Synthesis method of boiling-resistant acrylic acid modified polyester dispersion resin
By removing low molecular weight impurities, dehydration treatment of acrylic monomer, temperature adaptive algorithm control and modification reaction, the synthesis of boiled acrylic modified polyester dispersion resin is optimized, and the problem of unstable quality in traditional methods is solved, and higher boiled resistance and dispersion are achieved.
Patent Information
- Application Number
- CN202510573059.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-08-08
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The traditional boil-resistant acrylic modified polyester dispersion resin synthesis method lacks precise control and optimization, resulting in uneven product quality and lack of effective evaluation of dispersion stability, making it difficult to meet the application needs of high-temperature treatment or long-term contact with water.
By removing low molecular weight impurities in the polyester polyol, dehydration of acrylic monomers is carried out, the esterification reaction is controlled using a temperature adaptive algorithm, combined with silane coupling agent and epoxy resin modification, and finally, the boiling resistance of the resin is optimized through dispersant and grinding treatment.
The purity and stability of the resin are improved, the esterification reaction efficiency is enhanced, the reaction rate and conversion rate are optimized, and the resin is better boiling resistance, adhesion and chemical resistance are given, and a grinding dispersion resin with high dispersion and uniformity is obtained.
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Figure CN120452631A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a method for synthesizing boiling-resistant acrylic acid-modified polyester dispersion resin, and belongs to the field of material science and engineering. Background Art
[0002] The synthesis of boil-resistant acrylic-modified polyester dispersion resins involves copolymerizing acrylic monomers with polyester polyols through a series of chemical reactions to produce resin dispersions with specific properties, particularly boil-resistant properties. Boil-resistant acrylic-modified polyester dispersion resins are characterized by their excellent boil-resistant properties, making them widely applicable in coatings, inks, and other fields, particularly in applications requiring high-temperature processing or prolonged water contact.
[0003] The traditional synthesis method of water-boiling-resistant acrylic modified polyester dispersion resin usually adopts a simple copolymerization reaction under high temperature and high pressure conditions. It does not pay attention to the pretreatment of raw materials and the precise control of reaction conditions. It often uses a large amount of organic solvents. The lack of intelligent control leads to uneven product quality and a lack of effective evaluation and optimization of the dispersion stability of the final product. Summary of the Invention
[0004] The invention provides a method for synthesizing a boiling-resistant acrylic acid-modified polyester dispersion resin, the main purpose of which is to improve the boiling-resistant performance of the synthetic resin.
[0005] To achieve the above object, the present invention provides a method for synthesizing a boiling-resistant acrylic modified polyester dispersion resin, comprising: analyzing low molecular weight impurities in the polyester polyol, removing the low molecular weight impurities in the polyester polyol to obtain the target polyester polyol, and dehydrating the acrylic acid monomer to obtain a dehydrated acrylic acid monomer; In a preset reactor, an esterification reaction environment is established for the target polyester polyol and the dehydrated acrylic acid monomer, a temperature adjustment parameter of the esterification reaction environment is determined using a preset temperature adaptive algorithm, an esterification reaction is performed in the esterification reaction environment according to the temperature adjustment parameter, an esterification reactant is obtained, and an esterification coefficient of the esterification reactant is analyzed; When the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are subjected to a polymerization reaction to obtain a polymerization reactant, the polymerization degree of the polymerization reactant is calculated, and the polymerization reactant is cooled according to the polymerization degree to obtain a cooled polymerization reactant; Performing a modification reaction on the cooling polymerization reactant using a preset silane coupling agent and an epoxy resin to obtain a modified resin, obtaining a modification spectrum of the modified resin, and analyzing a modification effect of the modified resin based on the modification spectrum; Based on the modification effect, the modified resin and a preset dispersant are mixed to obtain a mixed dispersion resin, the mixed dispersion resin is ground to obtain a ground dispersion resin, and the boiling resistance coefficient of the ground dispersion resin is calculated. When the boiling resistance coefficient meets the preset boiling resistance threshold, the ground dispersion resin is used as the target dispersion resin.
[0006] Optionally, the analysis of low molecular weight impurities in polyester polyols comprises: dissolving the polyester polyol to obtain dissolved polyester polyol; filtering the dissolved polyester polyol to obtain filtered dissolved polyester polyol; centrifuging the filtered dissolved polyester polyol to obtain centrifugally dissolved polyester polyol; performing chromatographic separation on the centrifugally dissolved polyester polyol to obtain separated dissolved polyester polyol; analyzing the molecular structure and compound composition of the separated and dissolved polyester polyol; The low molecular weight impurities of the polyester polyol are determined based on the molecular structure and the compound components.
[0007] Optionally, constructing an esterification reaction environment for the target polyester polyol and the dehydrated acrylic acid monomer in a preset reactor includes: Establishing high temperature vacuum conditions of the reactor; Analyzing the sealing coefficient of the reactor under the high temperature vacuum condition; When the sealing coefficient meets a preset sealing threshold, preparing the target polyester polyol and the catalyst and green solvent of the dehydrated acrylic acid monomer; analyzing the reactor characteristics of the reactor; Based on the characteristics of the reactor, construct an esterification reaction device for the reactor; An esterification reaction environment of the target polyester polyol and the dehydrated acrylic acid monomer is constructed by the high-temperature vacuum condition, the catalyst, the green solvent and the esterification reaction equipment.
[0008] Optionally, the determining the temperature adjustment parameters of the esterification reaction environment by using a preset temperature adaptive algorithm includes: Initializing algorithm parameters of the temperature adaptive algorithm, wherein the algorithm parameters include a proportional coefficient, an integral coefficient, and a differential coefficient; defining a target temperature of the esterification reaction environment; collecting the current temperature of the esterification reaction environment; Based on the target temperature, the current temperature, and the algorithm parameters, the temperature adjustment parameters of the esterification reaction environment are determined using the temperature adaptive algorithm, wherein the temperature adaptive algorithm: in, Indicates the temperature adjustment parameter of the esterification reaction environment, Indicates the proportional coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature and the target temperature. represents the integral term, Represents the differential coefficient corresponding to the algorithm parameters, Indicates the integral coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature of the node and the target temperature in the previous acquisition. Indicates the sampling time interval.
[0009] Optionally, analyzing the esterification coefficient of the esterification reactant includes: defining the initial molar number of the esterification reactants; extracting the target ester from the esterification reaction product; Analyzing the purity coefficient of the target ester; Calculating the current molar number of the target ester according to the purity coefficient; An esterification coefficient of the esterification reactant is determined based on the initial mole number and the current mole number.
[0010] Optionally, when the esterification coefficient meets a preset esterification standard, the esterification reactant and a preset free radical initiator are subjected to a polymerization reaction to obtain a polymer reactant, comprising: When the esterification coefficient meets the preset esterification standard, dissolving the target ester corresponding to the esterification reactant into a preset toluene solution to obtain a target ester solution; defining an adaptive algorithm for initiator concentration of the target ester solution; integrating the free radical initiator into the target ester solution according to the initiator concentration adaptive algorithm to obtain a target polymerization solution; constructing a temperature controller and a degassing device for the target polymer solution; Based on the temperature controller and the degassing device, a polymerization reaction of the target polymerization solution is performed to obtain a polymerization reactant.
[0011] Optionally, the calculating the degree of polymerization of the polymer reactant comprises: labeling unit monomers of the polymer reactant; determining the monomer molecular weight of the unit monomer; labeling the polymer of the polymeric reaction; analyzing the polymer for polymer molecular weight and polymer mole fraction; Based on the monomer molecular weight, the polymer molecular weight and the polymer mole fraction, the degree of polymerization of the polymer reactant is calculated using the following formula: in, represents the degree of polymerization of the polymer reactant, Indicates the The polymer molecular weight of each polymer, Indicates the The polymer mole fraction of each polymer, Indicates monomer molecular weight.
[0012] Optionally, the step of modifying the cooling polymerization reactant with a preset silane coupling agent and epoxy resin to obtain a modified resin comprises: dissolving the epoxy resin to obtain dissolved epoxy resin; pretreating the silane coupling agent to obtain a pretreated silane coupling agent; Under stirring conditions, integrating the pretreated silane coupling agent and the dissolved epoxy resin into the cooling polymerization reactant to obtain a stirred polymerization reactant; Analyzing the uniformity coefficient of the stirred polymerization reaction product; The stirred polymerization reactant is solidified according to the uniformity coefficient to obtain the modified resin.
[0013] Optionally, analyzing the modification effect of the modified resin according to the modification spectrum includes: Performing baseline correction on the modified spectrum to obtain a corrected modified spectrum; De-noising the corrected modified spectrum to obtain a de-noised modified spectrum; Identifying characteristic absorption peaks of the denoised and modified spectrum; Marking a characteristic peak change of the characteristic absorption peak, wherein the characteristic peak change includes a peak intensity change and a peak position change; Based on the changes in the characteristic peaks, the modification effect of the modified resin is analyzed.
[0014] Optionally, the calculating the boiling resistance coefficient of the grinding dispersion resin includes: extracting a resin sample of the ground dispersion resin; integrating the resin sample into a predetermined substrate to obtain a coating substrate; Identifying the glossiness of the coating substrate before boiling; boiling the coating substrate in water to obtain a boiled coating substrate; Identifying the glossiness of the water-boiled coating substrate after water boiling; Based on the glossiness of the substrate before boiling and the glossiness of the substrate after boiling, the boiling resistance coefficient of the grinding dispersion resin is calculated using the following formula: in, Indicates the boiling resistance coefficient of the grinding dispersion resin, Indicates the glossiness of the substrate after boiling in water. Indicates the glossiness of the substrate before boiling.
[0015] In order to solve the above problem, the present invention further provides an electronic device, comprising: at least one processor; and, a memory communicatively connected to the at least one processor; wherein, The memory stores instructions that can be executed by the at least one processor, and the instructions are executed by the at least one processor to implement the above-mentioned method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin.
[0016] In order to solve the above problems, the present invention also provides a computer-readable storage medium, which stores at least one instruction. The at least one instruction is executed by a processor in an electronic device to implement the above-mentioned method for synthesizing the water-boiling-resistant acrylic modified polyester dispersion resin.
[0017] Compared to the problems described in the background art, first, by removing low-molecular-weight impurities in the polyester polyol, the purity and performance of the final resin are improved, ensuring its stability and reliability in application. Secondly, the dehydration treatment of the acrylic monomer enhances the efficiency of the esterification reaction, so that the synthesized resin has more excellent chemical and physical properties. The temperature adaptive algorithm is used to precisely control the esterification reaction environment, which not only optimizes the reaction rate and conversion rate, but also reduces the generation of by-products, improving the quality of the product. The analysis of the esterification coefficient ensures that the reaction reaches the preset esterification standard, laying the foundation for the smooth progress of the subsequent polymerization reaction. The calculation of the degree of polymerization of the polymer reactant and the cooling treatment further improve the molecular weight and performance of the resin, making it more valuable for application. The modification reaction of the silane coupling agent and the epoxy resin gives the resin better water boiling resistance, adhesion and chemical resistance. Finally, by mixing the dispersant and grinding, a ground dispersion resin with high dispersibility and uniformity is obtained. Therefore, the present invention can improve the water boiling resistance of the synthetic resin. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 A schematic flow chart of a method for synthesizing a boiling-resistant acrylic modified polyester dispersion resin provided in one embodiment of the present invention; The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION
[0019] It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.
[0020] The present embodiment provides a method for synthesizing a boil-resistant acrylic-modified polyester dispersion resin. The method can be executed by at least one electronic device, such as a server or terminal, that can be configured to execute the method provided in the present embodiment. In other words, the method can be executed by software or hardware installed on a terminal or server. The server includes, but is not limited to, a single server, a server cluster, a cloud server, or a cloud server cluster.
[0021] Example 1: Reference Figure 1 FIG. 1 is a flow chart of a method for synthesizing a boiling-resistant acrylic modified polyester dispersion resin according to an embodiment of the present invention. In this embodiment, the method for synthesizing a boiling-resistant acrylic modified polyester dispersion resin comprises: S1. Analyze low molecular weight impurities in the polyester polyol, remove the low molecular weight impurities in the polyester polyol to obtain target polyester polyol, and dehydrate the acrylic acid monomer to obtain a dehydrated acrylic acid monomer.
[0022] The present invention analyzes the low molecular weight impurities in the polyester polyol and can analyze the low molecular weight impurities in the polyester polyol in detail, providing a basis for improving the production process and enhancing the product quality.
[0023] In detail, the analysis of low molecular weight impurities in polyester polyols includes: dissolving the polyester polyol to obtain dissolved polyester polyol; filtering the dissolved polyester polyol to obtain filtered dissolved polyester polyol; centrifuging the filtered dissolved polyester polyol to obtain centrifugally dissolved polyester polyol; performing chromatographic separation on the centrifugally dissolved polyester polyol to obtain separated dissolved polyester polyol; analyzing the molecular structure and compound composition of the separated and dissolved polyester polyol; The low molecular weight impurities of the polyester polyol are determined based on the molecular structure and the compound components.
[0024] Among them, the dissolved polyester polyol refers to a solution obtained by completely dissolving the polyester polyol in a specific solvent (such as dimethyl sulfoxide, tetrahydrofuran, etc.), the filtered dissolved polyester polyol refers to a solution obtained by removing insoluble large particle impurities in the dissolved polyester polyol through a filtration operation, the centrifuged dissolved polyester polyol refers to a purer polyester polyol solution obtained after a centrifugal operation, the separated dissolved polyester polyol refers to a polyester polyol solution separated according to molecular weight obtained by a chromatographic separation technique (such as gel permeation chromatography GPC), the molecular structure refers to the chemical structure and molecular skeleton of the polyester polyol and its impurities determined by an analytical technique (such as nuclear magnetic resonance NMR, mass spectrometry MS, etc.), the compound component refers to the type and content of the specific compound present in the separated dissolved polyester polyol determined by an analytical technique, and the low molecular weight impurity refers to an impurity component with a lower molecular weight in the polyester polyol.
[0025] Optionally, the chromatographic separation of the centrifugally dissolved polyester polyol to obtain the separated dissolved polyester polyol can be achieved by gel permeation chromatography.
[0026] The present invention dehydrates acrylic acid monomers to obtain dehydrated acrylic acid monomers, which are suitable for subsequent polymerization reactions. The acrylic acid monomer refers to an organic compound containing a carbon-carbon double bond and a carboxyl functional group, and the dehydrated acrylic acid monomer refers to acrylic acid monomers that have undergone dehydration. Specifically, the dehydration of the acrylic acid monomer can be achieved using a desiccant (such as anhydrous sodium sulfate, anhydrous magnesium sulfate, or a molecular sieve).
[0027] S2. In a preset reactor, construct an esterification reaction environment for the target polyester polyol and the dehydrated acrylic acid monomer, determine temperature adjustment parameters of the esterification reaction environment using a preset temperature adaptive algorithm, perform an esterification reaction in the esterification reaction environment according to the temperature adjustment parameters, obtain an esterification reactant, and analyze the esterification coefficient of the esterification reactant.
[0028] The present invention constructs an esterification reaction environment for the target polyester polyol and the dehydrated acrylic acid monomer in a preset reactor, thereby constructing an environment suitable for the esterification reaction of the polyester polyol and the dehydrated acrylic acid monomer in the reactor, and ultimately obtaining the target polyester polyol product.
[0029] In detail, the esterification reaction environment of the target polyester polyol and the dehydrated acrylic acid monomer is constructed in a preset reactor, including: Establishing high temperature vacuum conditions of the reactor; Analyzing the sealing coefficient of the reactor under the high temperature vacuum condition; When the sealing coefficient meets a preset sealing threshold, preparing the target polyester polyol and the catalyst and green solvent of the dehydrated acrylic acid monomer; analyzing the reactor characteristics of the reactor; Based on the characteristics of the reactor, construct an esterification reaction device for the reactor; An esterification reaction environment of the target polyester polyol and the dehydrated acrylic acid monomer is constructed by the high-temperature vacuum condition, the catalyst, the green solvent and the esterification reaction equipment.
[0030] The high-temperature vacuum condition refers to raising the temperature in the reactor to the level required for the reaction through a heating system. The sealing coefficient refers to an indicator for measuring the sealing performance of the reactor. The sealing threshold refers to a pre-set standard for the sealing coefficient. The catalyst refers to a substance that can change the chemical reaction rate of the target polyester polyol and the dehydrated acrylic monomer without being consumed itself, such as tetrabutyl titanate. The green solvent refers to an environmentally friendly, low-toxic, and recyclable solvent, such as a water-soluble solution. The reactor characteristics include its material, size, design, heating and cooling capacity, maximum pressure and temperature, etc. The esterification reaction equipment refers to all hardware facilities used for the esterification reaction, including the heating system, cooling system, vacuum system, stirring system, etc. The esterification reaction environment refers to the overall environment suitable for the esterification reaction created by the above-mentioned equipment and conditions, including temperature, pressure, reactant concentration, the presence of catalyst, etc.
[0031] The present invention utilizes a preset temperature adaptive algorithm to determine the temperature adjustment parameters of the esterification reaction environment, and can dynamically adjust the temperature of the esterification reaction environment, ensuring that the reaction can proceed under optimal conditions, thereby improving the quality and yield of the product.
[0032] In detail, the method of determining the temperature adjustment parameters of the esterification reaction environment by using a preset temperature adaptive algorithm includes: Initializing algorithm parameters of the temperature adaptive algorithm, wherein the algorithm parameters include a proportional coefficient, an integral coefficient, and a differential coefficient; defining a target temperature of the esterification reaction environment; collecting the current temperature of the esterification reaction environment; Based on the target temperature, the current temperature, and the algorithm parameters, the temperature adjustment parameters of the esterification reaction environment are determined using the temperature adaptive algorithm, wherein the temperature adaptive algorithm: in, Indicates the temperature adjustment parameter of the esterification reaction environment, Indicates the proportional coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature and the target temperature. represents the integral term, Represents the differential coefficient corresponding to the algorithm parameters, Indicates the integral coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature of the node and the target temperature in the previous acquisition. Indicates the sampling time interval.
[0033] Among them, the proportional coefficient refers to a parameter used to adjust the impact of the current temperature deviation on the temperature control output, the integral coefficient refers to a parameter used to eliminate long-term temperature deviations, the differential coefficient refers to a parameter used to predict temperature change trends and reduce overshoot, the target temperature refers to the predetermined temperature that the reactor needs to reach, the current temperature refers to the temperature inside the reactor measured in real time by the temperature sensor, the temperature control parameter refers to the output of the temperature adaptive algorithm, which is used to adjust the heating or cooling device to achieve the target temperature, the integral term refers to the integral of the current temperature deviation over time, the temperature deviation refers to the difference between the target temperature and the current temperature, and the sampling time interval refers to the time interval between two temperature samples.
[0034] The present invention can effectively perform the esterification reaction in the esterification reaction environment according to the temperature adjustment parameters to obtain the esterification reactant, and obtain the desired esterification reactant. The esterification reactant refers to the ester and water generated by the reaction of the target polyester polyol and the dehydrated acrylic acid monomer in the esterification reaction environment.
[0035] The present invention analyzes the esterification coefficient of the esterification reactant to analyze the reaction effect of the esterification reaction and provide a basis for the subsequent polymerization reaction.
[0036] In detail, the analysis of the esterification coefficient of the esterification reactant includes: defining the initial molar number of the esterification reactants; extracting the target ester from the esterification reaction product; Analyzing the purity coefficient of the target ester; Calculating the current molar number of the target ester according to the purity coefficient; An esterification coefficient of the esterification reactant is determined based on the initial mole number and the current mole number.
[0037] Wherein, the initial molar number refers to the molar number of the target polyester polyol and the dehydrated acrylic acid monomer participating in the reaction before the esterification reaction, the target ester refers to the ester compound expected to be produced in the esterification reaction, the purity coefficient refers to the purity of the target ester extracted from the reaction mixture, the current molar number refers to the actual molar number of the target ester determined by experimental analysis, and the esterification coefficient refers to the ratio of the current molar number of the target ester to the initial molar number.
[0038] Optionally, the purity coefficient of the target ester can be determined by measuring the ratio of the actual purity of the target ester to the theoretical purity (100%) using analytical means (such as chromatography, mass spectrometry, spectroscopy, etc.).
[0039] S3. When the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are polymerized to obtain a polymer reactant, the polymerization degree of the polymer reactant is calculated, and the polymer reactant is cooled according to the polymerization degree to obtain a cooled polymer reactant.
[0040] In the present invention, when the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are polymerized to obtain a polymerized reactant which can be used as the basis of a resin.
[0041] In detail, when the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are polymerized to obtain a polymer reactant, comprising: When the esterification coefficient meets the preset esterification standard, dissolving the target ester corresponding to the esterification reactant into a preset toluene solution to obtain a target ester solution; defining an adaptive algorithm for initiator concentration of the target ester solution; integrating the free radical initiator into the target ester solution according to the initiator concentration adaptive algorithm to obtain a target polymerization solution; constructing a temperature controller and a degassing device for the target polymer solution; Based on the temperature controller and the degassing device, a polymerization reaction of the target polymerization solution is performed to obtain a polymerization reactant.
[0042] Among them, the esterification standard refers to the pre-set esterification threshold when conducting the esterification reaction, the target ester solution refers to a solution formed by dissolving the target ester that meets the esterification standard in a solvent such as toluene, the initiator concentration adaptive algorithm refers to an algorithm used to determine the appropriate concentration of the free radical initiator added to the target ester solution during the polymerization reaction, the target polymerization solution refers to a solution formed after integrating the free radical initiator into the target ester solution, the temperature controller refers to a controller used to maintain temperature stability during the polymerization reaction, the degassing device refers to a device used to remove oxygen and other gases from the reaction system to prevent these gases from interfering with the polymerization reaction or causing oxidation of the polymer, and the polymerization reactant refers to the product obtained by the polymerization reaction.
[0043] Optionally, the adaptive algorithm for defining the initiator concentration of the target ester solution may be constructed by defining a relationship between the initiator concentration and the corresponding polymerization degree of the target ester solution.
[0044] The degree of polymerization of the polymer reactant calculated in the present invention can reflect the polymerization effect of the polymerization reaction of the polymer reactant.
[0045] In detail, the calculation of the degree of polymerization of the polymer reactant includes: labeling unit monomers of the polymer reactant; determining the monomer molecular weight of the unit monomer; labeling the polymer of the polymeric reaction; analyzing the polymer for polymer molecular weight and polymer mole fraction; Based on the monomer molecular weight, the polymer molecular weight and the polymer mole fraction, the degree of polymerization of the polymer reactant is calculated using the following formula: in, represents the degree of polymerization of the polymer reactant, Indicates the The polymer molecular weight of each polymer, Indicates the The polymer mole fraction of each polymer, Indicates the monomer molecular weight.
[0046] Among them, the unit monomer refers to the basic structural unit that constitutes the polymer, the monomer molecular weight refers to the molecular weight of the basic unit monomer that constitutes the polymer chain, the polymer refers to a macromolecule formed by many repeated monomer units connected by polymerization reaction, the polymer molecular weight refers to the mass of a polymer molecule, and the polymer mole fraction refers to the molar proportion of polymers within a certain molecular weight range in the total polymer sample.
[0047] Optionally, the analysis of the polymer molecular weight and polymer mole fraction of the polymer may be performed by GPC (gel permeation chromatography).
[0048] It should be explained that the cooling polymerization reaction product refers to the reaction product after the polymerization reaction product is subjected to cooling treatment.
[0049] S4. Using a preset silane coupling agent and epoxy resin to perform a modification reaction on the cooling polymerization reactant to obtain a modified resin, obtaining a modification spectrum of the modified resin, and analyzing the modification effect of the modified resin based on the modification spectrum.
[0050] The present invention utilizes a preset silane coupling agent and epoxy resin to carry out a modification reaction on the cooling polymerization reactant to obtain a modified resin, which can improve the performance of the resin.
[0051] In detail, the method of modifying the cooling polymerization reactant using a preset silane coupling agent and an epoxy resin to obtain a modified resin comprises: dissolving the epoxy resin to obtain dissolved epoxy resin; pretreating the silane coupling agent to obtain a pretreated silane coupling agent; Under stirring conditions, integrating the pretreated silane coupling agent and the dissolved epoxy resin into the cooling polymerization reactant to obtain a stirred polymerization reactant; Analyzing the uniformity coefficient of the stirred polymerization reaction product; The stirred polymerization reactant is solidified according to the uniformity coefficient to obtain the modified resin.
[0052] The dissolved epoxy resin refers to completely dissolving the epoxy resin in an appropriate solvent to form a uniform solution. The pretreated silane coupling agent refers to subjecting the silane coupling agent to necessary treatment to enable it to effectively react with the epoxy resin and the cooling polymerization reactant. The stirred polymerization reactant refers to a reactant obtained by mixing the pretreated silane coupling agent and the dissolved epoxy resin into the cooling polymerization reactant under stirring conditions. The uniformity coefficient refers to a parameter that measures the uniformity of distribution of the components in the stirred polymerization reactant. The modified resin refers to a polymerization reactant modified by the silane coupling agent and the epoxy resin.
[0053] Optionally, the analysis of the uniformity coefficient of the stirred polymerization reactant can be performed by measuring the refractive index of the stirred polymerization reactant.
[0054] The present invention obtains a modified spectrum of the modified resin for modification analysis of the modified resin. The modified spectrum refers to a chart used to characterize and record changes in the spectral characteristics of the modified resin. Specifically, the modified spectrum can be constructed by scanning with an FTIR spectrometer.
[0055] The present invention analyzes the modification effect of the modified resin based on the modification spectrum, and can systematically analyze the modification effect of the modified resin to provide a basis for subsequent optimization of the modified resin performance.
[0056] In detail, the analysis of the modification effect of the modified resin according to the modification spectrum includes: Performing baseline correction on the modified spectrum to obtain a corrected modified spectrum; De-noising the corrected modified spectrum to obtain a de-noised modified spectrum; Identifying characteristic absorption peaks of the denoised and modified spectrum; Marking a characteristic peak change of the characteristic absorption peak, wherein the characteristic peak change includes a peak intensity change and a peak position change; Based on the changes in the characteristic peaks, the modification effect of the modified resin is analyzed.
[0057] Among them, the corrected modified spectrum refers to the spectrum after the original modified spectrum is baseline corrected, the denoised modified spectrum refers to the spectrum after the corrected modified spectrum is noise removed, the characteristic absorption peak refers to the absorption peak that appears at a specific wavelength or frequency in the spectrum, the peak intensity change refers to the change in the absorption intensity of the characteristic absorption peak in the spectrum before and after modification, the peak position change refers to the change in the wavenumber or wavelength of the characteristic absorption peak in the spectrum before and after modification, and the modification effect refers to the effect of changing the performance or characteristics of the resin material after modification.
[0058] S5. Based on the modification effect, the modified resin and a preset dispersant are mixed to obtain a mixed dispersion resin, the mixed dispersion resin is ground to obtain a ground dispersion resin, and the boiling resistance coefficient of the ground dispersion resin is calculated. When the boiling resistance coefficient meets a preset boiling resistance threshold, the ground dispersion resin is used as a target dispersion resin.
[0059] It should be explained that the dispersant refers to a chemical substance used to improve the dispersibility of a modified resin in a liquid medium (such as water or an organic solvent), such as polyacrylic acid (PAA) and polymethacrylic acid. The mixed dispersion resin refers to a mixture obtained by mixing a modified resin with a predetermined dispersant in a certain proportion. The ground dispersion resin refers to the product of a mixed dispersion resin subjected to a grinding process. The grinding process typically uses a grinder or sanding equipment to further refine the resin particles through mechanical force, thereby improving the uniformity and stability of the dispersion in the liquid medium.
[0060] The present invention calculates the water boiling resistance coefficient of the grinding dispersion resin to evaluate its durability in specific applications.
[0061] In detail, the calculation of the boiling resistance coefficient of the grinding dispersion resin includes: extracting a resin sample of the ground dispersion resin; integrating the resin sample into a predetermined substrate to obtain a coating substrate; Identifying the glossiness of the coating substrate before boiling; boiling the coating substrate in water to obtain a boiled coating substrate; Identifying the glossiness of the water-boiled coating substrate after water boiling; Based on the glossiness of the substrate before boiling and the glossiness of the substrate after boiling, the boiling resistance coefficient of the grinding dispersion resin is calculated using the following formula: in, Indicates the boiling resistance coefficient of the grinding dispersion resin, Indicates the glossiness of the substrate after boiling in water. Indicates the glossiness of the substrate before boiling.
[0062] Among them, the resin sample refers to a part of the resin taken out from the ground dispersion resin, the coating substrate refers to the material on whose surface the resin sample is evenly coated, usually a glass plate, a metal plate or a plastic sheet, the glossiness of the substrate before water boiling refers to the glossiness value of the coating substrate before water boiling treatment, the water-boiled coating substrate refers to the coating substrate after water boiling treatment, the glossiness of the substrate after water boiling refers to the glossiness value of the coating substrate after water boiling treatment, and the water boiling resistance coefficient refers to a parameter used to quantify the degree of performance retention of the ground dispersion resin after water boiling treatment.
[0063] Finally, in the present invention, when the boiling resistance coefficient meets a preset boiling resistance threshold, the grinding dispersion resin is used to produce a high-performance resin. The boiling resistance threshold refers to a pre-set standard value of the boiling resistance coefficient used to determine whether the boiling resistance performance of the grinding dispersion resin meets specific application requirements. The target dispersion resin refers to a grinding dispersion resin whose boiling resistance coefficient meets the preset boiling resistance threshold after testing and evaluation.
[0064] Compared to the problems described in the background art, first, by removing low-molecular-weight impurities in the polyester polyol, the purity and performance of the final resin are improved, ensuring its stability and reliability in application. Secondly, the dehydration treatment of the acrylic monomer enhances the efficiency of the esterification reaction, so that the synthesized resin has more excellent chemical and physical properties. The temperature adaptive algorithm is used to precisely control the esterification reaction environment, which not only optimizes the reaction rate and conversion rate, but also reduces the generation of by-products, improving the quality of the product. The analysis of the esterification coefficient ensures that the reaction reaches the preset esterification standard, laying the foundation for the smooth progress of the subsequent polymerization reaction. The calculation of the degree of polymerization of the polymer reactant and the cooling treatment further improve the molecular weight and performance of the resin, making it more valuable for application. The modification reaction of the silane coupling agent and the epoxy resin gives the resin better water boiling resistance, adhesion and chemical resistance. Finally, by mixing the dispersant and grinding, a ground dispersion resin with high dispersibility and uniformity is obtained. Therefore, the present invention can improve the water boiling resistance of the synthetic resin.
Claims
1. A method for synthesizing a boiling-resistant acrylic modified polyester dispersion resin, characterized in that: The method comprises: analyzing low molecular weight impurities in the polyester polyol, removing the low molecular weight impurities in the polyester polyol to obtain the target polyester polyol, and dehydrating the acrylic acid monomer to obtain a dehydrated acrylic acid monomer; In a preset reactor, an esterification reaction environment is established for the target polyester polyol and the dehydrated acrylic acid monomer, a temperature adjustment parameter of the esterification reaction environment is determined using a preset temperature adaptive algorithm, an esterification reaction is performed in the esterification reaction environment according to the temperature adjustment parameter, an esterification reactant is obtained, and an esterification coefficient of the esterification reactant is analyzed; When the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are subjected to a polymerization reaction to obtain a polymerization reactant, the polymerization degree of the polymerization reactant is calculated, and the polymerization reactant is cooled according to the polymerization degree to obtain a cooled polymerization reactant; Performing a modification reaction on the cooling polymerization reactant using a preset silane coupling agent and an epoxy resin to obtain a modified resin, obtaining a modification spectrum of the modified resin, and analyzing a modification effect of the modified resin based on the modification spectrum; Based on the modification effect, the modified resin and a preset dispersant are mixed to obtain a mixed dispersion resin, the mixed dispersion resin is ground to obtain a ground dispersion resin, and the boiling resistance coefficient of the ground dispersion resin is calculated. When the boiling resistance coefficient meets the preset boiling resistance threshold, the ground dispersion resin is used as the target dispersion resin.
2. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 1, wherein: The analysis of low molecular weight impurities in polyester polyols comprises: dissolving the polyester polyol to obtain dissolved polyester polyol; filtering the dissolved polyester polyol to obtain filtered dissolved polyester polyol; centrifuging the filtered dissolved polyester polyol to obtain centrifugally dissolved polyester polyol; performing chromatographic separation on the centrifugally dissolved polyester polyol to obtain separated dissolved polyester polyol; analyzing the molecular structure and compound composition of the separated and dissolved polyester polyol; The low molecular weight impurities of the polyester polyol are determined based on the molecular structure and the compound components.
3. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 2, wherein: The step of constructing an esterification reaction environment of the target polyester polyol and the dehydrated acrylic acid monomer in a preset reactor comprises: Establishing high temperature vacuum conditions of the reactor; Analyzing the sealing coefficient of the reactor under the high temperature vacuum condition; When the sealing coefficient meets a preset sealing threshold, preparing the target polyester polyol and the catalyst and green solvent of the dehydrated acrylic acid monomer; analyzing the reactor characteristics of the reactor; Based on the characteristics of the reactor, construct an esterification reaction device for the reactor; An esterification reaction environment of the target polyester polyol and the dehydrated acrylic acid monomer is constructed by the high-temperature vacuum condition, the catalyst, the green solvent and the esterification reaction equipment.
4. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 3, wherein: The method of determining the temperature adjustment parameters of the esterification reaction environment by using a preset temperature adaptive algorithm includes: Initializing algorithm parameters of the temperature adaptive algorithm, wherein the algorithm parameters include a proportional coefficient, an integral coefficient, and a differential coefficient; defining a target temperature of the esterification reaction environment; collecting the current temperature of the esterification reaction environment; Based on the target temperature, the current temperature, and the algorithm parameters, the temperature adjustment parameters of the esterification reaction environment are determined using the temperature adaptive algorithm, wherein the temperature adaptive algorithm: in, Indicates the temperature adjustment parameter of the esterification reaction environment, Indicates the proportional coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature and the target temperature. represents the integral term, Represents the differential coefficient corresponding to the algorithm parameters, Indicates the integral coefficient corresponding to the algorithm parameters, Indicates the temperature deviation between the current temperature of the node and the target temperature in the previous acquisition. Indicates the sampling time interval.
5. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 4, wherein: The analyzing the esterification coefficient of the esterification reactant includes: defining the initial molar number of the esterification reactants; extracting the target ester from the esterification reaction product; Analyzing the purity coefficient of the target ester; Calculating the current molar number of the target ester according to the purity coefficient; An esterification coefficient of the esterification reactant is determined based on the initial mole number and the current mole number.
6. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 5, wherein: When the esterification coefficient meets the preset esterification standard, the esterification reactant and a preset free radical initiator are polymerized to obtain a polymer reactant, comprising: When the esterification coefficient meets the preset esterification standard, dissolving the target ester corresponding to the esterification reactant into a preset toluene solution to obtain a target ester solution; defining an adaptive algorithm for initiator concentration of the target ester solution; integrating the free radical initiator into the target ester solution according to the initiator concentration adaptive algorithm to obtain a target polymerization solution; constructing a temperature controller and a degassing device for the target polymer solution; Based on the temperature controller and the degassing device, a polymerization reaction of the target polymerization solution is performed to obtain a polymerization reactant.
7. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 6, wherein: The calculating the degree of polymerization of the polymer reactant comprises: labeling unit monomers of the polymer reactant; determining the monomer molecular weight of the unit monomer; labeling the polymer of the polymeric reaction; analyzing the polymer for polymer molecular weight and polymer mole fraction; Based on the monomer molecular weight, the polymer molecular weight and the polymer mole fraction, the degree of polymerization of the polymer reactant is calculated using the following formula: in, represents the degree of polymerization of the polymer reactant, Indicates the The polymer molecular weight of each polymer, Indicates the The polymer mole fraction of each polymer, Indicates monomer molecular weight.
8. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 7, wherein: The method of modifying the cooling polymerization reactant by using a preset silane coupling agent and an epoxy resin to obtain a modified resin comprises: dissolving the epoxy resin to obtain dissolved epoxy resin; pretreating the silane coupling agent to obtain a pretreated silane coupling agent; Under stirring conditions, integrating the pretreated silane coupling agent and the dissolved epoxy resin into the cooling polymerization reactant to obtain a stirred polymerization reactant; Analyzing the uniformity coefficient of the stirred polymerization reaction product; The stirred polymerization reactant is solidified according to the uniformity coefficient to obtain the modified resin.
9. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 8, wherein: The step of analyzing the modification effect of the modified resin according to the modification spectrum includes: Performing baseline correction on the modified spectrum to obtain a corrected modified spectrum; De-noising the corrected modified spectrum to obtain a de-noised modified spectrum; Identifying characteristic absorption peaks of the denoised and modified spectrum; Marking a characteristic peak change of the characteristic absorption peak, wherein the characteristic peak change includes a peak intensity change and a peak position change; Based on the changes in the characteristic peaks, the modification effect of the modified resin is analyzed.
10. The method for synthesizing the boiling-resistant acrylic modified polyester dispersion resin according to claim 9, wherein: The calculation of the boiling resistance coefficient of the grinding dispersion resin comprises: extracting a resin sample of the ground dispersion resin; integrating the resin sample into a predetermined substrate to obtain a coating substrate; Identifying the glossiness of the coating substrate before boiling; boiling the coating substrate in water to obtain a boiled coating substrate; Identifying the glossiness of the water-boiled coating substrate after water boiling; Based on the glossiness of the substrate before boiling and the glossiness of the substrate after boiling, the boiling resistance coefficient of the grinding dispersion resin is calculated using the following formula: in, Indicates the boiling resistance coefficient of the grinding dispersion resin, Indicates the glossiness of the substrate after boiling in water. Indicates the glossiness of the substrate before boiling.