Disposable isolation plug with long-acting anti-aging performance and preparation process of disposable isolation plug

By synergistically constructing a silicon-oxygen hybrid compound, silicon-shelled triazine microspheres, and epoxy amine-cured flexible particles, the problem of flexibility and stability of disposable isolation plugs in complex environments is solved, achieving the maintenance of sealing performance and mechanical stability during long-term use, making it suitable for sealing applications in complex environments.

CN121699301APending Publication Date: 2026-03-20RUIJIA YIXING TECH
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Patent Information

Application Number
CN202610038068.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-01-13
Publication Date
2026-03-20

AI Technical Summary

Technical Problem

Existing disposable isolation plugs are prone to material chain loosening or breakage under long-term thermo-oxidative aging, ultraviolet irradiation or continuous compression, resulting in insufficient interfacial bonding strength, high compression set and reduced dimensional retention. Furthermore, they are prone to swelling, softening or volume changes in oil, water or composite chemical media, causing fluctuations in mechanical properties and making it difficult to balance flexibility and stability.

Method used

A multi-scale structure is formed by the synergistic construction of silicon-oxygen hybrid composites, silicon-shell triazine microspheres, and epoxy amine-cured flexible particles. The stress is dispersed through organic flexible segments, Si-O-Si three-dimensional network, and core-shell structure. Combined with the flexible epoxy-amine-cured particles providing a buffer rebound path, a dense and impermeable structure is formed, which improves the aging resistance and solvent resistance of the material.

Benefits of technology

It maintains stable rebound capability under macroscopic compression deformation, significantly reduces compression set, ensures that the isolation plug maintains sealing and mechanical stability in complex environments, resists liquid medium erosion and ultraviolet aging, and meets the needs of outdoor and complex environments.

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Abstract

The invention discloses a disposable isolation plug with long-acting aging resistance and a preparation process thereof, belongs to the technical field of isolation material preparation, and aims to solve the technical problem that the aging resistance and solvent resistance of a disposable isolation plug in the prior art need to be further improved. According to the invention, a silicon-oxygen hybrid triazine compound is adopted as a matrix, the silicon-oxygen hybrid compound is introduced to construct a stable spatial network, and silicon shell triazine microspheres and epoxy amine cured flexible particles are assisted to jointly adjust the interface structure and chain segment motion characteristics of the material; the obtained disposable isolation plug forms a structural system with balanced support and recoverable deformation capability, and all the components form a continuous and stable mechanical response path in the system, so that the material shows low compression permanent deformation rate and good size retentivity under the conditions of normal temperature, high temperature, soaking and aging.
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Description

Technical Field

[0001] This invention relates to the field of isolation material preparation technology, specifically to a disposable isolation plug with long-lasting aging resistance and its preparation process. Background Technology

[0002] Disposable isolation plugs are used in oil and gas well operations and chemical media barrier applications, where they are subjected to complex environments such as temperature fluctuations, mechanical compression, and ultraviolet radiation for extended periods. Therefore, aging resistance has become an important direction for the development of their materials. To mitigate structural relaxation and chain segment breakage caused by ultraviolet radiation, heat and oxygen, and mechanical stress, isolation plug materials have evolved from single organic elastomers to multi-component composite systems. By adjusting the chain segment structure, interface morphology, and filler characteristics, the structural stability and deformation recovery ability during long-term use can be improved. At the same time, oil, water, and various chemical media in the downhole environment can cause swelling, volume changes, or interface damage, making solvent resistance another key technical indicator. Recent research has gradually reduced the material's sensitivity to solvents by increasing the degree of chemical crosslinking, optimizing the interface structure, and using stable phase fillers, thereby maintaining the dimensional stability and mechanical reliability of the isolation plug under the action of complex media.

[0003] Currently, the preparation of disposable isolation plugs mostly relies on the modification of single elastomers or conventional fillers to improve performance. However, under long-term thermo-oxidative aging, ultraviolet irradiation, or continuous compression, the material chain segments are prone to loosening or breakage, resulting in insufficient interfacial bonding strength, leading to high compression set and decreased dimensional retention. In addition, inorganic components often have limited dispersion in traditional processes, and the interfacial transition region is discontinuous, making the material prone to stress concentration under high temperature and stress, resulting in unstable structural response. At the same time, due to the limited crosslinking density and simple structural hierarchy of conventional systems, isolation plugs are prone to swelling, softening, or volume changes in oil, water, or complex chemical media, resulting in fluctuations in mechanical properties. On the other hand, simply increasing the crosslinking density to improve solvent resistance can easily lead to brittleness of the material, making it difficult to balance flexibility and stability, resulting in insufficient overall performance matching.

[0004] To address this technical deficiency, a solution is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide a disposable isolation plug with long-lasting aging resistance and its preparation process, in order to solve the technical problem that the aging resistance and solvent resistance of disposable isolation plugs in the prior art need to be further improved.

[0006] The objective of this invention can be achieved through the following technical solution: a disposable isolation plug with long-lasting aging resistance, comprising the following raw material components by weight: 80-100 parts of silicon-oxygen hybrid composite, 15-20 parts of silicon-shell triazine microspheres, 20-30 parts of epoxy amine cured flexible particles and 0.4-0.6 parts of 2,6-di-tert-butyl-p-cresol;

[0007] The silicon-oxygen hybrid triazine complex was prepared by the following method:

[0008] A1. Add epoxy grafted copolymer elastomer, 1,3,5-tris(2-hydroxyethyl)isocyanuric acid and toluene to the reactor. Heat the reactor to 70-90℃ and stir until the materials are mixed evenly. Then add p-benzenesulfonic acid and heat the reactor to 80-100℃. Keep it warm and stir for 2-4 hours. The post-treatment yields trihydroxyisocyanate modified prepolymer.

[0009] A2. Add the triazine-reinforced epoxy prepolymer to the reactor, heat the reactor to 60-80℃, add 3-isocyanate-propyltrimethoxysilane and dibutyltin dilaurate, keep the mixture warm and stir for 1-2 hours, then cool the reactor to 50-60℃ and add the modification solution, continue to keep the mixture warm and stir for 2-4 hours, and then obtain the silicon-oxygen hybrid composite.

[0010] The reaction principle for preparing silicon-oxygen hybrid triazine complexes is as follows:

[0011] First, the epoxy side chains in the epoxy graft copolymer elastomer undergo ring-opening grafting with 1,3,5-tris(2-hydroxyethyl)isocyanuric acid under acidic conditions, allowing the triazine structure to be stably embedded in the flexible backbone in the form of multiple hydroxyl groups, thereby obtaining an enhanced prepolymer with triazine backbone characteristics. Subsequently, silane molecules with isocyanate and alkoxysilane bifunctional groups are introduced under mild conditions. The isocyanate groups can selectively form stable polyurethane bonds with the residual hydroxyl groups of the prepolymer, while the alkoxy groups at the silane end undergo further condensation under hydrolysis conditions, constructing a local Si-O-Si cross-linked network. This enables the organic chain segments, triazine structural units, and inorganic silicon-oxygen networks to achieve synergistic integration at the molecular scale, forming a hybrid composite system with flexibility, thermal stability, and structural regularity, resulting in a silicon-oxygen hybrid triazine complex.

[0012] Further, in step A1, the ratio of the epoxy grafted copolymer elastomer, 1,3,5-tris(2-hydroxyethyl)isocyanuric acid, p-benzenesulfonic acid, and toluene is 25g:5-8g:40-60mL:0.2-0.3g. The post-treatment includes: after the reaction is completed, the reaction system is adjusted to be neutral using a 1wt% sodium bicarbonate aqueous solution, the temperature of the reactor is controlled at 80℃ and vacuum degassed for 1-2 hours, and after natural cooling, the trihydroxyisocyanate modified prepolymer is obtained.

[0013] Further, in step A2, the ratio of the triazine-reinforced epoxy prepolymer, 3-isocyanate-propyltrimethoxysilane, dibutyltin dilaurate, and the modifying solution is 25g:4-6mL:0.1-0.2g:20-24mL. The modifying solution is obtained by mixing anhydrous ethanol, deionized water, and acetic acid in a ratio of 10-12mL:10-12mL:0.2mL. The post-treatment includes: after the reaction is completed, the temperature of the reaction vessel is controlled at 60℃ and vacuum degassing is performed for 1-2 hours. After natural cooling, a silicon-oxygen hybrid composite is obtained.

[0014] Furthermore, the preparation method of the epoxy grafted copolymer elastomer is as follows: isobutylene is introduced into a low-temperature reactor containing allyl glycidyl ether and anhydrous n-hexane. After the introduction is completed, the reactor is cooled to -65°C, boron trifluoride diethyl ether is added, and the mixture is kept warm and stirred for 1-2 hours. After stirring is completed, methanol is added. After the reactor is restored to room temperature and pressure, the epoxy grafted copolymer elastomer is obtained through post-treatment.

[0015] The reaction principle for preparing epoxy graft copolymer elastomers is as follows:

[0016] Under strong Lewis acid conditions, boron trifluoride ether can activate isobutylene monomers, causing them to generate continuously growing positively charged end groups, thereby initiating chain polymerization. At the same time, the allyl glycidyl ether present in the system can have its epoxy structure opened in a cationic environment or participate in chain growth in the form of allyl groups, so that epoxy-containing side chains are introduced onto the isobutylene backbone. Through this parallel mechanism of "continuous backbone growth + monomer lateral grafting", the polymer can combine the flexibility of isobutylene with the reactivity of epoxy groups, forming an epoxy grafted copolymer elastomer with specific structural controllability and potential for subsequent chemical modification.

[0017] Furthermore, the ratio of isobutylene, allyl glycidyl ether, anhydrous n-hexane, boron trifluoride ethyl ether, and methanol is 1200mL:12-18mL:100mL:0.1-0.2mL:3mL. The post-treatment includes: pressure distillation until no liquid is collected, then transferring the material to a drying oven at 60°C and vacuum drying for 1-2 hours to obtain an epoxy graft copolymer elastomer.

[0018] Furthermore, the silica-shelled triazine microspheres are prepared by the following method:

[0019] B1. After adding deionized water and polyvinyl alcohol to the reaction vessel and stirring evenly, add oil phase liquid and heat the reaction vessel to 50-70℃, keep it at the temperature for 2-4 hours, and then obtain triazine mercaptoether crosslinked microspheres.

[0020] B2. Triazine mercaptoether crosslinked microspheres, anhydrous ethanol and deionized water were added to the reaction vessel and stirred until they were evenly dispersed. Then, 3-(2,3-epoxypropoxy)propyltrimethoxysilane and acetic acid were added to the reaction vessel. The reaction vessel was then heated to 40-60℃ and stirred for 3-5 hours. The resulting product was a silicon-shelled triazine microsphere.

[0021] The reaction principle for preparing silica-shelled triazine microspheres is as follows:

[0022] In the microemulsion system, a thiol-containing pentaerythritol derivative and a triazine monomer containing polyene bonds undergo free radical cross-linking under photoinitiation conditions. This allows the triazine skeleton to be uniformly embedded in a high-density thiol ether network, forming a core of organic microspheres with controllable size and stable structure. Subsequently, silane molecules with dual epoxy and alkoxy silane functions are introduced. Their epoxy end groups can undergo interfacial ring-opening reactions with residual thiol or hydroxyl groups on the microsphere surface, allowing the silane molecules to be firmly anchored to the particle surface. Under acidic conditions, their alkoxy groups undergo further hydrolysis and condensation, gradually constructing a continuous Si-O-Si network shell around the microsphere. Through the synergistic assembly of the "organic cross-linked core + inorganic silicon-oxygen shell", the microspheres simultaneously possess the stability of the triazine structure and the heat resistance and interfacial adhesion of the silicon-oxygen network, thus forming silicon-shell triazine microspheres with core-shell characteristics.

[0023] Further, in step B1, the ratio of deionized water, polyvinyl alcohol, and oil phase is 300mL:2-3g:180g. The oil phase is obtained by mixing pentaerythritol tetra(3-mercaptopropionate), tri-2-acrylate [2,4,6-trioxo-1,3,5-triazine-1,3,5(2H,4H,6H)-trimethyl]tri-2,1-ethylene ester, and 2-hydroxy-2-methyl-1-phenyl-1-propanone in a ratio of 100-120g:90g:2g. The post-treatment includes: after the reaction is completed, the filter cake is collected by vacuum filtration, washed with deionized water 3-5 times, and then the filter cake is transferred to a drying oven at 60℃ and vacuum dried for 5h to obtain triazine mercaptoether crosslinked microspheres.

[0024] Further, in step B2, the ratio of the triazine mercaptoether crosslinked microspheres, anhydrous ethanol, deionized water, 3-(2,3-epoxypropoxy)propyltrimethoxysilane, and acetic acid is 100g:150mL:40-50mL:12-15mL:0.3mL. The post-treatment includes: after the reaction is completed, the filter cake is collected by vacuum filtration, washed with deionized water 3-5 times, and then the filter cake is transferred to a drying oven at 60℃ and vacuum dried for 5 hours to obtain silicon-shelled triazine microspheres.

[0025] Furthermore, the epoxy amine-cured flexible particles are prepared by the following method:

[0026] C1. Add adipic acid, neopentyl glycol, p-toluenesulfonic acid and 2,6-di-tert-butyl-p-cresol to a reactor. Under nitrogen protection, heat the reactor to 180-200℃, keep it at this temperature and stir. Reduce the pressure to 40 kPa within 15-20 min, then reduce the pressure to 10 kPa within 15-30 min. Continue to react at constant temperature and pressure for 1-2 h. Cool down and discharge to obtain adipic acid-neopentyl glycol polyester diol.

[0027] C2. Add adipic acid-neopentyl glycol polyester diol to the reactor and heat the reactor to 60-70℃. Then add polyetheramine and bisphenol A epoxy resin and heat the reaction to 80-100℃. Keep the temperature and stir for 2-4 hours. After post-treatment, epoxy amine cured flexible particles are obtained.

[0028] The reaction principle for preparing epoxy amine-cured flexible particles is as follows:

[0029] First, adipic acid and neopentyl glycol undergo a polycondensation reaction under acid catalysis, and linear polyester glycol is generated through esterification between carboxyl and hydroxyl groups, forming a polymer matrix with certain chain segment flexibility. Subsequently, under heating conditions, polyester glycol and polyetheramine are introduced into a bisphenol A type resin system containing epoxy structure. The epoxy groups undergo a ring-opening reaction under the action of amine groups, forming a stable cross-linked network between polyester segments, polyether segments and epoxy resin. This network combines the flexibility of polyester, the toughness adjustment ability of polyether segments and the strength and stability of epoxy-amine cured structure. Through the chemical bonding between the multi-components, the material exhibits a balanced distribution of flexible segments and cross-linking points in its microstructure, thus forming epoxy amine cured flexible particles suitable for subsequent composite systems.

[0030] Furthermore, in step C1, the ratio of adipic acid, neopentyl glycol, p-toluenesulfonic acid, and 2,6-di-tert-butyl-p-cresol is 100g:100-120g:0.5g:0.2g.

[0031] Further, in step C2, the ratio of adipic acid-neopentyl glycol polyester glycol, polyetheramine, and bisphenol A epoxy resin is 120g:60-80g:80-100g. The post-treatment includes: after stirring, casting and curing the mixture and keeping it in a drying oven at 90°C for 3 hours, then cooling it to room temperature and grinding it into particles with a particle size of 0.8mm to obtain epoxy amine cured flexible particles.

[0032] The present invention also discloses a method for preparing a disposable isolation plug with long-lasting aging resistance, comprising the following steps:

[0033] S1. Add the silicon-oxygen hybrid composite, silicon-shell triazine microspheres, epoxy amine-cured flexible particles and 2,6-di-tert-butyl-p-cresol to a mixer, heat the mixer to 100-120℃, and maintain the temperature for 15-20 minutes. After the mixer is completed, let the mixer cool to room temperature, take out the material and process it into a pre-blended material with a particle size of 3-5mm through a granulator.

[0034] S2. Spread the pre-mixed material evenly in the preheated mold cavity. After the mold is closed, treat it at 160-180℃ and 16-20MPa for 15-20 minutes. After hot pressing, cool the mold and the product together to 40-60℃, open the mold and remove the product to obtain a disposable isolation plug.

[0035] The present invention has the following beneficial effects:

[0036] 1. This invention utilizes the synergistic construction of a silicon-oxygen hybrid composite, silicon-shell triazine microspheres, and epoxy amine-cured flexible particles to enable the material to maintain stable resilience under macroscopic compressive deformation. The organic flexible segments in the silicon-oxygen hybrid composite provide reversible elastic deformation space, while the Si-O-Si three-dimensional network acts as a skeletal unit, restricting irreversible displacement of the segments and effectively suppressing permanent damage caused by compressive stress. Simultaneously, the core-shell structured silicon-shell triazine microspheres dispersed throughout the system form a microstructure resembling "point-like reinforcing pillars," which disperses localized stress concentrations and blocks excessive transmission of compressive deformation. Furthermore, the flexible epoxy-amine-cured particles provide a buffer rebound path during deformation recovery, enhancing the material's structural memory under pressure. This multi-scale complementary structure results in a significantly reduced compression set rate in both room temperature and 150°C aging environments, ensuring reliable sealing of the isolation plug during installation and long-term service.

[0037] 2. The isolation plug obtained by this invention has a dense, impermeable structure formed by the interweaving of organic cross-linked chains and inorganic silicon-oxygen networks, which significantly improves its resistance to liquid media. Among them, the silicon-oxygen hybrid complex provides a continuous phase structure, and its high cross-linking density and triazine skeleton endow the material with excellent chemical stability. The Si-O-Si shell of the silicon-shelled triazine microspheres constitutes a local inorganic barrier, which can block the diffusion path of solvents inside the material and reduce the risk of swelling and wetting. At the same time, the epoxy-amine cured flexible particles fill the residual pores in the system and form a secondary cross-linking network, which effectively limits the excessive extension of chain segments under the action of solvents. The three work together to make the material achieve a solvent-resistant system of "corrosion-resistant skeleton + barrier microspheres + buffer flexible chain", so that the isolation plug can maintain dimensional stability and mechanical retention rate even under long-term contact with common oils or processing liquids, and is suitable for sealing applications in complex environments.

[0038] 3. This invention also utilizes the combined effect of the anti-photodegradation properties of the triazine structure and the inorganic shielding ability of the silicon-oxygen network to maintain excellent resilience after UV aging. Specifically, the triazine groups in the silicon-oxygen hybrid composite have the ability to absorb and dissipate energy for UV light, which can effectively delay the photo-oxidative breakage of organic chain segments. The inorganic shell of the silicon-shell triazine microspheres prevents UV light from directly eroding the organic core structure, reducing the depth of damage caused by photoaging. Furthermore, the flexible epoxy-amine cured particles provide energy buffering during deformation recovery after UV-induced micro-damage, maintaining the reversibility of compression deformation. Relying on multi-dimensional synergistic protection, the material can still maintain a low compression set at room temperature and 150°C after UV aging, achieving long-term sealing reliability under the combined effects of high temperature and light, and meeting the safe use requirements of disposable isolation plugs in outdoor and complex environments. Detailed Implementation

[0039] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. 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.

[0040] In this application, the polyvinyl alcohol used was purchased from Shanghai Maclean Biochemical Technology Co., Ltd., with item number 767383; the polyetheramine used was purchased from Shanghai Maclean Biochemical Technology Co., Ltd., with item number P939193; and the bisphenol A type epoxy resin used was purchased from Shandong Qiansheng Chemical Co., Ltd., with brand name E51.

[0041] Example 1

[0042] This embodiment provides a method for preparing a silicon-oxygen hybrid triazine complex, including the following steps:

[0043] Step ①: Preparation of epoxy grafted copolymer elastomer

[0044] Weigh 1200.0 mL of isobutylene and introduce it into a low-temperature reactor containing 12.0 mL of allyl glycidyl ether and 100.0 mL of anhydrous n-hexane. After the introduction is complete, cool the reactor to -65°C and add 0.1 mL of boron trifluoride ether. Keep the reactor warm and stir for 1 hour. After stirring, add 3.0 mL of methanol. After the reactor returns to room temperature and pressure, reduce the pressure and distill until no liquid is collected. Transfer the material to a drying oven at 60°C and vacuum dry for 1 hour to obtain epoxy graft copolymer elastomer.

[0045] Step ②: Preparation of trihydroxyisocyanate modified prepolymer

[0046] 25.0 g of epoxy grafted copolymer elastomer, 5.0 g of 1,3,5-tris(2-hydroxyethyl) isocyanuric acid, and 40.0 mL of toluene were added to the reactor. The reactor was heated to 70 °C and stirred until the materials were mixed evenly. Then, 0.2 g of p-benzenesulfonic acid was added and the reactor was heated to 80 °C. The mixture was kept at this temperature and stirred for 2 h. After the reaction was completed, the reaction system was adjusted to neutrality using a 1 wt% sodium bicarbonate aqueous solution. The reactor temperature was then controlled at 80 °C and degassed under vacuum for 1 h. After natural cooling, the trihydroxyisocyanate modified prepolymer was obtained.

[0047] Step ③: Preparation of silicon-oxygen hybrid complex

[0048] Weigh out 10.0 mL of anhydrous ethanol, 10.0 mL of deionized water and 0.2 mL of acetic acid and mix them to obtain the modified solution;

[0049] Weigh 25.0g of triazine-reinforced epoxy prepolymer and add it to the reactor. After heating the reactor to 60℃, add 4.0mL of 3-isocyanate-propyltrimethoxysilane and 0.1g of dibutyltin dilaurate. After stirring for 1h, cool the reactor to 50℃ and add 20.0mL of the modification solution. Continue stirring for 2h. After the reaction is complete, control the reactor temperature to 60℃ and degas under vacuum for 1h. After natural cooling, the silicon-oxygen hybrid composite is obtained.

[0050] Example 2

[0051] This embodiment provides a method for preparing a silicon-oxygen hybrid triazine complex, including the following steps:

[0052] Step ①: Preparation of epoxy grafted copolymer elastomer

[0053] Weigh 1200.0 mL of isobutylene and introduce it into a low-temperature reactor containing 18.0 mL of allyl glycidyl ether and 100.0 mL of anhydrous n-hexane. After the introduction is complete, cool the reactor to -65°C and add 0.2 mL of boron trifluoride ether. Keep the reactor warm and stir for 2 hours. After stirring, add 3.0 mL of methanol. After the reactor returns to room temperature and pressure, reduce the pressure and distill until no liquid is collected. Transfer the material to a drying oven at 60°C and vacuum dry for 2 hours to obtain epoxy graft copolymer elastomer.

[0054] Step ②: Preparation of trihydroxyisocyanate modified prepolymer

[0055] 25.0 g of epoxy grafted copolymer elastomer, 8.0 g of 1,3,5-tris(2-hydroxyethyl) isocyanuric acid, and 60.0 mL of toluene were added to the reactor. The reactor was heated to 90 °C and stirred until the materials were mixed evenly. Then, 0.3 g of p-benzenesulfonic acid was added and the reactor was heated to 100 °C. The mixture was kept at this temperature and stirred for 4 h. After the reaction was completed, the reaction system was adjusted to neutrality using a 1 wt% sodium bicarbonate aqueous solution. The reactor temperature was then controlled at 80 °C and degassed under vacuum for 2 h. After natural cooling, the trihydroxyisocyanate modified prepolymer was obtained.

[0056] Step ③: Preparation of silicon-oxygen hybrid complex

[0057] Weigh out 12.0 mL of anhydrous ethanol, 12.0 mL of deionized water, and 0.2 mL of acetic acid, mix them, and obtain the modified solution.

[0058] Weigh 25.0g of triazine-reinforced epoxy prepolymer and add it to a reactor. After heating the reactor to 80℃, add 6.0mL of 3-isocyanate-propyltrimethoxysilane and 0.2g of dibutyltin dilaurate. Keep the reactor heated and stirred for 2h. Then, cool the reactor to 60℃ and add 24.0mL of the modified solution. Continue to keep the reactor heated and stirred for 4h. After the reaction is complete, control the reactor temperature at 60℃ and degas under vacuum for 2h. After natural cooling, the silicon-oxygen hybrid composite is obtained.

[0059] Example 3

[0060] This embodiment provides a method for preparing a silicon-oxygen hybrid triazine complex, including the following steps:

[0061] Step ①: Preparation of epoxy grafted copolymer elastomer

[0062] Weigh 1200.0 mL of isobutylene and introduce it into a low-temperature reactor containing 16.0 mL of allyl glycidyl ether and 100.0 mL of anhydrous n-hexane. After the introduction is complete, cool the reactor to -65°C and add 0.2 mL of boron trifluoride diethyl ether. Keep the reactor warm and stir for 2 hours. After stirring, add 3.0 mL of methanol. After the reactor returns to room temperature and pressure, reduce the pressure and distill until no liquid is collected. Transfer the material to a drying oven at 60°C and vacuum dry for 2 hours to obtain epoxy graft copolymer elastomer.

[0063] Step ②: Preparation of trihydroxyisocyanate modified prepolymer

[0064] 25.0 g of epoxy graft copolymer elastomer, 7.0 g of 1,3,5-tris(2-hydroxyethyl) isocyanuric acid and 50.0 mL of toluene were added to the reactor. The reactor was heated to 80 °C and stirred until the materials were mixed evenly. Then, 0.3 g of p-benzenesulfonic acid was added and the reactor was heated to 90 °C. The mixture was kept at this temperature and stirred for 3 h. After the reaction was completed, the reaction system was adjusted to neutrality using a 1 wt% sodium bicarbonate aqueous solution. The reactor temperature was then controlled at 80 °C and degassed under vacuum for 2 h. After natural cooling, the trihydroxyisocyanate modified prepolymer was obtained.

[0065] Step ③: Preparation of silicon-oxygen hybrid complex

[0066] Weigh out 12.0 mL of anhydrous ethanol, 12.0 mL of deionized water, and 0.2 mL of acetic acid, mix them, and obtain the modified solution.

[0067] Weigh 25.0g of triazine-reinforced epoxy prepolymer and add it to the reactor. After heating the reactor to 70℃, add 5.0mL of 3-isocyanate-propyltrimethoxysilane and 0.2g of dibutyltin dilaurate. After stirring for 2h, cool the reactor to 60℃ and add 20.0mL of the modification solution. Continue stirring for 3h. After the reaction is complete, control the reactor temperature at 60℃ and degas under vacuum for 2h. After natural cooling, the silicon-oxygen hybrid composite is obtained.

[0068] Example 4

[0069] This embodiment provides a method for preparing silicon-shelled triazine microspheres, including the following steps:

[0070] Step 1: Preparation of triazine thioether cross-linked microspheres

[0071] Weigh out 100.0 g pentaerythritol tetra(3-mercaptopropionate), 90.0 g tri-2-acrylate [2,4,6-trioxo-1,3,5-triazine-1,3,5(2H,4H,6H)-trimethyl]tri-2,1-ethylene ester and 2.0 g 2-hydroxy-2-methyl-1-phenyl-1-propanone and mix them to obtain an oil phase liquid;

[0072] Add 300.0 mL of deionized water and 2.0 g of polyvinyl alcohol to the reaction vessel and stir until homogeneous. Then add 180.0 g of oil phase liquid and heat the reaction vessel to 50 °C. Keep the temperature for 2 h. After the reaction is complete, filter the filter cake and wash it three times with deionized water. Transfer the filter cake to a drying oven at 60 °C and vacuum dry for 5 h to obtain triazine mercaptoether crosslinked microspheres.

[0073] Step 2: Preparation of silica-shelled triazine microspheres

[0074] Weigh 100.0g of triazine mercaptoether crosslinked microspheres, 150.0mL of anhydrous ethanol and 40.0mL of deionized water and add them to the reaction vessel. Stir until the mixture is evenly dispersed. Then add 12.0mL of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 0.3mL of acetic acid to the reaction vessel. Heat the reaction vessel to 40℃ and stir for 3h. After the reaction is complete, filter the filter cake and wash it 3 times with deionized water. Transfer the filter cake to a drying oven at 60℃ and vacuum dry for 5h to obtain silicon-shelled triazine microspheres.

[0075] Example 5

[0076] This embodiment provides a method for preparing silicon-shelled triazine microspheres, including the following steps:

[0077] Step 1: Preparation of triazine thioether cross-linked microspheres

[0078] Weigh out 120.0 g pentaerythritol tetra(3-mercaptopropionate), 90.0 g tri-2-acrylate [2,4,6-trioxo-1,3,5-triazine-1,3,5(2H,4H,6H)-trimethyl]tri-2,1-ethylene ester and 2.0 g 2-hydroxy-2-methyl-1-phenyl-1-propanone and mix them to obtain an oil phase liquid;

[0079] 300.0 mL of deionized water and 3.0 g of polyvinyl alcohol were added to the reaction vessel and stirred evenly. Then, 180.0 g of oil phase liquid was added and the reaction vessel was heated to 70 °C and kept at that temperature for 4 h. After the reaction was completed, the filter cake was collected by vacuum filtration. After washing with deionized water 5 times, the filter cake was transferred to a drying oven at 60 °C and vacuum dried for 5 h to obtain triazine mercaptoether crosslinked microspheres.

[0080] Step 2: Preparation of silica-shelled triazine microspheres

[0081] Weigh 100.0g of triazine mercaptoether crosslinked microspheres, 150.0mL of anhydrous ethanol and 50.0mL of deionized water and add them to the reaction vessel. Stir until the mixture is evenly dispersed. Then add 15.0mL of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 0.3mL of acetic acid to the reaction vessel. Heat the reaction vessel to 60℃ and stir for 5h. After the reaction is complete, filter the filter cake and wash it 5 times with deionized water. Transfer the filter cake to a drying oven at 60℃ and vacuum dry for 5h to obtain silicon-shelled triazine microspheres.

[0082] Example 6

[0083] This embodiment provides a method for preparing silicon-shelled triazine microspheres, including the following steps:

[0084] Step 1: Preparation of triazine thioether cross-linked microspheres

[0085] Weigh out 100.0 g pentaerythritol tetra(3-mercaptopropionate), 90.0 g tri-2-acrylate [2,4,6-trioxo-1,3,5-triazine-1,3,5(2H,4H,6H)-trimethyl]tri-2,1-ethylene ester and 2.0 g 2-hydroxy-2-methyl-1-phenyl-1-propanone and mix them to obtain an oil phase liquid;

[0086] 300.0 mL of deionized water and 3.0 g of polyvinyl alcohol were added to the reaction vessel and stirred evenly. Then, 180.0 g of oil phase liquid was added and the reaction vessel was heated to 60 °C and kept at that temperature for 3 h. After the reaction was completed, the filter cake was collected by vacuum filtration. After washing with deionized water 4 times, the filter cake was transferred to a drying oven at 60 °C and vacuum dried for 5 h to obtain triazine mercaptoether crosslinked microspheres.

[0087] Step 2: Preparation of silica-shelled triazine microspheres

[0088] Weigh 100.0g of triazine mercaptoether crosslinked microspheres, 150.0mL of anhydrous ethanol and 45.0mL of deionized water and add them to the reaction vessel. Stir until the mixture is evenly dispersed. Then add 13.5mL of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 0.3mL of acetic acid to the reaction vessel. Heat the reaction vessel to 50℃ and stir for 4 hours. After the reaction is complete, filter the filter cake and wash it 4 times with deionized water. Transfer the filter cake to a drying oven at 60℃ and vacuum dry for 5 hours to obtain silicon-shelled triazine microspheres.

[0089] Example 7

[0090] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0091] Step I: Preparation of adipic acid-neopentyl glycol polyester diol

[0092] Weigh out 100.0g adipic acid, 100.0g neopentyl glycol, 0.5g p-toluenesulfonic acid and 0.2g 2,6-di-tert-butyl-p-cresol and add them to the reactor. Under nitrogen protection, heat the reactor to 180℃, keep it at the temperature and stir. Reduce the pressure to 40kPa within 15min, then reduce the pressure to 10kPa within another 15min. Then, react at a constant temperature and pressure for 1h. Cool down and discharge to obtain adipic acid-neopentyl glycol polyester diol.

[0093] Step II: Preparation of epoxyamine-cured flexible particles

[0094] Weigh out 120.0g of adipic acid-neopentyl glycol polyester glycol and add it to the reactor. After heating the reactor to 60℃, add 60.0g of polyetheramine and 80.0g of bisphenol A epoxy resin. Then heat the reaction to 80℃ and stir for 2 hours. After stirring, cast the mixture into a solidified container and keep it in a drying oven at 90℃ for 3 hours. After cooling to room temperature, grind it into particles with a particle size of 0.8mm to obtain epoxy amine-cured flexible particles.

[0095] Example 8

[0096] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0097] Step I: Preparation of adipic acid-neopentyl glycol polyester diol

[0098] Weigh out 100.0g adipic acid, 120.0g neopentyl glycol, 0.5g p-toluenesulfonic acid and 0.2g 2,6-di-tert-butyl-p-cresol and add them to the reactor. Under nitrogen protection, heat the reactor to 200℃, keep it at this temperature and stir. Reduce the pressure to 40kPa within 20min, then reduce it to 10kPa within 30min. Continue to react at constant temperature and pressure for 2h. Cool down and discharge to obtain adipic acid-neopentyl glycol polyester glycol.

[0099] Step II: Preparation of epoxyamine-cured flexible particles

[0100] Weigh out 120.0g of adipic acid-neopentyl glycol polyester glycol and add it to the reactor. After heating the reactor to 70℃, add 80.0g of polyetheramine and 100.0g of bisphenol A epoxy resin. Then heat the reaction to 100℃ and stir for 4 hours. After stirring, cast the mixture into a solidified container and keep it in a drying oven at 90℃ for 3 hours. After cooling to room temperature, grind it into particles with a particle size of 0.8mm to obtain epoxy amine cured flexible particles.

[0101] Example 9

[0102] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0103] Step I: Preparation of adipic acid-neopentyl glycol polyester diol

[0104] Weigh out 100.0g adipic acid, 120.0g neopentyl glycol, 0.5g p-toluenesulfonic acid and 0.2g 2,6-di-tert-butyl-p-cresol and add them to the reactor. Under nitrogen protection, heat the reactor to 190℃, keep it at this temperature and stir. Reduce the pressure to 40kPa within 20min, then reduce it to 10kPa within another 20min. Continue to react at constant temperature and pressure for 2h. Cool down and discharge to obtain adipic acid-neopentyl glycol polyester glycol.

[0105] Step II: Preparation of epoxyamine-cured flexible particles

[0106] Weigh out 120.0g of adipic acid-neopentyl glycol polyester glycol and add it to the reactor. After heating the reactor to 65℃, add 70.0g of polyetheramine and 90.0g of bisphenol A epoxy resin. Then heat the reaction to 90℃ and stir for 3 hours. After stirring, cast the mixture into a solidified container and keep it in a drying oven at 90℃ for 3 hours. After cooling to room temperature, grind it into particles with a particle size of 0.8mm to obtain epoxy amine-cured flexible particles.

[0107] Example 10

[0108] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0109] Step 1: Preparation of pre-blended material

[0110] Weigh out the following by weight: 80 parts of the silicon-oxygen hybrid composite prepared in Example 1, 15 parts of the silicon-shell triazine microspheres prepared in Example 4, 20 parts of the epoxy amine-cured flexible particles prepared in Example 7, and 0.4 parts of 2,6-di-tert-butyl-p-cresol. Add them to a mixer, heat the mixer to 100°C, and maintain the temperature for 15 minutes. After the mixer is completed, let it cool to room temperature, then remove the material and process it into a pre-blended material with a particle size of 3 mm using a granulator.

[0111] Step 2: Prepare disposable isolation plugs

[0112] The pre-blended material is evenly spread in the preheated mold cavity. After the mold is closed, it is treated at 160℃ and 16MPa for 15 minutes. After hot pressing, the mold and the product are cooled to 40℃, the mold is opened and the product is removed to obtain a disposable isolation plug.

[0113] Example 11

[0114] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0115] Step 1: Preparation of pre-blended material

[0116] Weigh out the following by weight: 100 parts of the silicon-oxygen hybrid composite prepared in Example 2, 20 parts of the silicon-shell triazine microspheres prepared in Example 4, 30 parts of the epoxy amine-cured flexible particles prepared in Example 8, and 0.6 parts of 2,6-di-tert-butyl-p-cresol. Add them to a mixer, heat the mixer to 120°C, and maintain the temperature for 20 minutes. After the mixer is completed, let it cool to room temperature, then remove the material and process it into a pre-blended material with a particle size of 5 mm using a granulator.

[0117] Step 2: Prepare disposable isolation plugs

[0118] The pre-blended material is evenly spread in the preheated mold cavity. After the mold is closed, it is treated at 180℃ and 20MPa for 20 minutes. After hot pressing, the mold and the product are cooled to 60℃, the mold is opened and the product is removed to obtain a disposable isolation plug.

[0119] Example 12

[0120] This embodiment provides a method for preparing epoxy amine-cured flexible particles, including the following steps:

[0121] Step 1: Preparation of pre-blended material

[0122] Weigh out the following by weight: 90 parts of the silicon-oxygen hybrid composite prepared in Example 3, 18 parts of the silicon-shell triazine microspheres prepared in Example 6, 25 parts of the epoxy amine-cured flexible particles prepared in Example 9, and 0.5 parts of 2,6-di-tert-butyl-p-cresol. Add them to a mixer, heat the mixer to 120°C, and maintain the temperature for 20 minutes. After the mixer is completed, let it cool to room temperature, then remove the material and process it into a pre-blended material with a particle size of 4 mm using a granulator.

[0123] Step 2: Prepare disposable isolation plugs

[0124] The pre-blended material is evenly spread in the preheated mold cavity. After the mold is closed, it is treated at 170℃ and 180MPa for 18 minutes. After hot pressing, the mold and the product are cooled to 50℃, the mold is opened and the product is removed to obtain a disposable isolation plug.

[0125] Comparative Example 1

[0126] The difference between this comparative example and Example 12 is that step (2) is omitted in the preparation process of the silicon-shelled triazine microspheres used in step one.

[0127] Comparative Example 2

[0128] The difference between this comparative example and Example 12 is that the use of epoxy amine to cure flexible particles is omitted in step one.

[0129] Comparative Example 3

[0130] The difference between this comparative example and Example 12 is that step ③ is omitted in the preparation process of the silicon-oxygen hybrid composite used in step one.

[0131] Performance testing:

[0132] The room temperature compression set and 150°C compression set of the disposable isolation plugs prepared in Examples 10-12 and Comparative Examples 1-3 were determined according to standard GB / T 7759.1-2015 "Determination of compression set of vulcanized rubber or thermoplastic rubber - Part 1: Under normal and high temperature conditions".

[0133] The surface area change rate of disposable isolation plugs prepared in Examples 10-12 and Comparative Examples 1-3 was measured after immersion in liquid 2, in accordance with the standard GB / T 1690-2010 "Test Method for Liquid Resistance of Vulcanized Rubber or Thermoplastic Rubber".

[0134] The compression set at room temperature and compression set at 150°C after UV aging of disposable isolation plugs prepared in Examples 10-12 and Comparative Examples 1-3 were determined according to standard GB / T 3511-2018 "Weather Resistance of Vulcanized Rubber or Thermoplastic Rubber". Specific data are shown in Table 1.

[0135] Table 1 - Performance test data of each sample

[0136] Project Group Example 10 Example 11 Example 12 Comparative Example 1 Comparative Example 2 Comparative Example 3 room temperature compression set / % 18.2 18.0 17.9 19.7 23.4 21.6 Permanent compression set at 150℃ / % 31.6 31.1 30.8 34.9 41.3 38.7 Surface area change rate / % 3.8 3.6 3.5 9.6 4.9 6.1 Compression set at room temperature after aging / % 21.4 21.2 21.1 26.8 29.7 27.4 Permanent compression set at 150℃ after aging / % 35.2 35.0 34.9 42.5 47.8 44.1

[0137] Data Analysis:

[0138] Comparative analysis of the data in Table 1 reveals that the disposable isolation plug prepared by this invention exhibits a room temperature compression set of 18.2%, a 150℃ compression set of 31.6%, a surface area change rate of 3.8%, and an aged room temperature compression set of 21.4%, while the aged 150℃ compression set of 35.2%. All these data are superior to the comparative example, indicating that:

[0139] In Comparative Example 1, the interfacial silane grafting and subsequent hydrolysis-condensation reaction in step (2) were not carried out during the preparation of the silicon-shelled triazine microspheres. As a result, a dense inorganic network structure was not formed on the surface of the microspheres. Without such a stable interfacial barrier, the compatibility between the microspheres and the surrounding organic matrix changed, and the interfacial energy increased significantly. This made the microspheres prone to local debonding or microscale slippage under stress, thereby weakening the structural support of the material during compression deformation. At the same time, the barrier ability of the outer layer of the microspheres to the external environment was reduced, making it more susceptible to interfacial disturbance and structural relaxation under solvent immersion or ultraviolet irradiation. The energy dissipation and stress dispersion capabilities at the microscale decreased accordingly. Under the combined effect, the structural stability of the material under compression rebound, high temperature deformation and aging conditions was affected, resulting in an increase in irreversible residual amount after overall deformation.

[0140] In Comparative Example 2, the system lacks the multi-scale stress adjustment structure introduced by the flexible particles, causing the overall material to enter a deformation mode dominated by a single rigid network during compression and temperature cycling. Due to the lack of chain segments that can absorb stress in local deformation, the matrix is ​​more likely to form irreversible displacement after being compressed. The stress during compression is directly transmitted and accumulated along the main network, making it difficult for the structure to fully recover after unloading. In addition, the micro-relaxation process inside the material is more likely to become unbalanced under thermal effects, and the chain segments move in an irreversible direction in the high-temperature environment, leading to a further increase in high-temperature compression permanent deformation. Under photoaging conditions, the lack of flexible adjustment units also amplifies the cumulative damage caused by micro-cracks and loosening of cross-linking points, resulting in an upward trend in the compression permanent deformation rate at both high and room temperatures after aging.

[0141] In Comparative Example 3, the silicon-oxygen hybrid composite did not undergo the silane grafting and silicon-oxygen network construction process involved in step ③, keeping the main matrix at the pure organic structure level. Consequently, the spatial constraint and structural stability within the network were reduced. Due to the lack of dispersion constraints from inorganic nodes, the chain segments were more prone to cooperative migration under external loads and thermal excitation, resulting in large permanent displacements after compression and making it difficult to achieve effective rebound. At the same time, the diffusion paths and free volume within the material were not suppressed, making it easier for the solvent to induce surface-scale expansion changes under immersion conditions. Furthermore, during UV aging, the pure organic network was more susceptible to energy shocks, leading to microstructural relaxation and chain segment breakage accumulation, which amplified the impact of environmental effects on compression recovery and further reduced the deformation retention capacity after aging.

[0142] In conclusion, the disposable isolation plug prepared by this invention forms a multi-layered structural network composed of trihydroxyisocyanate-modified prepolymer, silicon-oxygen hybrid composite, silicon-shelled triazine microspheres, and epoxy amine-cured flexible particles. Each structural unit is interconnected in terms of chemical composition, interfacial characteristics, and chain segment movement, enabling the material to achieve balanced energy distribution and structural stability adjustment under varying external stress or environmental conditions. Specifically, the silicon-oxygen hybrid structure provides spatial constraints for the overall framework, the surface structure of the microspheres enhances interfacial mechanical continuity, and the flexible particles impart recoverable chain segment activity during local deformation, ensuring good deformation recovery and dimensional stability under compression, high temperature, and aging conditions. Ultimately, through the complementary effects of the multi-scale structures, the resulting isolation plug exhibits stable and reliable performance in compression set tests at room temperature, high temperature, and after aging, demonstrating the sufficiency of the system construction and the overall effectiveness of the material design.

[0143] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A disposable insulating plug with long-lasting aging resistance, characterized in that, The raw material composition includes the following parts by weight: 80-100 parts of silicon-oxygen hybrid composite, 15-20 parts of silicon-shelled triazine microspheres, 20-30 parts of epoxy amine-cured flexible particles and 0.4-0.6 parts of 2,6-di-tert-butyl-p-cresol; The silicon-oxygen hybrid triazine complex was prepared by the following method: A1. Add epoxy grafted copolymer elastomer, 1,3,5-tris(2-hydroxyethyl)isocyanuric acid and toluene to the reactor. Heat the reactor to 70-90℃ and stir until the materials are mixed evenly. Then add p-benzenesulfonic acid and heat the reactor to 80-100℃. Keep it warm and stir for 2-4 hours. The post-treatment yields trihydroxyisocyanate modified prepolymer. A2. Add the triazine-reinforced epoxy prepolymer to the reactor, heat the reactor to 60-80℃, add 3-isocyanate-propyltrimethoxysilane and dibutyltin dilaurate, keep the mixture warm and stir for 1-2 hours, then cool the reactor to 50-60℃ and add the modification solution, continue to keep the mixture warm and stir for 2-4 hours, and then obtain the silicon-oxygen hybrid composite.

2. The disposable insulating plug with long-lasting aging resistance according to claim 1, characterized in that, In step A1, the ratio of the epoxy grafted copolymer elastomer, 1,3,5-tris(2-hydroxyethyl)isocyanuric acid, p-benzenesulfonic acid, and toluene is 25g:5-8g:40-60mL:0.2-0.3g; in step A2, the ratio of the triazine-reinforced epoxy prepolymer, 3-isocyanate-propyltrimethoxysilane, dibutyltin dilaurate, and the modifying solution is 25g:4-6mL:0.1-0.2g:20-24mL, wherein the modifying solution is obtained by mixing anhydrous ethanol, deionized water, and acetic acid in a ratio of 10-12mL:10-12mL:0.2mL.

3. The disposable insulating plug with long-lasting aging resistance according to claim 1, characterized in that, The preparation method of the epoxy grafted copolymer elastomer is as follows: isobutylene is introduced into a low-temperature reactor containing allyl glycidyl ether and anhydrous n-hexane. After the introduction is completed, the reactor is cooled to -65°C, boron trifluoride diethyl ether is added, and the mixture is kept warm and stirred for 1-2 hours. After stirring is completed, methanol is added. After the reactor is restored to room temperature and pressure, the epoxy grafted copolymer elastomer is obtained through post-treatment.

4. A disposable insulating plug with long-lasting aging resistance as described in claim 3, characterized in that, The ratio of isobutylene, allyl glycidyl ether, anhydrous n-hexane, boron trifluoride ethyl ether, and methanol is 1200mL:12-18mL:100mL:0.1-0.2mL:3mL.

5. A disposable insulating plug with long-lasting aging resistance as described in claim 1, characterized in that, The silica-shelled triazine microspheres were prepared by the following method: B1. After adding deionized water and polyvinyl alcohol to the reaction vessel and stirring evenly, add oil phase liquid and heat the reaction vessel to 50-70℃, keep it at the temperature for 2-4 hours, and then obtain triazine mercaptoether crosslinked microspheres. B2. Triazine mercaptoether crosslinked microspheres, anhydrous ethanol and deionized water were added to the reaction vessel and stirred until they were evenly dispersed. Then, 3-(2,3-epoxypropoxy)propyltrimethoxysilane and acetic acid were added to the reaction vessel. The reaction vessel was then heated to 40-60℃ and stirred for 3-5 hours. The resulting product was a silicon-shelled triazine microsphere.

6. A disposable insulating plug with long-lasting aging resistance as described in claim 5, characterized in that, In step B1, the ratio of deionized water, polyvinyl alcohol, and oil phase is 300 mL: 2-3 g: 180 g, wherein the oil phase is obtained by mixing pentaerythritol tetra(3-mercaptopropionate), tri-2-acrylate [2,4,6-trioxo-1,3,5-triazine-1,3,5(2H,4H,6H)-trimethyl]tri-2,1-ethylene ester, and 2-hydroxy-2-methyl-1-phenyl-1-propanone in a ratio of 100-120 g: 90 g: 2 g; in step B2, the ratio of triazine mercaptoether crosslinked microspheres, anhydrous ethanol, deionized water, 3-(2,3-epoxypropoxy)propyltrimethoxysilane, and acetic acid is 100 g: 150 mL: 40-50 mL: 12-15 mL: 0.3 mL.

7. A disposable insulating plug with long-lasting aging resistance as described in claim 1, characterized in that, The epoxy amine-cured flexible particles are prepared by the following method: C1. Add adipic acid, neopentyl glycol, p-toluenesulfonic acid and 2,6-di-tert-butyl-p-cresol to a reactor. Under nitrogen protection, heat the reactor to 180-200℃, keep it at this temperature and stir. Reduce the pressure to 40 kPa within 15-20 min, then reduce the pressure to 10 kPa within 15-30 min. Continue to react at constant temperature and pressure for 1-2 h. Cool down and discharge to obtain adipic acid-neopentyl glycol polyester diol. C2. Add adipic acid-neopentyl glycol polyester diol to the reactor and heat the reactor to 60-70℃. Then add polyetheramine and bisphenol A epoxy resin and heat the reaction to 80-100℃. Keep the temperature and stir for 2-4 hours. After post-treatment, epoxy amine cured flexible particles are obtained.

8. A disposable insulating plug with long-lasting aging resistance according to claim 7, characterized in that, In step C1, the ratio of adipic acid, neopentyl glycol, p-toluenesulfonic acid, and 2,6-di-tert-butyl-p-cresol is 100g:100-120g:0.5g:0.2g; in step C2, the ratio of adipic acid-neopentyl glycol polyester glycol, polyetheramine, and bisphenol A epoxy resin is 120g:60-80g:80-100g.

9. A method for preparing a disposable insulating plug with long-lasting aging resistance as described in any one of claims 1-8, characterized in that, Includes the following steps: S1. Add the silicon-oxygen hybrid composite, silicon-shell triazine microspheres, epoxy amine-cured flexible particles and 2,6-di-tert-butyl-p-cresol to a mixer, heat the mixer to 100-120℃, and maintain the temperature for 15-20 minutes. After the mixer is completed, let the mixer cool to room temperature, take out the material and process it into a pre-blended material with a particle size of 3-5mm through a granulator. S2. Spread the pre-mixed material evenly in the preheated mold cavity. After the mold is closed, treat it at 160-180℃ and 16-20MPa for 15-20 minutes. After hot pressing, cool the mold and the product together to 40-60℃, open the mold and remove the product to obtain a disposable isolation plug.