Radiation resistant epoxy potting adhesive composition with high thermal conductivity, and preparation method and application thereof

Abstract

This invention provides a radiation-resistant and highly thermally conductive epoxy potting compound composition, its preparation method, and its application. The epoxy potting compound composition of this invention comprises component A and component B; wherein, per 100 parts by weight of component A, the raw materials of component A include: 60-98 parts by weight of epoxy resin; 1-10 parts by weight of diluent; and 1-30 parts by weight of radiation-resistant particles; per 150 parts by weight of component B, the raw materials of component B include: 80-110 parts by weight of anhydride curing agent; 0.1-0.5 parts by weight of accelerator; 1-5 parts by weight of additives; and 34.5-68.9 parts by weight of modified thermally conductive filler. Through the synergistic combination of the above components, the epoxy potting compound composition of this invention ultimately achieves a harmonious balance of flowability, curing speed, temperature resistance, radiation resistance, and thermal conductivity.

Description

Technical Field

[0001] This invention belongs to the field of radiation-resistant and thermally conductive potting compound technology, specifically relating to a radiation-resistant and highly thermally conductive epoxy potting compound composition, its preparation method, and its application. Background Technology

[0002] Developing new energy sources is an inevitable trend for achieving sustainable development in my country. Nuclear power, as a low-carbon energy source, is an important component of new energy and a crucial foundation for my country's future sustainable energy development. Currently, my country's nuclear power industry is in a phase of rapid development.

[0003] Nuclear radiation can easily cause problems such as bubbling, powdering, and cracking of potting compounds, thereby compromising their protective function. Therefore, potting compounds must possess certain radiation resistance and strong adhesion properties to be used in nuclear radiation environments. For the safe and sustainable use of nuclear power energy, radiation-resistant potting compounds are typically used to protect equipment and related facilities in nuclear power plants. Especially for high-power, high-heat-generating components, high thermal conductivity, radiation-resistant potting compounds are usually used for potting protection.

[0004] In the field of radiation-resistant potting compounds, epoxy resin is widely used in shielding materials due to its advantages such as good corrosion resistance, resistance to neutron and gamma ray radiation damage, simple curing process, good heat resistance, low curing shrinkage, and strong adhesion. For example, epoxy resin can be used as potting compound for nuclear power plant walls or floor coatings.

[0005] CN101245215A discloses a radiation-resistant coating for nuclear power plants, consisting of two components, A and B. Component A comprises epoxy resin, radiation-resistant filler, reactive diluent, and a small amount of additives, while component B is a modified amine curing agent. Although this radiation-resistant coating has certain radiation resistance and absorption properties, its thermal conductivity and heat resistance are both low, and its curing speed is not adjustable, making it unsuitable for radiation-resistant encapsulation of high-power devices.

[0006] CN111286156B discloses a low-temperature radiation-resistant insulating material, whose resin components are bisphenol A type epoxy and alicyclic epoxy, and whose curing agent components are aromatic diamine curing agent and flexible amine curing agent. However, its mechanical properties and thermal conductivity are both low, with an impact strength ≤7kJ.m² and a thermal conductivity ≤0.7W / (m·K).

[0007] CN114773964A discloses a radiation-resistant phenolic epoxy paint, with phenolic epoxy as the main resin, polyamide as the curing agent, and various additives, such as mixed solvents, silane coupling agents, anti-settling agents, wetting and dispersing agents, leveling agents, defoamers, etc., but does not mention thermal conductivity.

[0008] With the rapid development of nuclear power technology in my country, the requirements for nuclear power safety protection systems are becoming increasingly stringent. Therefore, it is of great significance to provide an epoxy potting compound with excellent radiation resistance, good thermal conductivity, and adjustable curing speed. Summary of the Invention

[0009] To address the shortcomings of existing technologies, the present invention adopts the following technical solution:

[0010] An epoxy potting compound composition comprising component A and component B; wherein,

[0011] Based on 100 parts by weight of component A, the raw materials of component A include:

[0012] 60-98 parts by weight of epoxy resin;

[0013] 1-10 parts by weight of diluent;

[0014] 1-30 parts by weight of radiation-resistant particles;

[0015] Based on 150 parts by weight of component B, the raw materials of component B include:

[0016]

[0017] According to an embodiment of the present invention, in the epoxy potting compound composition, the mass ratio of component A to component B is 1:1-2, for example, 1:1.5.

[0018] According to an embodiment of the present invention, component A and component B do not come into contact.

[0019] According to an embodiment of the present invention, in component A, the amount of epoxy resin added per 100 parts by weight can be 65 parts by weight, 70 parts by weight, 75 parts by weight, 80 parts by weight, 85 parts by weight, 90 parts by weight, 95 parts by weight, or a range between any two of the above values.

[0020] According to an embodiment of the present invention, in component A, the amount of the active diluent added per 100 parts by weight can be 1 part by weight, 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 parts by weight, 10 parts by weight, or a range between any two of the above points.

[0021] According to an embodiment of the present invention, in component A, the amount of radiation-resistant particles added per 100 parts by weight can be 5 parts by weight, 10 parts by weight, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, or a range between any two of the above values.

[0022] According to an embodiment of the present invention, in component B, the amount of anhydride curing agent added per 150 parts by weight is 85 parts by weight, 90 parts by weight, 95 parts by weight, 100 parts by weight, 105 parts by weight, or a range between any two of the above values.

[0023] According to an embodiment of the present invention, in component B, the amount of the accelerator added per 150 parts by weight is 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, or a range between any two of the above values.

[0024] According to an embodiment of the present invention, in component B, the amount of the additive added per 150 parts by weight is 1 part by weight, 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 parts by weight, or a range between any two of the above values.

[0025] According to an embodiment of the present invention, in component B, the amount of the modified thermally conductive filler added per 150 parts by weight is 35 parts by weight, 40 parts by weight, 50 parts by weight, 60 parts by weight, or a range between any two of the above values.

[0026] According to embodiments of the present invention, the epoxy resin refers to a linear organic polymer compound containing two or more epoxy groups. Preferably, the epoxy resin includes one or two of trifunctional alicyclic epoxy and alicyclic epoxy. Further, the mass ratio of the trifunctional alicyclic epoxy to the alicyclic epoxy is 1-5:1, for example, 2:1.

[0027] According to an embodiment of the present invention, the epoxy equivalent of the epoxy resin is greater than 100 g / eq, for example, 110 g / eq, 120 g / eq, 130 g / eq, or 150 g / eq.

[0028] According to an embodiment of the present invention, the viscosity of the epoxy resin is less than 400 mPa·s (25°C), for example, 220 to 260 mPa·s (25°C).

[0029] According to an embodiment of the present invention, the trifunctional alicyclic epoxy is 4,5-epoxycyclohexane-1,2-dicarboxylic acid diglycidyl ester, for example, commercially available MF-3285.

[0030] According to an embodiment of the present invention, the alicyclic epoxy is dicyclopentadiene dioxide, for example, R-122 resin.

[0031] According to an embodiment of the present invention, the trifunctional alicyclic epoxy has an epoxy equivalent greater than 100 g / eq, for example, 120 g / eq.

[0032] According to an embodiment of the present invention, the alicyclic epoxy has an epoxy equivalent greater than 100 g / eq, for example, 130 g / eq. The viscosity of the alicyclic epoxy is 220–260 mPa·s (25°C).

[0033] In this invention, component A is selected as epoxy resin as the main body. Due to the chemical activity of the epoxy groups in the epoxy resin, it can react with various compounds containing active hydrogen to open the ring, cure and crosslink to form a network structure, and has excellent chemical stability, corrosion resistance, adhesion and electrical insulation properties. At the same time, epoxy resin has better processing technology and wider application compared with other resins. Among them, trifunctional aliphatic epoxy has a higher epoxy value and a higher degree of crosslinking after reaction with acid anhydrides, thus giving the epoxy potting compound better heat resistance. The epoxy groups of alicyclic epoxy are not derived from epichlorohydrin, but are obtained by epoxidation of the double bonds of alicyclic olefins. Therefore, its chlorine content is low, which can effectively avoid the generation of free radicals with long half-lives by chlorine atoms to accelerate epoxy degradation, thereby improving the weather resistance and radiation resistance of the potting compound.

[0034] According to an embodiment of the present invention, in component A, the diluent is an active diluent.

[0035] According to an embodiment of the present invention, the reactive diluent is selected from at least one of propylene oxide butyl glycidyl ether, propylene oxide phenyl ether, polypropylene glycol diglycidyl ether, and / or benzyl glycidyl ether. The reactive diluent of the present invention can directly participate in the curing reaction of the potting compound, becoming part of the product after curing, and can significantly improve process performance.

[0036] According to an embodiment of the present invention, in component A, the radiation-resistant particles are selected from at least one of talc, mica powder, titanium dioxide, and potassium titanate whiskers. The radiation-resistant particles added in this invention, such as potassium titanate, can be used for absorbing radiation; the sheet-like shielding fillers, mica powder and talc powder, not only improve the radiation resistance of the potting compound, but also increase the intermolecular forces of the polymer, enhance the flexural and compressive strength of the cured potting compound, effectively disperse internal stress, reduce the risk of stress concentration in the cured compound, inhibit crack growth, and improve the impact resistance of the cured compound.

[0037] According to an embodiment of the present invention, the particle size of the radiation-resistant particles is selected from 10 nm to 10 μm, for example, 10 to 100 nm, 1 to 5 μm, 1 to 10 μm, or 10 to 20 μm.

[0038] Preferably, the talc powder has a particle size of 1 to 5 μm, such as 1 μm, 2 μm, 3 μm, 4 μm, 5 μm or 30 μm, or a specific particle size between the above values.

[0039] Preferably, the mica powder has a particle size of 1 to 10 μm, for example, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, or specific particle sizes between the above values.

[0040] Preferably, the titanium dioxide particle size is 10-20 μm, for example 10 μm, 12 μm, 14 μm, 16 μm, 18 μm, 20 μm, or specific particle sizes between the above values.

[0041] Preferably, the potassium titanate whisker has a particle size of 10–100 nm, such as 10 nm, 20 nm, 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, or any specific value between any two of the above values.

[0042] According to an embodiment of the present invention, in component B, the anhydride curing agent is selected from at least one or more of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, and methylmethylenetetrahydrophthalic anhydride. The anhydride curing agent in component B of the present invention has low viscosity, and its resonance effect with the conjugated benzene ring structure in the cured product after epoxy reaction disperses energy transfer, preventing energy concentration and valence bond damage, thus ensuring the stability of the radiation resistance of the final potting compound.

[0043] According to an embodiment of the present invention, in component B, the accelerator is selected from at least one or more of 2,4,6-tris(dimethylaminomethyl)phenol / DMP-30, 2-ethyl-4-methylimidazole, N,N-dimethylbenzylamine / BDMA, and boron trifluoride ethylamine.

[0044] According to embodiments of the present invention, the additives include leveling agents and / or defoamers. Preferably, the defoamer is at least one selected from polydimethylpolysiloxanes, polyethers, and polyether-modified silicones. Preferably, the leveling agent is at least one selected from polyvinyl alcohols and polysiloxanes. The additives added to component B can effectively improve the leveling and / or defoaming properties of the potting compound system.

[0045] According to an embodiment of the present invention, the modified thermally conductive filler is selected from at least one of coupling agent-modified thermally conductive fillers and amine-modified thermally conductive fillers. Preferably, the thermally conductive filler is selected from at least one or more of alumina, boron nitride, and aluminum nitride. Preferably, the coupling agent is selected from one or more of silane coupling agents, such as KH-560, KH-550, KH-570, KH-580, and B-201. Preferably, the amine is selected from one or more of dopamine, dopamine hydrochloride, and melamine.

[0046] The modified thermally conductive filler in component B of this invention not only possesses strong thermal conductivity, significantly improving the thermal conductivity of the epoxy potting compound, but also effectively reduces the curing shrinkage rate of the epoxy potting compound, ensuring the adhesion performance and dimensional stability of the final cured product. For example, the modified boron nitride thermally conductive filler has a plate-like structure and its crystal type is atomic crystal, possessing strong atomic bonds. This effectively reduces phonon scattering caused by lattice defects, thereby exhibiting strong thermal conductivity and significantly improving the thermal conductivity of the epoxy potting compound.

[0047] According to an embodiment of the present invention, the coupling agent-modified thermally conductive filler is obtained by the following method: mixing the coupling agent and the thermally conductive filler in a solvent, and then heating and reacting under an inert atmosphere to obtain the coupling agent-modified thermally conductive filler. Preferably, the heating reaction temperature is 80-85°C. Preferably, the solvent is selected from alcohol solvents, such as anhydrous ethanol.

[0048] According to a preferred embodiment of the present invention, the coupling agent modified thermally conductive filler is obtained by the following method:

[0049] Step 1: Dissolve the coupling agent in a solvent to obtain a coupling agent solution;

[0050] Step 2: Add the thermally conductive filler to the coupling agent solution, heat to 80-85℃, reflux for 30-40 minutes under a nitrogen atmosphere, cool and centrifuge, and finally dry at 100-120℃ for 2 hours to obtain the coupling agent modified thermally conductive filler.

[0051] According to an embodiment of the present invention, the amine-modified thermally conductive filler is obtained by the following method: mixing an amine and a thermally conductive filler in a solvent, and then heating the mixture to react, thereby obtaining the amine-modified thermally conductive filler. Preferably, the temperature of the heating reaction is 80-85°C. Preferably, the solvent is selected from alcohol solvents, such as anhydrous ethanol.

[0052] Step 1': Dissolve the thermally conductive filler in a solvent to obtain a suspension of the thermally conductive filler;

[0053] Step 2': The amine substances are dissolved in the suspension of the thermally conductive filler, and then the pH is adjusted to alkaline (e.g., 8.5). The amine substances self-polymerize on the surface of the thermally conductive filler particles to form a thermally conductive filler coated with polyamine substances, which is the thermally conductive filler modified with amine substances.

[0054] The present invention also provides a method for preparing the above-mentioned epoxy potting compound composition, the method comprising: preparing component A and component B respectively to obtain the epoxy potting compound composition.

[0055] According to an embodiment of the present invention, the method for preparing component A is as follows: two epoxy resins, a diluent, and radiation-resistant particles are mixed to obtain component A.

[0056] According to an embodiment of the present invention, the method for preparing component B is as follows: mixing an anhydride curing agent, an accelerator, a modified thermally conductive filler, and an additive to obtain component B.

[0057] According to an embodiment of the present invention, when preparing component A or component B, the mixing can be carried out using methods known in the art, as long as uniform mixing is achieved.

[0058] The present invention also provides a method of using the above-mentioned epoxy potting compound composition, the method comprising: uniformly mixing component A and component B in the above-mentioned epoxy potting compound composition, and heating for gradient curing.

[0059] According to an embodiment of the present invention, the gradient curing includes a first step of heat curing, a second step of heat curing, and a third step of heat curing. Further, the first step of heat curing refers to curing at a temperature not exceeding 80°C for 0.5-5 hours. Further, the second step of heat curing refers to curing at a temperature not exceeding 100°C for 0.5-5 hours. Further, the third step of heat curing refers to curing at a temperature not exceeding 120°C for 0.5-5 hours. Exemplarily, the gradient curing conditions are: 80°C / 3 hours, 100°C / 6 hours, and 120°C / 6 hours, with a heating rate of 2°C / min. The inventors have found that gradient curing can effectively prevent a sudden increase in curing temperature from triggering a violent polymerization reaction, and can also prevent rapid changes in external temperature from causing stress concentration in the cured material, thereby preventing cracking.

[0060] According to an embodiment of the present invention, the cured epoxy potting compound composition has at least one of the following properties:

[0061] 1) Unnotched impact strength greater than 10 KJ / m 2 For example, 16KJ / m 2 ;

[0062] 2) Thermal conductivity greater than 0.5 W / (m·K), for example 1.532 W / (m·K);

[0063] 3) The radiation tolerance dose is not less than 800 kGy, for example, 1250 kGy.

[0064] This invention also provides the application of the above-described epoxy potting compound composition in irradiation scenarios, such as in the nuclear power field, and preferably in thermally conductive devices used in irradiation scenarios. Preferably, the epoxy potting compound composition is used in irradiation scenarios after being cured by the above-described application method.

[0065] Compared with the prior art, the present invention has the following beneficial effects:

[0066] The epoxy potting compound composition provided by this invention includes component A and component B. Each component uses a combination of specific raw materials to achieve the optimal ratio and synergistic effect, ultimately resulting in a high-performance epoxy potting compound with coordinated and unified flowability, curing speed, temperature resistance, radiation resistance, and thermal conductivity.

[0067] The purpose of this invention is to provide a radiation-resistant and highly thermally conductive epoxy potting compound composition, its preparation method, and its application. The radiation-resistant and highly thermally conductive epoxy potting compound composition comprises two components. Through the rational design of each component, it has advantages such as high strength, good heat resistance, good thermal conductivity, and excellent radiation resistance. Detailed Implementation

[0068] The technical solution of the present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are merely illustrative and explanatory of the present invention, and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are covered within the scope of protection intended by the present invention.

[0069] Unless otherwise stated, the raw materials and reagents used in the following examples are commercially available products or can be prepared by known methods.

[0070] In particular, some raw material information involved in the specific embodiments of the present invention is as follows:

[0071] Trifunctional alicyclic epoxy resin (hereinafter referred to as trifunctional alicyclic epoxy): purchased from Hubei Zhenzhengfeng New Material Co., Ltd., model number MF-3285.

[0072] Alicyclic epoxy: Dicyclopentadiene dioxide, selected from domestically produced resin with the grade R-122.

[0073] The defoamer was a polydimethylpolysiloxane, purchased from Yueguan New Materials Co., Ltd.

[0074] The boron nitride particles were purchased from Wuxi Shengheyu New Materials Co., Ltd., with a particle size of 20 μm.

[0075] The alumina particles were purchased from Wuxi Shengheyu New Materials Co., Ltd., with a particle size of 20μm.

[0076] Diluent: Specifically, propylene oxide butyl glycidyl ether, purchased from Aladdin, model (501).

[0077] Radiation-resistant particles: specifically talc powder, purchased from Guangzhou Yifeng Chemical Technology Co., Ltd., model number 2500 mesh.

[0078] Preparation Example 1

[0079] The preparation method of KH-560 modified boron nitride is as follows: boron nitride with a particle size of 20 μm is added to a mixed solution of γ-glycidoxypropyltrimethoxysilane and ethanol, and stirred at 80℃ for 5 h. After cooling, it is centrifuged and finally dried at 120℃ for 3 h to obtain KH-560 modified boron nitride.

[0080] The preparation method of KH-560 modified alumina is as follows: Alumina with a particle size of (20) μm is added to a mixed solution of γ-glycidyl etheroxypropyltrimethoxysilane and ethanol, and stirred at 80°C for 5 h. After cooling, it is centrifuged and finally dried at 120°C for 3 h to obtain KH-560 modified alumina.

[0081] Preparation Example 2

[0082] 1. The specific steps for modifying boron nitride with dopamine hydrochloride are as follows:

[0083] Step 1: Place the boron nitride particles in an oven and dry them at 80℃ for 12 hours for later use;

[0084] Step 2: Weigh a certain amount of dried boron nitride particles and add them to ethanol to obtain a boron nitride suspension. The mass ratio of boron nitride to ethanol is 1:15.

[0085] Step 3: Weigh a certain amount of dopamine hydrochloride and add it to the boron nitride suspension obtained in Step 2. Stir and dissolve to obtain a mixed suspension. The mass ratio of dopamine hydrochloride to boron nitride particles is 1:4.

[0086] Step 4: Add tris(hydroxymethyl)aminomethane (Tris, a buffer solution used to adjust the pH of the dopamine solution) to the mixed suspension in Step 3, stir well, and use a pH meter to measure the pH of the suspension in real time. Continue to add Tris until the pH of the suspension is adjusted to 8.5.

[0087] Step 5: Place the suspension with pH 8.5 from Step 4 in a fume hood and stir. After dopamine self-polymerizes to form polydopamine coating on the surface of boron nitride particles, stop the reaction, filter, and wash three times with deionized water to obtain polydopamine-coated boron nitride particles. Dry them at 60°C for 12 hours for later use.

[0088] 2. Following steps one through five above, and replacing boron nitride with aluminum oxide, dopamine hydrochloride-modified aluminum oxide is prepared.

[0089] The modified alumina and boron nitride in Examples 1 and 2 above both had a particle size of 20 μm.

[0090] In the following examples, after preparing component A and component B, they were stored separately.

[0091] Example 1

[0092] A radiation-resistant, high thermal conductivity epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1.5;

[0093] The raw materials of component A include the following components in parts by weight:

[0094] 80 parts by weight of trifunctional alicyclic epoxy;

[0095] 5 parts by weight of propylene oxide butyl ether;

[0096] 15 parts by weight of talc;

[0097] The preparation method of component A includes: uniformly mixing trifunctional alicyclic epoxy, propylene oxide butyl ether, and talc at 60°C to obtain component A for later use;

[0098] The raw materials for component B include the following components by weight:

[0099] 100 parts by weight of methyltetrahydrophthalic anhydride;

[0100] 0.15 parts by weight of N,N-dimethylbenzylamine;

[0101] 1.5 parts by weight of defoamer;

[0102] 48.35 parts by weight of KH-560 modified alumina;

[0103] The preparation method of component B includes: uniformly mixing methyltetrahydrophthalic anhydride, N,N-dimethylbenzylamine, KH-560 modified alumina, and defoamer to obtain component B for later use.

[0104] Example 2

[0105] A radiation-resistant, high thermal conductivity epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1.5;

[0106] The raw materials of component A include the following components in parts by weight:

[0107]

[0108] The preparation method of component A includes: uniformly mixing trifunctional alicyclic epoxy, modified alicyclic epoxy, propylene oxide butyl ether, talc powder, and potassium titanate whiskers at 60°C to obtain component A for later use;

[0109] The raw materials for component B include the following components by weight:

[0110]

[0111] The preparation method of component B includes: uniformly mixing methyltetrahydrophthalic anhydride, N,N-dimethylbenzylamine, KH-560 modified alumina, and defoamer to obtain component B for later use.

[0112] Example 3

[0113] A radiation-resistant, high thermal conductivity epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1.5;

[0114] The raw materials of component A include the following components in parts by weight:

[0115]

[0116] The preparation method of component A includes: uniformly mixing trifunctional alicyclic epoxy, alicyclic epoxy, propylene oxide butyl ether, talc powder, and potassium titanate whiskers at 60°C to obtain component A for later use;

[0117] The raw materials for component B include the following components by weight:

[0118]

[0119] The preparation method of component B includes: uniformly mixing methyltetrahydrophthalic anhydride, 2-ethyl-4-methylimidazole, KH-560 modified boron nitride, and defoamer to obtain component B for later use.

[0120] Example 4

[0121] A radiation-resistant, high thermal conductivity epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1.5;

[0122] The raw materials of component A include the following components in parts by weight:

[0123]

[0124] The preparation method of component A includes: uniformly mixing trifunctional alicyclic epoxy, alicyclic epoxy, propylene oxide butyl ether, talc powder, and potassium titanate whiskers at 60°C to obtain component A for later use;

[0125] The raw materials for component B include the following components by weight:

[0126]

[0127] The preparation method of component B includes: uniformly mixing methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, KH-560 modified boron nitride, and defoamer to obtain component B for later use.

[0128] Example 5

[0129] A radiation-resistant, high thermal conductivity epoxy potting compound composition differs from Example 4 in that methyl hexahydrophthalic anhydride is replaced with methyl nadic anhydride, while the other components, dosages, and preparation methods are the same as in Example 4.

[0130] Example 6

[0131] A radiation-resistant, high thermal conductivity epoxy potting compound composition differs from Example 5 in that the dopamine hydrochloride-modified alumina is replaced with dopamine hydrochloride-modified boron nitride; the other components, dosages, and preparation methods are the same as in Example 5.

[0132] Example 7

[0133] A radiation-resistant, high thermal conductivity epoxy potting compound composition differs from Example 6 in that the dopamine hydrochloride-modified boron nitride is replaced with KH-560-modified boron nitride; the other components, dosages, and preparation methods are the same as in Example 6.

[0134] Example 8

[0135] A radiation-resistant, high thermal conductivity epoxy potting compound composition differs from Example 7 in that KH-560 modified boron nitride is replaced with KH-560 modified aluminum nitride, while the other components, dosages, and preparation methods are the same as in Example 7.

[0136] Comparative Example 1

[0137] A radiation-resistant epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1;

[0138] Component A comprises the following components in parts by weight:

[0139] Trifunctional toughened aromatic epoxy (MF-3301) 70 parts by weight;

[0140] 15 parts by weight of low-halogenated bisphenol A type epoxy;

[0141] 15 parts by weight of mica powder;

[0142] The preparation method of component A includes: uniformly mixing trifunctional toughened aromatic epoxy (MF-3301), low-halogen bisphenol A type epoxy, and mica powder at 60°C to obtain component A for later use;

[0143] Component B comprises the following components in parts by weight:

[0144] 60 parts by weight of diamine curing agent;

[0145] 38.5 parts by weight of quartz powder;

[0146] 1.2 parts by weight of defoamer;

[0147] The preparation method of component B includes: uniformly mixing diamine curing agent, quartz powder and defoamer to obtain component B for later use.

[0148] Comparative Example 2

[0149] A radiation-resistant epoxy potting compound composition comprising component A and component B in a mass ratio of 1:1.2;

[0150] Component A comprises the following components in parts by weight:

[0151] Trifunctional toughened aromatic epoxy (MF-3301) 70 parts by weight;

[0152] 15 parts by weight of low-halogenated bisphenol A type epoxy;

[0153] 15 parts by weight of mica powder;

[0154] The preparation method of component A includes: uniformly mixing trifunctional toughened aromatic epoxy, low-halogen bisphenol A type epoxy, and mica powder at 60°C to obtain component A for later use;

[0155] Component B comprises the following components in parts by weight:

[0156]

[0157] The preparation method of component B includes: uniformly mixing methyltetrahydrophthalic anhydride, 2-ethyl-4-methylimidazolium, quartz powder, and defoamer to obtain component B for later use.

[0158] Comparative Example 3

[0159] A radiation-resistant epoxy potting compound composition differs from Comparative Example 1 in that the aromatic amine replaces the diamine curing agent, while the other components, dosages, and preparation methods are the same as those in Comparative Example 1.

[0160] Comparative Example 4

[0161] A radiation-resistant epoxy potting compound composition differs from Comparative Example 1 in that alumina replaces talc powder, while the other components, dosages, and preparation methods are the same as those in Comparative Example 1.

[0162] Test Example 1

[0163] Components A and B from the above examples and comparative examples were mixed separately, vacuum degassed at 80°C for 40 min, and cured at room temperature to obtain the test samples; the following tests were performed, and the test results are shown in Table 1:

[0164] (1) Viscosity at 25℃: (Test standard: Single cylinder rotational viscometer method: GB / T 2794-2013);

[0165] (2) Thermal conductivity: (Testing standard: GB / T 39862-2021);

[0166] (3) Radiation tolerance: (Test method and index: Maintaining good performance after ionizing radiation of 700-1250 kGy);

[0167] (4) Bending strength: (Test standard: Test method for performance of resin castings GB / T 2567-2021);

[0168] (5) Compressive strength: (Test standard: Test method for performance of resin castings GB / T 2567-2021);

[0169] (6) Unnotched impact strength: (Test standard: Test method for performance of resin castings GB / T2567-2021).

[0170] Table 1

[0171]

[0172] According to Table 1:

[0173] 1) Examples 1-8 use epoxy resin potting compounds, which have significant advantages in radiation resistance and thermal conductivity: The potting compound sample of Example 8 can withstand a radiation dose of up to 1250 kGy, and the sample surface has no cracks, radiation corrosion, ablation, etc., and the size remains unchanged, proving that the potting compound of the present invention has good radiation resistance; and the thermal conductivity of the epoxy potting compound of the present invention can reach 1.532 W / (m·K), which is 770% of the thermal conductivity of pure epoxy resin (the thermal conductivity of pure epoxy resin is 0.2 W / (m·K).

[0174] 2) As shown in Examples 1-8, adding modified aliphatic epoxy to epoxy resin can effectively reduce the viscosity of the system, improve the flowability of the system, and increase the impact strength of the system, reaching a value of 16 KJ / m. 2 .

[0175] 3) Adding potassium titanate thermally conductive filler to the potting compound composition can effectively absorb radiation damage and further improve the system's radiation resistance.

[0176] 4) Comparing the thermal conductivity of the examples and comparative examples, it can be seen that in the potting compound composition, the thermally conductive filler improves the thermal conductivity of the system in the following way: KH-560 modified aluminum nitride > KH-560 modified boron nitride > dopamine hydrochloride modified boron nitride > dopamine hydrochloride modified alumina > KH-560 modified alumina > quartz powder.

[0177] The exemplary embodiments of the present invention have been described above. However, the scope of protection of this application is not limited to the above embodiments. Any modifications, equivalent substitutions, improvements, etc., made by those skilled in the art within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. An epoxy potting compound composition, characterized in that, The epoxy potting compound composition comprises component A and component B; wherein... Based on 100 parts by weight of component A, the raw materials of component A include: 60-98 parts by weight of epoxy resin; 1-10 parts by weight of diluent; 1-30 parts by weight of radiation-resistant particles; Based on 150 parts by weight of component B, the raw materials of component B include:

2. The epoxy potting compound composition according to claim 1, characterized in that, In the epoxy potting compound composition, the mass ratio of component A to component B is 1:1-2. Preferably, component A and component B do not come into contact. Preferably, the epoxy resin refers to a linear organic polymer compound containing two or more epoxy groups. Preferably, the epoxy resin includes one or two of trifunctional alicyclic epoxy and alicyclic epoxy. Further, the mass ratio of the trifunctional alicyclic epoxy to the alicyclic epoxy is 1-5:

1. Preferably, the epoxy equivalent of the epoxy resin is greater than 100 g / eq. Preferably, the viscosity of the epoxy resin is less than 400 mPa·s. Preferably, the trifunctional alicyclic epoxy is 4,5-epoxycyclohexane-1,2-dicarboxylic acid diglycidyl ester. Preferably, the alicyclic epoxy is dicyclopentadiene dioxide.

3. The epoxy potting compound composition according to claim 1 or 2, characterized in that, In component A, the diluent is an active diluent. Preferably, the reactive diluent is selected from at least one of propylene oxide butyl glycidyl ether, propylene oxide phenyl ether, polypropylene glycol diglycidyl ether, and / or benzyl glycidyl ether. Preferably, in component A, the radiation-resistant particles are selected from at least one of talc, mica, titanium dioxide, and potassium titanate whiskers. Preferably, the particle size of the radiation-resistant particles is selected from 10 nm to 10 μm.

4. The epoxy potting compound composition according to any one of claims 1-3, characterized in that, In component B, the anhydride curing agent is selected from at least one or more of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, and methylnemidytetrahydrophthalic anhydride. Preferably, in component B, the accelerator is selected from at least one or more of 2,4,6-tris(dimethylaminomethyl)phenol / DMP-30, 2-ethyl-4-methylimidazole, N,N-dimethylbenzylamine / BDMA, and boron trifluoride ethylamine. Preferably, the additives include leveling agents and / or defoamers. Preferably, the modified thermally conductive filler is selected from at least one of coupling agent-modified thermally conductive fillers and amine-modified thermally conductive fillers.

5. A method for preparing the epoxy potting compound composition according to any one of claims 1-4, characterized in that, The preparation method includes: preparing component A and component B respectively to obtain an epoxy potting compound composition.

6. The preparation method according to claim 5, characterized in that, The method for preparing component A is as follows: two epoxy resins, a diluent, and radiation-resistant particles are mixed to obtain component A. Preferably, the method for preparing component B is as follows: mixing an anhydride curing agent, an accelerator, a modified thermally conductive filler, and an additive to obtain component B.

7. The method of using the epoxy potting compound composition according to any one of claims 1-4, characterized in that, The method of use includes: uniformly mixing component A and component B of the epoxy potting compound composition according to any one of claims 1-4, and heating for gradient curing.

8. The method of use according to claim 7, characterized in that, The gradient curing process includes a first step of heat curing, a second step of heat curing, and a third step of heat curing. Further, the first step of heat curing refers to curing at a temperature not exceeding 80°C for 0.5-5 hours. Further, the second step of heat curing refers to curing at a temperature not exceeding 100°C for 0.5-5 hours. Further, the third step of heat curing refers to curing at a temperature not exceeding 120°C for 0.5-5 hours.

9. The method of use according to claim 7 or 8, characterized in that, The cured epoxy potting compound composition has at least one of the following properties: 1) Unnotched impact strength greater than 10 KJ / m 2 ; 2) Thermal conductivity greater than 0.5 W / (m·K); 3) The radiation tolerance dose is not less than 800 kGy.

10. The use of the epoxy potting compound composition according to any one of claims 1-4 in irradiation scenarios.

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