A method for optimizing the formulation of HTV silicone rubber insulation materials

By setting up an orthogonal test formula table of aluminum hydroxide content, particle size and mass ratio and surface treatment method, combining electromechanical performance testing and extreme difference analysis, the formulation of HTV silicone rubber insulating material is optimized, the problem of insufficient optimization in the existing technology is solved, the mechanical, electrical and thermal properties of composite insulators are improved, and the aging phenomenon is reduced.

CN118197501BActive Publication Date: 2025-08-12ELECTRIC POWER RES INST CHINA SOUTHERN POWER GRID CO LTD
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Patent Information

Application Number
CN202410421463.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Priority Date
2023-08-29
Filing Date
2024-04-09
Publication Date
2025-08-12
Estimated Expiration
2044-04-09

AI Technical Summary

Technical Problem

The prior art lacks the optimization of multiple factors in the formulation of HTV silicone rubber insulating material, especially the comprehensive consideration of aluminum hydroxide content, particle size and surface treatment method, which makes it difficult for composite insulators to balance between electrocorrosion resistance and pulverization and aging phenomenon.

Method used

By setting the orthogonal test formula table of aluminum hydroxide content, particle size and mass ratio and surface treatment method, combining electromechanical performance testing and extreme difference analysis, the formulation of HTV silicone rubber insulating material is optimized, the TiO2 and SiO2 mass ratio of functional filler TiO2@SiO2 is adjusted, and the mechanical, electrical and thermal properties are optimized.

Benefits of technology

Multi-factor optimization of the HTV silicone rubber insulating material formulation has been achieved, improving the mechanical, electrical and thermal properties of composite insulators, reducing the phenomenon of powder aging, and improving the overall performance stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application belongs to the technical field of insulating materials, and in particular relates to a method for optimizing the formulation of HTV silicone rubber insulating materials. The method for optimizing the formulation of HTV silicone rubber insulating materials provided by the present application first weighs the raw materials of the HTV silicone rubber insulating materials according to an orthogonal test formulation table, and then performs a range analysis on the test results of the mechanical and electrical properties of the HTV silicone rubber insulating materials. According to the range results, the aluminum hydroxide content parameters, particle size ratio parameters, and surface treatment method parameters corresponding to the formulation of the HTV silicone rubber insulating materials with excellent mechanical and electrical properties can be determined. At the same time, the present application can further optimize the mass ratio of TiO2 and SiO2 of the functional filler TiO2@SiO2 in the HTV silicone rubber insulating materials, thereby solving the technical problem in the prior art of lacking the optimization of multiple factors in the formulation of the HTV silicone rubber insulating materials.
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Description

[0001] This application claims priority. The application date of the prior application is August 29, 2023, the application number is 2023111033135, and the name of the invention is: A method for optimizing the formula of HTV silicone rubber insulation material. Technical Field

[0002] The present application belongs to the technical field of insulating materials, and in particular relates to a method for optimizing the formulation of an HTV silicone rubber insulating material. Background Art

[0003] Insulators mainly include ceramic, glass and composite materials. Composite insulators mainly include HTV silicone rubber and other materials. Composite insulators made of HTV silicone rubber insulation materials are widely used in electrical equipment such as transmission lines, substations, urban rail transit vehicles, wind farms and solar power stations.

[0004] HTV silicone rubber insulation material is prepared by vulcanization reaction using methyl vinyl siloxane as the base rubber, adding aluminum hydroxide (ATH) flame retardant, reinforcing agents such as nano-silica, color masterbatches such as ferric oxide, silane coupling agents, crosslinking agents, and vulcanizing agents. In addition to acting as a flame retardant, aluminum hydroxide (ATH) in the HTV silicone rubber insulation formula also improves the material's electrical erosion resistance. However, the addition of aluminum hydroxide (ATH) affects the stable structure of the HTV silicone rubber matrix, PDMS. Degradation of PDMS can cause pulverization and aging of HTV composite insulators. Therefore, increasing the silicone rubber matrix content and reducing the ATH content in the insulator can alleviate the pulverization phenomenon to a certain extent, but it also reduces the electrical erosion resistance of the HTV composite insulator.

[0005] Currently, there is a lack of research on how to optimize the formulation of HTV silicone rubber insulation materials. The commonly used optimization method is to use the aluminum hydroxide (ATH) content as an independent variable in the HTV silicone rubber insulation material formula, test the performance of HTV silicone rubber insulation materials with different aluminum hydroxide (ATH) contents, and select HTV silicone rubber insulation material formulas with better performance. However, this method for optimizing the HTV silicone rubber insulation material formula is relatively simple and can only optimize the single variable of the aluminum hydroxide (ATH) content in the HTV silicone rubber insulation material formula. When multiple variables such as aluminum hydroxide particle size and aluminum hydroxide surface treatment appear, there is no suitable method to optimize the aluminum hydroxide (ATH) content, aluminum hydroxide particle size, and aluminum hydroxide surface treatment in the HTV silicone rubber insulation material formula. The current HTV silicone rubber insulation material formula optimization method lacks optimization of multiple factors in the HTV silicone rubber insulation material formula. Summary of the Invention

[0006] In view of this, the present application provides a method for optimizing the formulation of HTV silicone rubber insulation materials, which is used to solve the technical problem in the prior art of lacking optimization of multiple factors in the formulation of HTV silicone rubber insulation materials.

[0007] The first aspect of the present application provides a method for optimizing the formulation of an HTV silicone rubber insulation material, comprising the steps of:

[0008] Step S1, setting an orthogonal test formula table of aluminum hydroxide according to aluminum hydroxide content parameters, particle size mass ratio parameters and surface treatment method parameters;

[0009] Step S2, weighing the corresponding aluminum hydroxide according to the orthogonal test formula table;

[0010] Step S3, reacting the weighed aluminum hydroxide with methyl vinyl siloxane, functional filler, masterbatch, silane coupling agent, crosslinking agent and vulcanizing agent respectively to obtain HTV silicone rubber insulating material;

[0011] Step S4, performing electromechanical performance testing on the HTV silicone rubber insulation material;

[0012] Step S5: performing range analysis on the electromechanical performance test results of the HTV silicone rubber insulation material, and obtaining an optimized formula of the HTV silicone rubber insulation material according to the results of the range analysis.

[0013] Preferably, in step S1, setting the orthogonal test formula table of aluminum hydroxide according to the aluminum hydroxide content parameter, the particle size mass ratio parameter and the surface treatment method parameter specifically includes:

[0014] An orthogonal experimental formula table was set up based on the aluminum hydroxide content of 100 phr, 110 phr and 120 phr, the mass ratio of 1 μm particle size: 5 μm particle size in aluminum hydroxide of 8:1, 6:1 and 4:1, and the 1 μm particle size and 5 μm particle size aluminum hydroxide were not surface treated, the 1 μm particle size aluminum hydroxide was surface treated and the 5 μm particle size aluminum hydroxide was not surface treated, and the 1 μm particle size aluminum hydroxide was not surface treated and the 5 μm particle size aluminum hydroxide was surface treated.

[0015] Preferably, in step S3, the functional filler is selected from TiO2@SiO2;

[0016] The color masterbatch is selected from ferric oxide;

[0017] The silane coupling agent is selected from KH550 and / or KH560;

[0018] The cross-linking agent is selected from hydrogen-containing silicone oil;

[0019] The vulcanizing agent is selected from 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

[0020] Preferably, in step S4, performing electromechanical performance testing on the HTV silicone rubber insulation material specifically includes:

[0021] HTV silicone rubber insulation materials are tested for hardness, tensile strength, tensile elongation and tear strength, and volume resistivity, breakdown field strength, dielectric constant and dielectric loss tangent.

[0022] Preferably, after step S5, steps S6 to S10 are further included;

[0023] Step S6, adjusting the mass ratios of TiO2 and SiO2 in the functional filler TiO2@SiO2 in the optimized formula of the HTV silicone rubber insulation material to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, and 0.7, to prepare a correlation analysis formula group for the HTV silicone rubber insulation material;

[0024] Step S7, preparing the HTV silicone rubber insulation material correlation analysis group to obtain an HTV silicone rubber insulation material correlation analysis group;

[0025] Step S8, performing electromechanical and thermal performance tests on the HTV silicone rubber insulation material correlation analysis group respectively;

[0026] Step S9, performing correlation analysis on the electromechanical and thermal performance test results of the HTV silicone rubber insulation material correlation analysis group;

[0027] Step S10: performing significance determination on the correlation analysis result of the mass ratio of TiO2 and SiO2.

[0028] In step S8, the HTV silicone rubber insulation material correlation analysis group is subjected to electromechanical and thermal performance tests respectively, including: the HTV silicone rubber insulation material correlation analysis group is subjected to tensile strength, elongation at break, power frequency dielectric constant, power frequency dielectric loss, saturated water absorption rate, thermal weight loss residual mass and hardness tests respectively.

[0029] Preferably, in step S9, the correlation analysis is to perform correlation analysis on the electromechanical and thermal performance test results of the HTV silicone rubber insulation material using the Pearson correlation coefficient r;

[0030] The expression for the correlation analysis using the Pearson correlation coefficient r is:

[0031]

[0032] Where x i and y i are the observed values of two correlated variables, and is the average of two related variables.

[0033] Preferably, in step S10, the significance determination process is: using SPSS software to calculate the correlation coefficient r and the significance level a; when the significance level a is less than 0.01, it is determined that the mechanical properties, electrical performance test, and thermodynamic properties of the HTV silicone rubber insulation material are significantly correlated with the mass ratio;

[0034] When the significance level a is less than 0.05, it is determined that the mechanical properties, electrical performance test and thermodynamic properties of HTV silicone rubber insulation materials are correlated with the mass ratio.

[0035] Preferably, after step S10, the method further includes steps S11 to S15;

[0036] Step S11, adjusting the optimized formula of the HTV silicone rubber insulating material to not add the functional filler TiO2@SiO2, adjusting the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 and 0.7, and adjusting the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 and 0.7 without adding aluminum hydroxide, to obtain an HTV silicone rubber insulating material performance optimization evaluation and analysis group;

[0037] Step S12: preparing an HTV silicone rubber insulation material performance optimization evaluation and analysis group to obtain an HTV silicone rubber insulation material performance optimization evaluation and analysis group;

[0038] Step S13, performing performance optimization evaluation and analysis on the HTV silicone rubber insulation material group, respectively, for tensile strength, thermal weight loss residual mass, and dielectric loss tangent value;

[0039] Step S14: performing performance optimization evaluation analysis on the tensile strength, thermal weight loss residual mass, and dielectric loss tangent test results of the HTV silicone rubber insulation material correlation analysis group;

[0040] Step S15: obtaining an optimized formula of the HTV silicone rubber insulation material based on the results of the performance optimization evaluation analysis;

[0041] In step S14, the performance optimization evaluation formula used in the performance optimization evaluation analysis is:

[0042]

[0043] Where M ATH E is the improvement rate of tensile strength of HTV silicone rubber insulation material after adding ATH; ATH M is the reduction rate of dielectric loss tangent of HTV silicone rubber insulation material after adding ATH; TiO2is the improvement rate of the elongation at break of silicone rubber material after adding core-shell structure TiO2@SiO2 microcapsule material; T TiO2 It is the increase rate of thermal weight loss residual mass after adding core-shell structure TiO2@SiO2 microcapsule material.

[0044] In summary, the present application provides a method for optimizing the formula of HTV silicone rubber insulating material. The method for optimizing the formula of HTV silicone rubber insulating material first prepares HTV silicone rubber insulating material by weighing aluminum hydroxide, methyl vinyl silicone, and other raw rubbers and other fillers according to the orthogonal test formula table, and then performs range analysis on the mechanical and electrical performance test results of the HTV silicone rubber insulating material. The range results can show the aluminum hydroxide content, particle size ratio and surface treatment method that affect the mechanical and electrical properties of the HTV silicone rubber insulating material. The aluminum hydroxide content, particle size ratio and surface treatment method, methyl vinyl silicone, reinforcing agent, masterbatch, silane coupling agent, hydrogen-containing silicone oil, crosslinking agent and vulcanizing agent are used as the optimized formula of the HTV silicone rubber insulating material, thereby solving the technical problem in the prior art of lacking optimization of multiple factors in the formula of the HTV silicone rubber insulating material. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] In order to more clearly illustrate the specific implementation methods of the present application or the technical solutions in the prior art, the following is a brief introduction to the drawings required for use in the specific implementation methods or the description of the prior art. Obviously, the drawings described below are some implementation methods of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0046] Figure 1 This is a schematic flow chart of the method for optimizing the formulation of the HTV silicone rubber insulation material provided in Example 1 of the present application. DETAILED DESCRIPTION

[0047] The present application provides a method for optimizing the formulation of an HTV silicone rubber insulating material, which is used to solve the technical problem in the prior art of lacking the ability to optimize multiple factors in the formulation of an HTV silicone rubber insulating material.

[0048] The following will clearly and completely describe the technical solution of this application in conjunction with the accompanying drawings. Obviously, the embodiments described are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of this application.

[0049] Example 1

[0050] Given that the current optimization method for HTV silicone rubber insulation materials only optimizes a single variable, Example 1 of the present application provides a method for optimizing the formulation of HTV silicone rubber insulation materials;

[0051] The optimization method includes the steps of setting an orthogonal test formula table of aluminum hydroxide, weighing aluminum hydroxide, preparing HTV silicone rubber insulation material, performing electromechanical performance testing on the HTV silicone rubber insulation material, and performing range analysis.

[0052] Among them, the step of setting up the orthogonal test formula table of aluminum hydroxide includes: setting up the orthogonal test formula table of aluminum hydroxide according to the aluminum hydroxide content, particle size mass ratio and surface treatment method, and the orthogonal test formula table is shown in Table 1; wherein, phr refers to the number of grams of aluminum hydroxide added per 100 grams of methyl vinyl silicone raw rubber, and the surface treatment method refers to the silanization treatment of the aluminum hydroxide surface.

[0053]

[0054] Table 1

[0055] The step of weighing aluminum hydroxide includes: weighing aluminum hydroxide according to the orthogonal test formula table shown in Table 1 to obtain corresponding nine aluminum hydroxide raw materials, and the 9 aluminum hydroxide raw materials include: 100 parts of aluminum hydroxide include one-ninth aluminum hydroxide with a particle size of 5 μm, and eight-ninths aluminum hydroxide with a particle size of 1 μm; one-sixth aluminum hydroxide with a particle size of 5 μm, and surface silanization treatment, and five-sixths aluminum hydroxide with a particle size of 1 μm; one-fifth aluminum hydroxide with a particle size of 5 μm, and surface silanization treatment, and four-fifths aluminum hydroxide with a particle size of 1 μm, and surface silanization treatment; the weighing process uses a hundredth of a day balance to weigh, accurate to two decimal places; 110 parts of aluminum hydroxide include one-ninth aluminum hydroxide with a particle size of 5 μm, and surface silanization treatment, and eight-ninths aluminum hydroxide with a particle size of 1 μm. Aluminum, and the surface is silanized; one-sixth of the aluminum hydroxide has a particle size of 5μm, and five-sixths of the aluminum hydroxide has a particle size of 1μm; one-fifth of the aluminum hydroxide has a particle size of 5μm, and the surface is silanized, and four-fifths of the aluminum hydroxide has a particle size of 1μm; the weighing process uses a hundredth of a day balance to weigh, accurate to two decimal places; 120 parts of aluminum hydroxide include one-ninth of the aluminum hydroxide with a particle size of 5μm, and eight-ninths of the aluminum hydroxide with a particle size of 1μm; one-sixth of the aluminum hydroxide has a particle size of 5μm, and the surface is silanized, and five-sixths of the aluminum hydroxide has a particle size of 1μm; one-fifth of the aluminum hydroxide has a particle size of 5μm, and the surface is silanized, and four-fifths of the aluminum hydroxide has a particle size of 1μm and the surface is silanized; the weighing process uses a hundredth of a day balance to weigh, accurate to two decimal places.

[0056] The steps of preparing an HTV silicone rubber insulating material include: adding 9 groups of aluminum hydroxide listed in Table 1 and 4g of a functional filler TiO2@SiO2 to 100g of methyl vinyl silicone rubber raw rubber, respectively, and kneading the mixture thoroughly in a kneader. After the addition process is completed, the mixture is further mixed for 0.5 to 1 hour; then, 3g of a red iron oxide masterbatch, 4g of a KH550 silane coupling agent, and 2g of a hydrogenated silicone oil are added to the kneader, vacuuming the mixture for vacuum meshing at a vacuum degree of 0.05MPa and a temperature of 130 to 160°C, and mixing the mixture for 2 to 3 hours to obtain a rubber mixture; rolling the rubber mixture on an open mill, adding 5g of 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, thinning the mixture into a sheet, and then placing the sheet on a flat vulcanizer for vulcanization molding, wherein the vulcanization temperature is 185°C, the pressure is 12MPa, and the time is 12 minutes, to obtain HTV silicone rubber insulating materials 1-9.

[0057] The steps of conducting electromechanical performance testing on HTV silicone rubber insulation materials include: conducting hardness, tensile strength, tensile elongation and tear strength testing on HTV silicone rubber insulation materials 1-9 and conducting volume resistivity, breakdown field strength, dielectric constant and dielectric loss tangent testing on HTV silicone rubber insulation materials 1-9.

[0058] The steps of performing range analysis include: performing range analysis on the hardness, tensile strength, tensile elongation, and tear strength tests of HTV silicone rubber insulation materials 1-9, and performing range analysis on the volume resistivity, breakdown field strength, dielectric constant, and dielectric loss tangent test results. The influence of each factor on the electromechanical properties is shown in Table 2:

[0059]

[0060]

[0061] Table 2

[0062] In Table 2, the blank columns represent experimental errors and irrelevant factors. According to the range analysis, the range of the blank column is not less than the range of all other factors, indicating that there may be non-negligible interactions between the factors, or other factors that have a significant impact on the experimental results have not been considered. Therefore, when the range values of aluminum hydroxide content, particle size mass ratio, and surface treatment method are not greater than the range values of the blank column, it is considered that the factor has little effect on the electromechanical properties of HTV silicone rubber insulation materials, and the factor is excluded when selecting the optimal solution factors.

[0063] For the other factors that have a significant impact, the following criteria are used to determine: the higher the tensile strength, tensile elongation, tear strength, volume resistivity, and breakdown field strength, the better the electromechanical properties of the silicone rubber sample under these parameters; the lower the dielectric constant and dielectric loss tangent, the better the electrical properties of the silicone rubber sample under these parameters;

[0064] The results of the range analysis are shown in Table 3. In Table 3, “\” indicates that the factor has little effect on the performance, so the parameters are not specifically written.

[0065] Extremely poor Content / phr Particle size ratio Surface treatment hardness 120 \ \ tensile strength 100 8:1 \ Tensile elongation 110 6:1 Large particle size processing Tear strength 100 6:1 Large particle size processing Volume resistivity 100 \ \ Breakdown field strength 110 \ \ Dielectric constant 100 6:1 \ Dielectric loss tangent 100 8:1 All processed

[0066] Table 3

[0067] In the range analysis results, the parameters with the most repetitions for the optimal parameters for each performance factored in were the optimal parameters for overall electromechanical performance. Aluminum hydroxide content of 100 phr appeared five times, particle size ratio of 6:1 appeared three times, and large particle size surface treatment appeared twice. Therefore, the optimized formulation for HTV silicone rubber insulation material contains 100 g of aluminum hydroxide per 100 g of methyl vinyl silicone rubber, a 6:1 mass ratio of 5 μm to 1 μm particles, and silanization of the 5 μm aluminum hydroxide surface treatment.

[0068] It can be determined from Example 1 that the formula optimization method of the HTV silicone rubber insulating material provided in the present application is to first set an orthogonal experimental formula table of aluminum hydroxide content, particle size mass ratio and surface treatment method, then prepare the HTV silicone rubber insulating material corresponding to the orthogonal experimental formula table and perform an electromechanical performance test, and then perform a range analysis on the electromechanical performance test results to obtain the optimized aluminum hydroxide content, particle size mass ratio and surface treatment method, thereby optimizing the formula of the HTV silicone rubber insulating material; the optimized formula of the HTV silicone rubber insulating material is 100phr methyl vinyl silicone rubber raw rubber including 4phr functional filler TiO2@SiO2, 3phr iron oxide red masterbatch, 4phr KH550 silane coupling agent, 2phr hydrogenated silicone oil, 4-6phr 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane and 100phr aluminum hydroxide (in the aluminum hydroxide, the mass ratio of 5μm and 1μm particles is 6:1, and the 5μm aluminum hydroxide is surface treated).

[0069] Example 2

[0070] This Example 2 further optimizes the optimized formula of the HTV silicone rubber insulation material described in Example 1. The optimization process includes setting a correlation analysis formula group, preparing HTV silicone rubber insulation material correlation analysis group samples, conducting electromechanical thermal performance tests, performing correlation analysis, significance judgment, and performance evaluation.

[0071] Among them, setting up the correlation analysis formula group includes: adjusting the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 in the optimized formula of HTV silicone rubber insulation material to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 and 0.7 to configure the HTV silicone rubber insulation material correlation analysis formula group; that is, adjusting the mass ratio of TiO2 and SiO2 in 4phr functional filler TiO2@SiO2 to obtain a correlation analysis formula group including 7 formulas.

[0072] The process of preparing the HTV silicone rubber insulation material correlation analysis group samples is the same as the steps of preparing the HTV silicone rubber insulation material in Example 1.

[0073] The electromechanical and thermal performance tests include: tensile strength, elongation at break, power frequency dielectric constant, power frequency dielectric loss, saturated water absorption, thermal weight loss residual mass and hardness tests.

[0074] Correlation analysis and significance judgment include:

[0075] The Pearson correlation coefficient r is used to perform correlation analysis on the electromechanical thermal performance test results and to make a significance judgment. When the significance level a is less than 0.05, it is considered that the two variables have a certain correlation. When the significance level a is less than 0.01, it is considered that the two variables have a significant correlation. The calculation formula of the Pearson correlation coefficient r is:

[0076]

[0077] In the formula, xi and yi are the observed values of the two related variables, and sum is the average value of the two related variables. Use SPSS software to calculate the significance level a, and then use specialized analysis software to calculate the test statistic t;

[0078]

[0079] Determine the degrees of freedom df = n-2, and use a t-distribution table or statistical software to obtain the value of the significance level a based on the t-statistic and the degrees of freedom df. The calculation results of the correlation coefficient r and the significance level a are shown in Table 4.

[0080] Feature Correlation coefficient r Significance level a Correlation results tensile strength -0.866 0.026 negative correlation Elongation at break -0.939 0.005 Significant negative correlation Power frequency dielectric constant -0.43 0.394 Not relevant Power frequency dielectric loss -0.798 0.057 Not relevant Saturated water absorption 0.533 0.276 Not relevant Thermal loss residual mass 0.962 0.002 Significant positive correlation hardness -0.231 0.087 Not relevant

[0081] Table 4

[0082] According to the correlation analysis results shown in Table 4, the elongation at break and the residual mass after thermal weight loss of HTV silicone rubber insulation materials are significantly correlated with the mass ratio of TiO2 and SiO2. Therefore, in order to optimize the elongation at break and the residual mass after thermal weight loss of HTV silicone rubber insulation materials, the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 can be adjusted to optimize the elongation at break and the residual mass after thermal weight loss of HTV silicone rubber insulation materials.

[0083] The performance evaluation includes: preparing HTV silicone rubber insulation materials 11-17 and HTV silicone rubber insulation materials 18-24 and 10 for comparison according to the steps for preparing the HTV silicone rubber insulation material in Example 1; then measuring the tensile strength, thermal weight loss residual mass, and dielectric loss tangent of the HTV silicone rubber insulation materials 10-24 according to the operating requirements of the composite insulator, and performing performance optimization evaluation.

[0084] Wherein, the preparation method of HTV silicone rubber insulation material 11-17 is:

[0085] Add 100g of aluminum hydroxide and 4g of functional filler TiO2@SiO2 to 100g of methyl vinyl silicone rubber, then fully knead in a kneader. After the addition process is completed, mix for 0.5 to 1 hour; then add 3g of ferric oxide red masterbatch, 4g of KH550 silane coupling agent, and 2g of hydrogenated silicone oil to the kneader, evacuate and perform vacuum meshing, the vacuum degree is 0.05MPa, the temperature is 130 to 160℃, and mix for 2 to 3h to obtain a rubber compound; Roll the mixing mill, add 5 g of 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, thinly sheet the mixture, and then place the sheet on a flat vulcanizer for vulcanization molding; wherein the vulcanization temperature is 185°C, the pressure is 12 MPa, and the time is 12 min. In 4 g of the functional filler TiO2@SiO2, the mass ratios of TiO2 and SiO2 are 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, and 0.7, respectively, to obtain HTV silicone rubber insulation material 10-16.

[0086] The difference between the preparation methods of HTV silicone rubber insulation materials 18-24 and 11-17 is that 100g of aluminum hydroxide is not added to 4g of the functional filler TiO2@SiO2 when the mass ratio of TiO2 to SiO2 is 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, and 0.7, respectively. The difference between the preparation methods of HTV silicone rubber insulation material 10 and 11-17 is that 4g of the functional filler TiO2@SiO2 is not added.

[0087] The performance optimization evaluation includes: obtaining the performance optimization evaluation coefficient Tz based on the tensile strength of the HTV silicone rubber insulation material at 10-24, the residual mass after thermal weight loss, the dielectric loss tangent value, and the performance optimization evaluation formula; the larger the performance optimization evaluation coefficient Tz, the better the performance optimization of the HTV silicone rubber insulation material; wherein, the performance optimization evaluation formula is:

[0088]

[0089] Where M ATH E is the improvement rate of tensile strength of HTV silicone rubber insulation material after adding ATH; ATH It is the reduction rate of the dielectric loss tangent value of the HTV silicone rubber insulation material after adding ATH; that is, compared with the HTV silicone rubber insulation materials 18-24, the improvement rate of the tensile strength and the reduction rate of the dielectric loss tangent value of the HTV silicone rubber insulation materials 11-17.

[0090] M TiO2 is the improvement rate of the elongation at break of silicone rubber material after adding core-shell structure TiO2@SiO2 microcapsule material; T TiO2 It is the increase rate of thermal weight loss residual mass after adding core-shell structure TiO2@SiO2 microcapsule material; based on the increase rate of elongation at break and thermal weight loss residual mass of HTV silicone rubber insulation materials 11-17 compared with HTV silicone rubber insulation material 10.

[0091] The performance optimization evaluation coefficient Tz obtained by calculation is shown in Table 5:

[0092] X 0.1 0.2 0.3 0.4 0.5 0.6 0.7 <![CDATA[T z ]]> 0.053 0.098 0.145 0.147 0.149 0.109 0.045

[0093] Table 5

[0094] As can be seen from Table 5, in 4g of functional filler TiO2@SiO2, the mass ratio of TiO2 to SiO2 is 0.5, that is, when the mass of TiO2 and SiO2 is both 2g, the performance of the HTV silicone rubber insulation material is better optimized; that is, Example 2 of the present application is further optimized on the basis of the HTV silicone rubber insulation material formula provided in Example 1 to obtain the HTV silicone rubber insulation material formula: 100phr methyl vinyl silicone rubber raw rubber includes 4phr functional filler TiO2@SiO2, 3phr iron oxide red masterbatch, 4phr KH550 silane coupling agent, 2phr hydrogenated silicone oil, 4-6phr 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane and 100phr aluminum hydroxide (in the aluminum hydroxide, the mass ratio of 5μm and 1μm particle size is 6:1, the 5μm aluminum hydroxide is surface-treated, and in the functional filler TiO2@SiO2, the mass ratio of TiO2 to SiO2 is 0.5).

[0095] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for optimizing the formulation of HTV silicone rubber insulation materials, characterized in that: Including steps: Step S1, setting an orthogonal test formula table of aluminum hydroxide according to aluminum hydroxide content parameters, particle size mass ratio parameters and surface treatment method parameters; Step S2, weighing the corresponding aluminum hydroxide according to the orthogonal test formula table; Step S3, reacting the weighed aluminum hydroxide with methyl vinyl siloxane, functional filler, masterbatch, silane coupling agent, crosslinking agent and vulcanizing agent respectively to obtain HTV silicone rubber insulating material; Step S4, performing electromechanical performance testing on the HTV silicone rubber insulation material; Step S5, performing range analysis on the electromechanical performance test results of the HTV silicone rubber insulation material, and obtaining an optimized formula of the HTV silicone rubber insulation material according to the results of the range analysis; Step S6, adjusting the mass ratios of TiO2 and SiO2 in the functional filler TiO2@SiO2 in the optimized formula of the HTV silicone rubber insulation material to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, and 0.7, to prepare a correlation analysis formula group for the HTV silicone rubber insulation material; Step S7, preparing the HTV silicone rubber insulation material correlation analysis group to obtain an HTV silicone rubber insulation material correlation analysis group; Step S8, performing electromechanical and thermal performance tests on the HTV silicone rubber insulation material correlation analysis group respectively; Step S9, performing correlation analysis on the electromechanical and thermal performance test results of the HTV silicone rubber insulation material correlation analysis group; Step S10: performing significance determination on the correlation analysis result of the mass ratio of TiO2 and SiO2.

2. The method for optimizing the formulation of an HTV silicone rubber insulating material according to claim 1, characterized in that: In step S1, setting an orthogonal test formula table of aluminum hydroxide according to the aluminum hydroxide content parameter, the particle size mass ratio parameter, and the surface treatment method parameter specifically includes: An orthogonal experimental formula table was set up based on the aluminum hydroxide content of 100 phr, 110 phr and 120 phr, the mass ratio of 1 μm particle size: 5 μm particle size in aluminum hydroxide of 8:1, 6:1 and 4:1, and the 1 μm particle size and 5 μm particle size aluminum hydroxide were not surface treated, the 1 μm particle size aluminum hydroxide was surface treated and the 5 μm particle size aluminum hydroxide was not surface treated, and the 1 μm particle size aluminum hydroxide was not surface treated and the 5 μm particle size aluminum hydroxide was surface treated.

3. The method for optimizing the formulation of an HTV silicone rubber insulating material according to claim 1, characterized in that: In step S3, the functional filler is selected from TiO2@SiO2; The color masterbatch is selected from ferric oxide; The silane coupling agent is selected from KH550 and / or KH560; The cross-linking agent is selected from hydrogen-containing silicone oil; The vulcanizing agent is selected from 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

4. The method for optimizing the formulation of an HTV silicone rubber insulating material according to claim 1, wherein: In step S4, the electromechanical performance test of the HTV silicone rubber insulation material specifically includes: HTV silicone rubber insulation materials are tested for hardness, tensile strength, tensile elongation and tear strength, and volume resistivity, breakdown field strength, dielectric constant and dielectric loss tangent.

5. The method for optimizing the formulation of an HTV silicone rubber insulating material according to claim 1, characterized in that: In step S8, the HTV silicone rubber insulation material correlation analysis group is subjected to electromechanical and thermal performance tests, including: the HTV silicone rubber insulation material correlation analysis group is subjected to tensile strength, elongation at break, power frequency dielectric constant, power frequency dielectric loss, saturated water absorption, thermal weight loss residual mass and hardness tests.

6. The method for optimizing the formulation of an HTV silicone rubber insulating material according to claim 1, characterized in that: In step S9, the correlation analysis is to perform correlation analysis on the electromechanical and thermal performance test results of the HTV silicone rubber insulation material using the Pearson correlation coefficient r; The calculation formula for performing the correlation analysis is: Where x i and y i are the observed values of two correlated variables, and is the average of two related variables.

7. The method for optimizing the formulation of an HTV silicone rubber insulation material according to claim 1, characterized in that: In step S10, the significance determination process is as follows: when the significance level a is less than 0.01, it is determined that the mechanical properties, electrical performance test, and thermodynamic properties of the HTV silicone rubber insulation material are significantly correlated with the mass ratio; When the significance level a is less than 0.05, it is determined that the mechanical properties, electrical performance test and thermodynamic properties of HTV silicone rubber insulation materials are correlated with the mass ratio.

8. The method for optimizing the formulation of HTV silicone rubber insulation materials according to claim 5, characterized in that: In step S10, the significance of the correlation analysis result of the mass ratio of TiO2 and SiO2 is determined by using a t-distribution table or statistical software to obtain a value of a significance level a according to the t-statistic and the degree of freedom df; The calculation formula for the t statistic and degrees of freedom df is: Where t is the statistic and n-2 is the degrees of freedom.

9. The method for optimizing the formulation of an HTV silicone rubber insulation material according to claim 1, characterized in that: After step S10, the method further includes steps S11 to S15; Step S11, adjusting the optimized formula of the HTV silicone rubber insulating material to not add the functional filler TiO2@SiO2, adjusting the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 and 0.7, and adjusting the mass ratio of TiO2 and SiO2 in the functional filler TiO2@SiO2 to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 and 0.7 without adding aluminum hydroxide, to obtain an HTV silicone rubber insulating material performance optimization evaluation and analysis group; Step S12: preparing an HTV silicone rubber insulation material performance optimization evaluation and analysis group to obtain an HTV silicone rubber insulation material performance optimization evaluation and analysis group; Step S13, performing performance optimization evaluation and analysis on the HTV silicone rubber insulation material group, respectively, for tensile strength, thermal weight loss residual mass, and dielectric loss tangent value; Step S14: performing performance optimization evaluation analysis on the tensile strength, thermal weight loss residual mass, and dielectric loss tangent test results of the HTV silicone rubber insulation material correlation analysis group; Step S15: obtaining an optimized formula of the HTV silicone rubber insulation material based on the results of the performance optimization evaluation analysis; In step S14, the performance optimization evaluation formula used in the performance optimization evaluation analysis is: Where M ATH E is the improvement rate of tensile strength of HTV silicone rubber insulation material after adding ATH; ATH M is the reduction rate of dielectric loss tangent of HTV silicone rubber insulation material after adding ATH; TiO2 is the improvement rate of the elongation at break of silicone rubber material after adding core-shell structure TiO2@SiO2 microcapsule material; T TiO2 It is the increase rate of thermal weight loss residual mass after adding core-shell structure TiO2@SiO2 microcapsule material.

Citation Information

Patent Citations

  • A determination method for vulcanization parameters of an HTV insulating material with excellent electromechanical performance

    CN108776214A

  • Silicone Rubber With ATH Filler

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