Method for regulating impurity ions of epoxy resin and regulating material and preparation method thereof
By constructing core-shell microcapsules with an ionic liquid functional layer and an anion and cation exchange resin core and shell working together, the problem of low removal efficiency of impurity ions in epoxy resin insulating materials is solved, improving insulation performance and stability, and making them suitable for high-voltage electrical and electronic packaging applications.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- MEGAVOLT TECH (SUZHOU) CO LTD
- Filing Date
- 2026-04-13
- Publication Date
- 2026-06-19
AI Technical Summary
Existing epoxy resin insulation materials are difficult to effectively remove impurity ions in high-voltage electrical and electronic packaging applications, resulting in electric field distortion, increased dielectric loss, reduced breakdown field strength, and shortened service life. Traditional ion exchange materials suffer from low ion exchange efficiency and poor stability.
The core-shell structure microcapsules, which employ a microcapsule structure with an ionic liquid functional layer and an anion and cation exchange resin core and shell working in synergy, promote the migration and diffusion of impurity ions through ionic liquid and improve dispersibility and interfacial compatibility through shell modification, thereby achieving deep removal and long-term stable storage of impurity ions.
It significantly improves the volume resistivity and breakdown field strength of epoxy resin, reduces dielectric loss, and extends the service life of insulating devices. Furthermore, the process is controllable and the raw materials are readily available, making it suitable for the field of high-end insulating materials.
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Figure CN122234528A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of polymer insulating materials technology, specifically relating to a functional material and preparation method for regulating the content of impurity ions in epoxy resin systems, and particularly to an ion exchange resin microcapsule containing an ionic liquid functional layer and its application in epoxy composite materials for high-voltage electrical insulation and electronic packaging. Background Technology
[0002] With the development of science and technology and the increase in social demand, higher requirements are being placed on insulation materials. For example, in fields such as ultra-high voltage power transmission, superconducting technology, and new energy vehicles, new insulation materials with excellent properties such as high breakdown strength, low dielectric loss, and high thermal conductivity are needed. However, existing insulation materials often fail to meet these requirements, or suffer from problems such as excessive cost, substandard parameters, and short service life. Therefore, developing new, efficient, energy-saving, environmentally friendly, safe, and sustainable insulation materials is an important need in today's society.
[0003] Epoxy resins are widely used in key fields such as high-voltage electrical insulation, electronic component encapsulation, and power composite materials due to their excellent mechanical properties, adhesive properties, electrical insulation properties, and processability. During the synthesis, storage, and curing of epoxy resins, residual epoxy resins inevitably remain within the system. , , Trace amounts of impurity ions. These ions are prone to directional migration and accumulation under the action of DC or alternating electric fields, causing distortion of the internal electric field of the material, resulting in a decrease in the volume resistivity of epoxy resin, an increase in dielectric loss, and a reduction in breakdown field strength, which seriously shortens the service life and operational reliability of insulating devices under high temperature, high humidity, and strong electric field conditions.
[0004] Currently, the control of impurity ions in epoxy systems mainly employs techniques such as ion exchange resin adsorption, inorganic filler physical adsorption, and chemical complexation. While traditional ion exchange materials possess a certain ion removal capability, they suffer from significant drawbacks: First, ion exchange resins have low surface energy and poor compatibility with epoxy groups, making them prone to aggregation and difficult to achieve uniform dispersion. Second, impurity ions diffuse slowly within resin particles, limiting ion transport and resulting in low exchange efficiency. Third, their effect on complexed and weakly bound impurity ions is limited, making deep removal difficult. Fourth, the ion exchange process is reversible, and ion re-release is common in humid and hot environments, hindering long-term stable fixation. Furthermore, conventional adsorption fillers have limited functionality, failing to simultaneously address rapid ion migration, efficient capture, and stable latch-up, thus failing to meet the stringent requirements of high-end insulating materials for low ion impurities and high insulation stability.
[0005] Therefore, developing a novel control material that combines ion migration promotion, deep exchange capture, and long-term stable fixation functions has significant engineering application value for improving the comprehensive electrical properties and environmental stability of epoxy resin-based insulation materials. Summary of the Invention
[0006] To address the problems existing in the above-mentioned technologies, the present invention provides a method for controlling impurity ions in epoxy resin, as well as the control material and its preparation method, which achieves deep removal of impurity ions and significantly reduces the risk of ion conduction in the system.
[0007] The objective of this invention is achieved through the following technical solution:
[0008] A material for controlling impurity ions in epoxy resin, the material being composed of microcapsules, the microcapsules comprising a resin core and... Shell, and the resin core and At least a portion between the shell layers is filled with an ionic liquid layer, and the resin core comprises a cation exchange resin and an anion exchange resin.
[0009] Preferably, the ionic liquid is selected from imidazole or quaternary ammonium salt ionic liquids;
[0010] Preferably, the cation exchange resin is a resin containing sulfonic acid groups. Strongly acidic cation exchange resins, including type 732 cation exchange resin, are used in adsorption systems. , Isocational impurities;
[0011] Anion exchange resins are strongly basic anion exchange resins containing quaternary ammonium groups. Strongly basic anion exchange resins include type 717 anion exchange resins, used in adsorption systems. Anionic impurities.
[0012] Preferably, the The shell is a shell whose surface has been treated with a silane coupling agent.
[0013] Preferably, the microcapsules have a particle size of 1-20 μm.
[0014] Preferably, the resin core has a mass of 10 parts, and the ionic liquid layer has a mass of 0.5 to 1 part. The mass of the shell is 4-8 parts;
[0015] The mass ratio of cation exchange resin to anion exchange resin in the resin core is 1:2 to 1:1.
[0016] The preparation method of the epoxy resin impurity ion control material provided by the present invention includes the following steps:
[0017] Step S1: Preparation of resin micro powder: Cation exchange resin and anion exchange resin are pulverized to a particle size of 1-10 μm to obtain micro powder;
[0018] Step S2: Ionic liquid composite treatment, dissolving the ionic liquid in a mixed solvent of water and ethanol; adding resin micro powder to the solution; stirring to coat the resin surface with the ionic liquid; obtaining ionic liquid modified resin composite particles;
[0019] Step S3: Dispersion and emulsification: The composite particles are added to the aqueous phase containing the dispersant and sheared to disperse them, forming a stable suspension system;
[0020] Step S4: Shell Construction: A silicon source is added to the system, and a sol-gel reaction is carried out under alkaline conditions to form a shell. Shell;
[0021] Step S5: Surface modification: The shell surface is modified with a silane coupling agent to improve compatibility with epoxy resin.
[0022] Step S6: Post-processing: Separate, wash and dry to obtain microcapsules.
[0023] The present invention provides a method for preparing epoxy resin impurity ion control materials, which includes the following steps:
[0024] In step S1: ion exchange resin pretreatment: cation exchange resin and anion exchange resin are taken separately and washed multiple times with deionized water to remove surface-soluble impurities; then washed multiple times with anhydrous ethanol to remove organic residues; then dried in a vacuum drying oven for later use; pulverization and grinding: the dried ion exchange resin is added to a planetary ball mill for pulverization; after ball milling, the sample is sieved, and the particle size distribution is detected using a laser particle size analyzer to control the overall D50 particle size of the resin powder within 1-10 μm;
[0025] In step S2: Prepare the ionic liquid solution: Weigh the ionic liquid and add it to a mixed solvent composed of anhydrous ethanol and deionized water. Stir magnetically at room temperature to form a uniform and transparent solution. Weigh the ion exchange resin powder obtained in step S1 and slowly add it to the above ionic liquid solution.
[0026] Composite adsorption treatment: First, premix by magnetic stirring, then ultrasonically disperse; then continue mechanical stirring; during this process, the ionic liquid gradually adsorbs, wets and partially impregnates the surface and pore structure of the ion exchange resin particles, thereby obtaining ion liquid modified resin composite particles; solid-liquid separation: centrifuge the obtained suspension; discard the supernatant and wash quickly with a small amount of ethanol to remove unadsorbed free ionic liquid; drying: place the precipitate in a vacuum environment to dry, thereby obtaining ion liquid modified resin composite particles;
[0027] In step S3: Dispersion and emulsification: Preparation of the dispersion aqueous phase: Take deionized water, add polyvinyl alcohol (PVA), stir and dissolve at 80°C to prepare a PVA aqueous solution; cool to room temperature for later use; Add composite particles: Slowly add the ionic liquid modified resin composite particles obtained in step S2 to the above PVA aqueous solution; Shear dispersion: Use a shear emulsifier (e.g., a high-speed shear emulsifier, speed 5000-7000 rpm) for dispersion treatment; Shear while adding material, and maintain the system temperature not exceeding 35°C during the shearing process; Formation of a suspension system: After the treatment, a stable suspension system with uniform dispersion and no obvious sedimentation is obtained;
[0028] In step S4: Shell construction: The reaction system is established by adding anhydrous ethanol to the suspension system obtained in step S3 to improve the dispersion and hydrolysis conditions of tetraethyl orthosilicate (TEOS) in the system; then stirring at room temperature; adjusting the pH by slowly adding ammonia to the system to adjust the pH to 9.5-10.5; adding the silicon source, tetraethyl orthosilicate, which is pre-diluted with anhydrous ethanol, and then slowly added to the above system under stirring, with the addition time controlled at 20-30 min; sol-gel coating reaction: After the TEOS is added, the reaction is stirred continuously. Under alkaline conditions, TEOS undergoes hydrolysis and condensation reactions, gradually depositing on the surface of the composite particles and forming a continuous layer. Shell;
[0029] In step S5: Surface modification: Modifier is added, and silane coupling agent KH560 is added to the system after the reaction in step S4, and the reaction is continued with stirring; KH560 and The hydroxyl groups on the shell surface undergo a condensation reaction and form an organosilane modified layer on the particle surface, thereby improving its interfacial compatibility in epoxy resin.
[0030] In step S6: Post-processing: The system after the reaction in step S5 is centrifuged; Washing: Washed sequentially with deionized water and anhydrous ethanol; Centrifuged after each wash to remove unreacted silicon source, ammonia and free coupling agent; Drying: The washed microcapsules are placed in a vacuum drying oven to dry.
[0031] After drying, the powder is ground or lightly sieved to break up soft agglomerated particles and obtain microcapsule powder with good flowability. The final product is a light white or pale yellow microcapsule powder, which is a functional material used for the regulation of impurity ions in epoxy resin.
[0032] The present invention also provides a method for controlling impurity ions in epoxy resin, which includes the following steps:
[0033] Step 1: Epoxy resin matrix preparation: Select an epoxy system (e.g., a conventional epoxy system or an existing epoxy system), place it in a mixing container, preheat it to reduce its viscosity, and facilitate subsequent dispersion.
[0034] Step 2: Microcapsule addition, add the above microcapsules to the epoxy resin;
[0035] Step 3: Pre-dispersion treatment: mechanical stirring;
[0036] Step 4: Degassing treatment. The mixture is placed in a vacuum environment to degas in order to prevent air bubbles from affecting the insulation performance.
[0037] Preferably, in step 1, the preheating is carried out at 40-60℃; in step 3, the mechanical stirring speed is 500-1000 rpm and the time is 15-30 min; in step 4, the vacuum degree is -0.08 MPa and the time is 10-20 min.
[0038] Compared with the prior art, the beneficial effects of the present invention include at least the following:
[0039] This invention constructs an ionic liquid functional layer, an anion and cation exchange resin core, and... Core-shell structured microcapsules with synergistic shell-shell structure have significant beneficial effects when applied to epoxy resin insulating materials:
[0040] A composite system of cation and anion exchange resins can be used to simultaneously and efficiently adsorb and remove impurities from epoxy resin systems. , isocations and The removal of anionic impurities enables deep removal of impurity ions, significantly reducing the risk of ion conduction in the system.
[0041] Introducing an ionic liquid functional layer can effectively promote the rapid migration and diffusion of impurity ions into the resin interior, thereby increasing the ion exchange rate and exchange capacity, while preventing ion re-release and achieving long-term stable storage.
[0042] pass Shell coating and KH560 surface modification significantly improve the dispersibility and interfacial compatibility of microcapsules in epoxy resin, reduce interfacial defects, and avoid electric field distortion and local breakdown caused by agglomeration.
[0043] The resulting composite material exhibits significantly improved volume resistivity and breakdown field strength, reduced dielectric loss, and maintains excellent insulation stability under high temperature, high humidity, and strong electric field conditions, thus extending the service life of insulating devices.
[0044] The preparation process is mild and controllable, the raw materials are readily available and have good repeatability, making it easy to scale up production. It is suitable for high-end epoxy insulation materials such as high-voltage electrical insulation and electronic component packaging. Attached Figure Description
[0045] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0046] Figure 1 This is an electron microscope scan image of the microcapsules prepared in Example 1 of the present invention. Detailed Implementation
[0047] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0048] Example 1: Preparation of ion exchange resin microcapsules with ionic liquid functional layers:
[0049] Step S1: Preparation of resin micronized powder: Take 5g of cation exchange resin (732 type cation exchange resin) and 5g of anion exchange resin (717 type anion exchange resin), wash thoroughly with deionized water 3 times to remove soluble impurities on the surface, and then wash twice with anhydrous ethanol to remove organic residues. Place the washed resin in a vacuum drying oven at 60℃ and dry for 12 hours for later use. Add the dried resin to a planetary ball mill and ball mill for 4 hours at a ball-to-material ratio of 10:1, a rotation speed of 350 rpm, and zirconia balls as the medium. After ball milling, sieve and use a laser particle size analyzer to detect the particle size distribution, controlling the overall particle size (D50) of the resin powder to be 1-10 μm. Place the obtained resin micronized powder in a desiccator for later use.
[0050] Step S2: Ionic Liquid Composite Treatment: Weigh 1g of 1-ethyl-3-methylimidazolium tetrafluoroborate (in other examples, 0.5g, 2g, or 3g) of imidazole ionic liquid and add it to a mixed solvent consisting of 80mL anhydrous ethanol and 20mL deionized water. Stir magnetically at room temperature for 10min to obtain a uniform and transparent solution. Weigh 10.0g of the resin micropowder obtained in Step S1 and slowly add it to the above solution. First, premix magnetically for 20min, then ultrasonically disperse for 30min, controlling the temperature at 25-30℃, followed by mechanical stirring for 2h to allow the ionic liquid to adsorb, wet, and impregnate the surface and pore structure of the resin particles. Centrifuge the resulting suspension at 4000rpm for 10min, discard the supernatant, wash once quickly with a small amount of ethanol, and dry the precipitate in a vacuum environment at 40℃ for 6h to obtain ionic liquid modified resin composite particles.
[0051] Step S3: Dispersion and Emulsification: Take 200 mL of deionized water, add 4.0 g of PVA, stir and dissolve at 80 °C for 30 min to prepare a PVA aqueous solution with a mass fraction of approximately 2 wt%, and cool to room temperature for later use. Slowly add the ionic liquid modified resin composite particles obtained in Step S2 to the above PVA aqueous solution, and disperse using a high-speed shear emulsifier at 6000 rpm and 25 °C for 15 min, controlling the system temperature to not exceed 35 °C, to obtain a stable suspension system with uniform dispersion and no obvious sedimentation.
[0052] Step S4: Shell Construction: Add 80 mL of anhydrous ethanol to the suspension system obtained in Step S3, stir at room temperature for 10 min, and slowly add ammonia to adjust the pH of the system to 9.5-10.5. Weigh 8 g of TEOS (tetraethyl orthosilicate) (in other examples, this can be 6 g, 7 g, 10 g, or 9 g), pre-dilute with 20 mL of anhydrous ethanol, and slowly add it to the system with stirring over 20-30 min. After the addition is complete, stir the reaction at 35℃-40℃ for 4 h. TEOS hydrolyzes and condenses under alkaline conditions, forming a continuous layer on the surface of the composite particles. After the reaction is complete, allow the shell to stand for 2 hours to age.
[0053] Step S5: Surface Modification: Add 1.0 g of KH560 (or 0.5 g, 1.2 g, 2 g, or 0.2 g in other embodiments) to the system after the reaction in Step S4, and stir the mixture at 50°C for 2 hours. KH560 reacts with... The condensation of hydroxyl groups on the shell surface forms an organosilane modified layer, which improves the interfacial compatibility between the microcapsule and the epoxy resin.
[0054] Step S6: Post-processing: Centrifuge the system after the reaction in step S5 at 5000 rpm for 10 min, and wash twice each with deionized water and anhydrous ethanol. Centrifuge after each wash to remove unreacted silicon source, ammonia, and free coupling agent. Place the washed microcapsules in a vacuum drying oven and dry at 50℃ and –0.08 MPa for 12 h. After drying, lightly grind or sieve to break up soft agglomerated particles to obtain light white or pale yellow microcapsule powder.
[0055] Application of microcapsules in epoxy resin insulating materials:
[0056] Step 1: Preparation of epoxy resin matrix: Weigh 100 parts by weight of bisphenol A type epoxy resin E-51, place it in a stirring container, and preheat it at 50°C to reduce its viscosity and facilitate subsequent dispersion.
[0057] Step 2: Microcapsule addition: Add the microcapsules prepared above to the epoxy resin. The amount added is 0.01% of the mass of the epoxy resin (adjusted according to the actual ion concentration, such as 0.02% or 0.03%).
[0058] Step 3: Pre-dispersion treatment: Mechanically stir at 500-1000 r / min for 20 min, and control the system temperature below 50℃ to ensure uniform dispersion of microcapsules.
[0059] Step 4: Degassing treatment: Degas the mixture under a vacuum of -0.08MPa for 20 minutes to eliminate bubbles and ensure insulation performance.
[0060] Step 5: Allow to cool naturally to room temperature to obtain an epoxy resin composite insulating material containing ion exchange resin microcapsules with an ion liquid functional layer.
[0061] The modified epoxy resin composite insulation material obtained can be processed and produced using existing technologies, which will not be elaborated here.
[0062] like Figure 1 As shown in the figure, this is a scanning electron microscope (SEM) morphology image of the ion exchange resin microcapsules of the ion liquid functional layer described in this invention. The image shows that the prepared microcapsules are regularly spherical or near-spherical, with uniform particle distribution and clear boundaries. The diameter of a single microcapsule is approximately 3-5 μm. This confirms... The coating layer successfully constructed a core-shell structure. This surface can effectively improve the dispersibility of microcapsules in the epoxy resin matrix, while increasing the contact area between the ionic liquid and the resin, providing a structural basis for the migration and capture of impurity ions.
[0063] Example 2
[0064] Compared with Example 1, only the amount of 1-ethyl-3-methylimidazolium tetrafluoroborate in step S2 was adjusted to 0.8g, while the other raw materials, preparation process, parameters and application methods were the same as in Example 1.
[0065] Example 3
[0066] Compared with Example 1, only the amount of TEOS used in step S4 was adjusted to 6g, while the other raw materials, preparation process, parameters and application methods were the same as in Example 1.
[0067] Example 4
[0068] Compared with Example 1, only the amount of microcapsules added in the application step was adjusted to 0.02% of the epoxy resin mass, while the other raw materials, preparation process and parameters were the same as in Example 1.
[0069] Scale settings
[0070] Comparative Example 1 (Blank Control Group)
[0071] No microcapsules were added, and the selection of other epoxy resins, curing regimes, and processing techniques were the same as in Example 1.
[0072] Comparative Example 2 (Non-ionic liquid group)
[0073] No ionic liquid was added during the preparation of the microcapsules, and the other raw materials, ratios, and process parameters were the same as in Example 1.
[0074] Performance Comparison Table and Effect Description
[0075] The test results are shown in Table 1, which compares the performance of each group of epoxy resin insulation materials.
[0076] Table 1
[0077]
[0078] Data Explanation: As can be seen from the data in Table 1, in the blank epoxy resin system The content is 85 ppm. The concentration was 18 ppm, indicating a high content of impurity ions and poor insulation performance. Comparative Example 2, without added ionic liquid, only showed some adsorption effect on impurity ions, with an ion removal rate of less than 60%, resulting in limited improvement in insulation performance.
[0079] The embodiments 1-4 of this invention further improve the ion removal by about 30% based on Comparative Example 2, significantly reduce the impurity ion content, and significantly improve the breakdown strength. This indicates that the ionic liquid, core-shell structure and anionic resin have a significant synergistic effect, which can effectively reduce the content of migratable impurity ions in the epoxy system and significantly improve the dielectric properties and stability of the insulating material.
[0080] This invention constructs an ionic liquid functional layer, an anion and cation exchange resin core, and... Core-shell structured microcapsules with synergistic shell-shell structure have significant beneficial effects when applied to epoxy resin insulating materials:
[0081] A composite system of cation and anion exchange resins can be used to simultaneously and efficiently adsorb and remove impurities from epoxy resin systems. , isocations and The removal of anionic impurities enables deep removal of impurity ions, significantly reducing the risk of ion conduction in the system.
[0082] Introducing an ionic liquid functional layer can effectively promote the rapid migration and diffusion of impurity ions into the resin interior, thereby increasing the ion exchange rate and exchange capacity, while preventing ion re-release and achieving long-term stable storage.
[0083] pass Shell coating and KH560 surface modification significantly improve the dispersibility and interfacial compatibility of microcapsules in epoxy resin, reduce interfacial defects, and avoid electric field distortion and local breakdown caused by agglomeration.
[0084] The resulting composite material exhibits significantly improved volume resistivity and breakdown field strength, reduced dielectric loss, and maintains excellent insulation stability under high temperature, high humidity, and strong electric field conditions, thus extending the service life of insulating devices.
[0085] The preparation process is mild and controllable, the raw materials are readily available and have good repeatability, making it easy to scale up production. It is suitable for high-end epoxy insulation materials such as high-voltage electrical insulation and electronic component packaging.
[0086] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A material for controlling impurity ions in epoxy resin, characterized in that, The material is composed of microcapsules, which include a resin core and... Shell, and the resin core and At least a portion between the shell layers is filled with an ionic liquid layer, and the resin core comprises a cation exchange resin and an anion exchange resin.
2. The material for controlling impurity ions in epoxy resin according to claim 1, characterized in that, The ionic liquid is selected from imidazole or quaternary ammonium salt ionic liquids.
3. The material for controlling impurity ions in epoxy resin according to claim 1, characterized in that, The cation exchange resin is a sulfonic acid group-containing resin. Strongly acidic cation exchange resins, including type 732 cation exchange resin, are used in adsorption systems. , cationic impurities; Anion exchange resins are strongly basic anion exchange resins containing quaternary ammonium groups. Strongly basic anion exchange resins include type 717 anion exchange resins, used in adsorption systems. Anionic impurities.
4. The material for controlling impurity ions in epoxy resin according to claim 1, characterized in that, The The shell is a shell whose surface has been treated with a silane coupling agent.
5. The material for controlling impurity ions in epoxy resin according to claim 1, characterized in that, The microcapsules have a particle size of 1-20 μm.
6. The material for controlling impurity ions in epoxy resin according to claim 1, characterized in that, The resin core has a mass of 10 parts, and the ionic liquid layer has a mass of 0.5 to 1 part. The mass of the shell is 4-8 parts; The mass ratio of cation exchange resin to anion exchange resin in the resin core is 1:2 to 1:
1.
7. The method for preparing a material for controlling impurity ions in epoxy resin according to any one of claims 1 to 6, characterized in that, Includes the following steps: Step S1: Preparation of resin micro powder: Cation exchange resin and anion exchange resin are pulverized to a particle size of 1-10 μm to obtain micro powder; Step S2: Ionic liquid composite treatment, dissolving the ionic liquid in a mixed solvent of water and ethanol; adding resin micro powder to the solution; stirring to coat the resin surface with the ionic liquid; obtaining ionic liquid modified resin composite particles; Step S3: Dispersion and emulsification: The composite particles are added to the aqueous phase containing the dispersant and sheared to disperse them, forming a stable suspension system; Step S4: Shell Construction: A silicon source is added to the system, and a sol-gel reaction is carried out under alkaline conditions to form a shell. Shell; Step S5: Surface modification: The shell surface is modified with a silane coupling agent to improve compatibility with epoxy resin. Step S6: Post-processing: Separate, wash and dry to obtain microcapsules.
8. The method for preparing the epoxy resin impurity ion control material according to claim 7, characterized in that, In step S1: ion exchange resin pretreatment, take cation exchange resin and anion exchange resin respectively, wash them multiple times with deionized water to remove soluble impurities on the surface; then wash them multiple times with anhydrous ethanol to remove organic residues. Then, the washed ion exchange resin is dried in a vacuum drying oven for later use; pulverization and grinding: the dried ion exchange resin is added to a planetary ball mill for pulverization; after ball milling, the sample is sieved and the particle size distribution is detected by a laser particle size analyzer so that the overall particle size of the resin powder D50 is controlled within 1-10μm. In step S2: Prepare the ionic liquid solution: Weigh the ionic liquid and add it to a mixed solvent composed of anhydrous ethanol and deionized water. Stir magnetically at room temperature to form a uniform and transparent solution. Weigh the ion exchange resin powder obtained in step S1 and slowly add it to the above ionic liquid solution. Composite adsorption treatment: First, premix by magnetic stirring, then disperse by ultrasonication; then continue mechanical stirring; during this process, the ionic liquid gradually adsorbs, wets and partially impregnates the surface and pore structure of the ion exchange resin particles, thereby obtaining ion liquid modified resin composite particles. Solid-liquid separation: The resulting suspension is centrifuged and the supernatant is discarded. Then, it is quickly washed with a small amount of ethanol to remove the unadsorbed free ionic liquid. Drying: The precipitate was dried in a vacuum environment to obtain ionic liquid modified resin composite particles; In step S3: Dispersion and emulsification: Preparation of the dispersion aqueous phase: Take deionized water, add polyvinyl alcohol (PVA), stir and dissolve at 80°C to prepare a PVA aqueous solution; cool to room temperature for later use; Add composite particles: Slowly add the ionic liquid modified resin composite particles obtained in step S2 to the above PVA aqueous solution; Shear dispersion: Use a shear emulsifier for dispersion treatment; Shear while adding material, and maintain the system temperature not exceeding 35°C during the shearing process; Formation of a suspension system: After the treatment, a stable suspension system with uniform dispersion and no obvious sedimentation is obtained; In step S4: Shell construction: The reaction system is established by adding anhydrous ethanol to the suspension system obtained in step S3 to improve the dispersion and hydrolysis conditions of tetraethyl orthosilicate (TEOS) in the system. The mixture was then stirred at room temperature. The pH was adjusted by slowly adding ammonia dropwise to the system until it reached 9.5-10.
5. Tetraethyl orthosilicate (TEOS), a silicon source, was added. TEOS was pre-diluted with anhydrous ethanol and slowly added dropwise to the system while stirring, with the addition time controlled at 20-30 minutes. Sol-gel coating reaction: After the TEOS was added, the reaction was continued with stirring. Under alkaline conditions, TEOS underwent hydrolysis and condensation reactions, gradually depositing on the surface of the composite particles and forming a continuous... Shell; In step S5: Surface modification: Modifier is added, and silane coupling agent KH560 is added to the system after the reaction in step S4, and the reaction is continued with stirring; KH560 and The hydroxyl groups on the shell surface undergo a condensation reaction and form an organosilane modified layer on the particle surface, thereby improving its interfacial compatibility in epoxy resin. In step S6: Post-processing: The system after the reaction in step S5 is centrifuged; Washing: Washed sequentially with deionized water and anhydrous ethanol; Centrifuged after each washing to remove unreacted silicon source, ammonia and free coupling agent. Drying: Place the washed microcapsules in a vacuum drying oven to dry; After drying, grind or lightly sieve to break up soft agglomerated particles and obtain microcapsule powder with better flowability; Finished product: The final product is a light white or pale yellow microcapsule powder, which is the functional material used for regulating impurity ions in epoxy resin.
9. A method for controlling impurity ions in epoxy resin, characterized in that, Includes the following steps: Step 1: Preparation of epoxy resin matrix: Select an epoxy system, place it in a mixing container, preheat it to reduce its viscosity, and facilitate subsequent dispersion; Step 2: Microcapsule addition, adding the microcapsules according to any one of claims 1-6 to the epoxy resin; Step 3: Pre-dispersion treatment: mechanical stirring; Step 4: Degassing treatment. The mixture is placed in a vacuum environment to degas in order to prevent air bubbles from affecting the insulation performance.
10. The method for controlling impurity ions in epoxy resin according to claim 9, characterized in that, In step 1, preheat at 40-60℃; in step 3, mechanical stirring speed: 500-1000 rpm, time: 15-30 min; in step 4, vacuum degree: –0.08 MPa, time: 10-20 min.