standards in the database to obtain the compound components corresponding to the chromatographic peaks. The retention time refers to the time value required from the start of injection to the appearance of the maximum value of the chromatographic peak. The types of compounds are determined, the peak areas of the compounds are summed to obtain the peak area value of the compounds, and multiplied by the adjustment factor coefficient value to obtain the concentration value of the compounds. The concentration values of the compounds are sorted according to the reaction time, the concentration value of the compound sorted later is subtracted from the concentration value of the compound sorted earlier to obtain the compound increase value, and multiplied by the time value between adjacent sorts to obtain the reactant conversion rate value. The reactant conversion rate values at each time point are summed and divided by the number of time points to obtain the average reactant conversion rate. During the production reaction process of methyltributanone oxime silane, the dielectric constant of the reaction system is measured by a dielectric constant tester; Multiply the average reactant conversion rate by the weight factor coefficient p1 to obtain the product value one, multiply the dielectric constant by the weight factor coefficient p2 to obtain the product value two, multiply the catalyst carrier effective rate value xs by the weight factor coefficient p3 to obtain the product value three, multiply the product value one by the product value three and divide it by the product value two to obtain the overall reaction rate value hhz of the compound.

[0026] The control and adjustment module includes a control unit and an adjustment unit; The control unit is used to obtain the production temperature value based on the blade thermal state value, raw material thermal state value and compound reaction rate value sent by the analysis module, and control the temperature of the production equipment according to the obtained production equipment temperature; The blade thermal state value jrz, raw material thermal state value yrz and compound reaction rate value hhz are normalized according to the set formula , calculate and obtain the estimated production temperature value GWZ, where h1, h2 and h3 are the preset weight coefficients of the blade thermal state value, the raw material thermal state value and the compound reaction rate value, and are set to 1.12, 1.11 and 1.95 respectively; The production estimated temperature value is compared with the temperature ranges of several preset production equipment. A production estimated temperature value is set corresponding to the temperature range of each production equipment. When the temperature range of the production equipment is determined, the corresponding production equipment temperature is obtained, and the temperature of the production equipment is controlled according to the obtained production equipment temperature.

[0027] After completing the temperature control of the production equipment, the adjustment unit analyzes the components in the product by verifying the adjustment strategy and obtains different adjustment solutions. The verification of the adjustment strategy includes the following steps: After the temperature control of the production equipment is completed, the product is vaporized by gas chromatography and then enters the chromatographic column under the promotion of carrier gas. According to the different distribution coefficients, the by-products, main products and reactants move at different speeds in the column and are separated. The separated components enter the detector and generate signals. The different retention times of the by-products, main products and reactants in the chromatographic column are measured by gas chromatography, and compared with the retention time of the standard products in the database and the standard retention time of the peak corresponding to the reactant raw materials, the by-products, main products and reactants are identified, and the peak areas of each are summed to obtain the content values ​​of the by-products, main products and reactants. The content values ​​of the by-products, main products and reactants are summed to obtain the total value, the by-product content is divided by the total value to obtain the by-product content ratio, and the reactant content is divided by the total value to obtain the unreacted content ratio; Compare and analyze the product content of each production equipment under temperature control with the set product content. When the by-product content ratio in the product content is less than or equal to the set by-product content ratio threshold and the unreacted content ratio is less than or equal to the set unreacted content ratio threshold, it is determined that the temperature of the production equipment is executed according to the setting of the control unit and is not adjusted; When the by-product content ratio in the product content is greater than the set by-product content ratio threshold, the control temperature set by the control unit is gradually reduced according to a certain amplitude, and the specific certain amplitude value can be 1 degree, until the by-product content ratio in the product content is less than the set by-product content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the production equipment temperature control; When the unreacted content ratio is greater than the set unreacted content ratio threshold, the control temperature set by the control unit is increased in sequence according to a certain amplitude. The specific certain amplitude value can be 1 degree, until the unreacted content ratio is less than the set unreacted content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the temperature control of the production equipment.

[0028] The above is an illustration of the present invention and should not be considered as limiting thereof. Although several exemplary embodiments of the present invention have been described, it will be readily understood by those skilled in the art that many modifications may be made to the exemplary embodiments without departing from the novel teachings and advantages of the present invention. Therefore, all such modifications are intended to be included within the scope of the present invention as defined by the claims. It should be understood that the above is an illustration of the present invention and should not be considered as being limited to the specific embodiments disclosed, and modifications to the disclosed embodiments and other embodiments are intended to be included within the scope of the appended claims. The present invention is defined by the claims and their equivalents.

Claims

1. An intelligent control system for methyl tributylidene oxime silane production equipment, characterized in that: include: The data acquisition module is used to collect blade information, raw material information, catalyst carrier information and production reaction information, and transmit it to the analysis module; The analysis module includes a blade shape and motion unit, a material analysis unit, and a reaction analysis unit. The blade shape and motion unit evaluates the blade's edge 3D structure, blade material properties, blade surface undulations, and operating motion characteristics to obtain a thermal gain value. The raw material analysis unit determines and analyzes the agglomeration, crystallization, impurities and purity of the raw materials to obtain the raw material state value; the reaction analysis unit determines and analyzes the reaction rate of the compound to obtain the compound reaction rate value; The control and adjustment module includes a control unit and an adjustment unit. The control unit is used to obtain the production temperature estimate value based on the blade thermal expansion value, raw material expansion value and compound reaction rate comprehensive value sent by the analysis module, and to control the temperature of the production equipment based on the obtained production equipment temperature; the adjustment unit is used to analyze the components in the product by verifying the adjustment strategy after completing the temperature control of the production equipment, and obtain different adjustment plans.

2. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 1, characterized in that: The specific analysis steps of the thermal growth value are as follows: The rotational acceleration, swing amplitude-frequency value, and eccentric velocity value of the blade working motion are analyzed and then normalized. A cube is constructed by taking the rotational acceleration as the side length of the cube, and the center point of the cube's upper surface as the vertex of the cone. The sum of the rotational acceleration and the swing amplitude-frequency value is the height, and the eccentric velocity value is the diameter of the cone base to construct a cone. The volume of the irregular shape formed by the cube and cone is used as the standard for measuring the working motion state of the blade; The blade edge roughness value, blade material thermal conductivity value, blade surface undulation value and irregular body volume are calculated to obtain the blade thermal increase value.

3. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 2, characterized in that: The specific analysis steps for the blade edge clutter value, blade material thermal conductivity value, and blade surface undulation value are as follows: The three-dimensional structural shape of the blade edge is divided into several facets, and the solid angle of each facet in space is calculated. The solid angles of each facet of the blade are integrated and summed to obtain the edge clutter value of the blade; the blade material characteristics refer to the thermal conductivity of the blade material and the specific heat capacity of the material, and the sum is used to obtain the thermal conductivity value of the blade material; the blade surface undulation feature refers to when the light beam is focused on the blade surface through the optical lens, the spot diameter increment, spot ellipticity and light intensity contrast are obtained, and their weighted calculation and multiplication by the corresponding weight factor coefficient are used to obtain the blade surface undulation value. The spot ellipticity refers to the ratio of the major axis to the minor axis of the ellipse, and the light intensity contrast refers to the ratio of the maximum intensity to the minimum intensity.

4. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 1, characterized in that: The specific analysis steps of the raw material state-added value are as follows: The raw material agglomeration value, raw material crystallinity value, raw material impurity concentration value and raw material purity value are calculated to obtain the raw material state value.

5. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 4, characterized in that: The specific analysis steps of the raw material agglomeration value, raw material crystallinity value, raw material impurity concentration value and raw material purity value are as follows: Obtaining a particle size value of a methyl tributylidene monoxime silane raw material using a laser particle size analyzer, subtracting a minimum particle size of the raw material from a maximum particle size of the raw material to obtain a particle size distribution value of the raw material, placing a solution containing the raw material in an electric field environment, obtaining a distance and a time interval of movement of raw material agglomerates using an optical microscope, and dividing the two to obtain a migration velocity of the raw material agglomerates, obtaining a viscosity value of the solution using a viscometer, calculating a surface potential value of the raw material agglomerates, multiplying the particle size distribution value of the raw material and the surface potential value of the raw material agglomerates by corresponding correction factor coefficients, and summing the products to obtain an agglomeration value of the raw material; The X-ray diffraction pattern of the raw material is obtained by an X-ray diffractometer, and the background curve is fitted by a polynomial, and the background curve is subtracted from the original X-ray diffraction pattern to remove the instrument noise and the background signal of the sample scattering to obtain the diffraction peak. The peak shape is fitted by a combination of Gaussian function and Lorentz function, and the area of ​​each diffraction peak is calculated by integration, marked as the diffraction peak intensity, and the peak intensity of each diffraction peak is obtained. The area of ​​each diffraction peak is divided by the peak intensity of each diffraction peak to obtain the integral width of each diffraction peak. The peak intensity of each diffraction peak and the integral width of each diffraction peak are compared and analyzed with the set reference peak intensity and integral width. When each diffraction peak The peak intensity of the diffraction peak is less than or equal to the set reference peak intensity, and the integral width of each diffraction peak is greater than or equal to the set reference integral width, then the corresponding diffraction peak is a non-crystalline phase; when the peak intensity of each diffraction peak is greater than the set reference peak intensity, and the integral width of each diffraction peak is less than the set reference integral width, then the corresponding diffraction peak is a crystalline phase, the diffraction peak area of ​​the non-crystalline phase and the diffraction peak area of ​​the crystalline phase are counted, and the summation is performed to obtain the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase, and the diffraction peak intensity of the crystalline phase is divided by the sum of the diffraction peak intensity of the non-crystalline phase and the diffraction peak intensity of the crystalline phase to obtain the crystallinity value of the raw material; The methyl tributylan oxime silane raw material is prepared into a series of impurity standard solutions with different concentrations, and the absorbance of the impurity solutions with different concentrations is measured by a spectrometer. A standard absorbance versus concentration variation curve is established with the concentration of the impurity standard solution as the horizontal axis and the obtained absorbance as the vertical axis. The variation curve is fitted by the least squares method to obtain Equation 1. The absorbance of the raw material and the standard solution is measured under the same measurement conditions. The concentration value of the raw material impurity is obtained from Equation 1. The acidic impurity of the methyl tributylan oxime silane raw material is titrated with a standard alkali solution with a molar concentration of b1 and a volume of b2. The amount of the acidic impurity substance is obtained according to the reaction chemical formula. The mass sz of the acidic impurity is calculated by the formula. Specifically, the molar mass of the impurity is obtained through a database. The mass of the acidic impurity is subtracted from the mass of the measured total mass of the raw material to obtain the mass of the effective component. The mass of the effective component is divided by the total mass of the raw material to obtain the purity value of the raw material.

6. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 1, characterized in that: The specific analysis steps of the compound reaction rate value are as follows: Multiply the average reactant conversion rate by the weight factor coefficient p1 to obtain the product value one, multiply the dielectric constant by the weight factor coefficient p2 to obtain the product value two, multiply the catalyst carrier effective rate value xs by the weight factor coefficient p3 to obtain the product value three, multiply the product value one by the product value three and divide it by the product value two to obtain the overall reaction rate value hhz of the compound.

7. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 6, characterized in that: The specific analysis steps of the reactant conversion rate mean, dielectric constant and catalyst support effective rate value are as follows: The test liquid is dripped onto the surface of the raw catalyst carrier through a micro syringe. The contact angle meter identifies the outline of the droplet through the optical system and calculates the contact angle jθ of the carrier based on the shape of the droplet and the geometric equation of the ellipse. The specific surface area and pore size of the carrier are obtained and combined with the contact angle jθ of the carrier to calculate the catalyst carrier efficiency value xs by the formula; In the methyl tributylanoxime silane production reaction system, gas chromatography is used to measure the different retention times of different compounds in the chromatographic column, and compare them with the retention times of standards in the database to obtain the compound components corresponding to the chromatographic peaks. The types of compounds are determined, and the peak areas of the compounds are summed to obtain the peak area values ​​of the compounds, which are multiplied by the adjustment factor coefficient value to obtain the concentration values ​​of the compounds. The concentration values ​​of the compounds are sorted according to the reaction time, and the concentration values ​​of the compounds in the later order are subtracted from the concentration values ​​of the compounds in the earlier order to obtain the compound increase values, which are multiplied by the time interval between adjacent order values ​​to obtain the reactant conversion rate values. The reactant conversion rate values ​​at each time point are summed and divided by the number of time points to obtain the reactant conversion rate average. During the methyl tributylanoxime silane production reaction process, the dielectric constant of the reaction system is measured by a dielectric constant tester.

8. The intelligent control system for methyl tributylidene oxime silane production equipment according to claim 1, characterized in that: The specific analysis steps for temperature control and verification adjustment strategy of the production equipment are as follows: The blade thermal expansion value, the raw material expansion value, and the compound reaction rate are combined to calculate the production temperature estimate; the production temperature estimate is compared with the temperature ranges of several preset production equipment. Each temperature range of the production equipment is set to a corresponding production temperature estimate, and the corresponding production equipment temperature is obtained. The temperature of the production equipment is controlled according to the obtained production equipment temperature; After the temperature control of the production equipment is completed, the product is vaporized by gas chromatography and then enters the chromatographic column under the push of carrier gas. According to the distribution coefficient and retention time, it is analyzed to obtain the by-product content ratio and the unreacted content ratio; When the by-product content ratio in the product content is less than or equal to the set by-product content ratio threshold and the unreacted content ratio is less than or equal to the set unreacted content ratio threshold, the production equipment temperature is determined to be executed according to the control unit setting; When the by-product content ratio in the product content is greater than the set by-product content ratio threshold, the control temperature set by the control unit is lowered in a certain range until the by-product content ratio in the product content is less than the set by-product content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the production equipment temperature control; When the unreacted content ratio is greater than the set unreacted content ratio threshold, the control temperature set by the control unit is increased in sequence according to a certain amplitude until the unreacted content ratio is less than the set unreacted content ratio threshold, and the adjusted temperature at this time is used as the final temperature value of the production equipment temperature control.

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