Temperature-resistant polyfunctional epoxy resin and preparation method thereof

Abstract

The invention discloses temperature-resistant polyfunctional epoxy resin and a preparation method thereof. On one hand, the invention provides the temperature-resistant polyfunctional epoxy resin, and the temperature-resistant polyfunctional epoxy resin is prepared from the following raw material components in parts by mass: 100 parts of AFG-90 polyfunctional epoxy resin, 20 to 40 parts of epoxy-terminated polyphenyl ether, 8 to 16 parts of epoxy modified silicone oil and 6 to 12 parts of hydrophobic fumed silica. On the other hand, the invention provides a preparation method of the temperature-resistant polyfunctional epoxy resin. The glass transition temperature exceeds 240 DEG C, and the composite material has relatively excellent temperature resistance, excellent moisture resistance and extremely low water absorption rate.

Description

Technical Field

[0001] This application relates to the field of electronic packaging materials technology, and in particular to a temperature-resistant multifunctional epoxy resin and its preparation method. Background Technology

[0002] The fabrication of electronic components is the foundation of the electronics industry, and packaging technology is crucial for ensuring the normal operation of these components. As electronic devices evolve towards miniaturization, lightweighting, and high performance, higher demands are placed on packaging technology, driving its continuous development and also promoting the evolution of packaging materials. The market has gradually shifted from being dominated by metal and ceramic packaging materials to plastic packaging. Among these, epoxy molding compounds, with their high reliability, low cost, and simple processing, occupy more than 97% of the microelectronic packaging material market and are widely used in various packaging fields such as semiconductor devices, integrated circuits, consumer electronics, automobiles, aerospace, and military applications.

[0003] Epoxy molding compounds are composed of epoxy resin, various fillers, and various additives. Their function is to strengthen the overall integrity of electronic devices, improve their resistance to external impacts and vibrations, enhance the insulation between internal components and circuits, facilitate device miniaturization and weight reduction, prevent direct exposure of components and circuits, and improve the waterproof and moisture-proof performance of devices. Among these, epoxy resin, as the base material of the encapsulation material, is the core that determines the performance of the encapsulation material.

[0004] With the development of the electronics industry, the performance requirements for various electronic components are becoming increasingly stringent; correspondingly, the operating temperatures of these components are also rising. Many existing electronic components, such as common industrial chips and computer processors, operate at relatively high temperatures. The insufficient high-temperature resistance of epoxy resin materials is a major drawback as an encapsulation material for electronic components. Existing research indicates that increasing the crosslinking density of epoxy resin can effectively raise its glass transition temperature, thereby improving its high-temperature resistance. However, increasing the crosslinking density also increases the hygroscopicity of the epoxy resin, leading to insufficient moisture resistance. This can cause problems such as cracking and delamination in encapsulated electronic components under high-temperature operating conditions, and in severe cases, even short circuits.

[0005] Therefore, designing an epoxy resin material with relatively superior high-temperature resistance and excellent moisture resistance is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0006] To address at least one of the aforementioned technical problems, and to develop an epoxy resin material with a glass transition temperature exceeding 240°C, relatively excellent temperature resistance, excellent moisture resistance, and extremely low water absorption, this application provides a temperature-resistant multifunctional epoxy resin and its preparation method.

[0007] On one hand, this application provides a heat-resistant multifunctional epoxy resin, wherein the mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin includes: 100 parts of AFG-90 multifunctional epoxy resin, 20-40 parts of epoxy-terminated polyphenylene ether, 8-16 parts of epoxy-modified silicone oil, and 6-12 parts of hydrophobic fumed silica.

[0008] Optionally, the mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin includes: 100 parts of AFG-90 multifunctional epoxy resin, 24-28 parts of epoxy-terminated polyphenylene ether, 10-12 parts of epoxy-modified silicone oil, and 8-10 parts of hydrophobic fumed silica.

[0009] Optionally, the preparation of the epoxy-terminated polyphenylene ether includes the following steps: S1-a. Dihydroxy-terminated polyphenylene ether and epichlorohydrin are mixed in a mass ratio of 10:6.8~7.2, toluene is added to dissolve them, and then quaternary ammonium salt, sodium hydroxide and 15-crown ether-5 catalyst are added to prepare a reaction solution. S1-b: The reaction solution prepared in step S1-a is reacted at 70~75℃ for more than 3 hours under nitrogen protection, allowed to stand and cool to room temperature, and then filtered through a nanofiltration membrane to obtain the filtrate. S1-c: The filtrate obtained in step S1-b is subjected to vacuum distillation at 100~105℃ to remove the 15-crown ether-5 catalyst, and then added to methanol for crystallization. After filtering out the crystals, the solution is washed with water and dried to obtain epoxy-terminated polyphenylene ether.

[0010] Further optionally, in step S1-a, the amount of quaternary ammonium salt added accounts for 3-5% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin.

[0011] Further optionally, in step S1-a, the amount of sodium hydroxide added accounts for 8-10% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin.

[0012] Further optionally, in step S1-a, the amount of 15-crown ether-5 catalyst added accounts for 2-4% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin.

[0013] Optionally, in step S1-b, after nanofiltration, the filtrate needs to be dechlorinated by a bimetallic oxide of calcium oxide and aluminum oxide.

[0014] Optionally, the preparation of the epoxy-modified silicone oil includes the following steps: S2-a. Mix 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane at a molar ratio of not less than 2.1:1, add Ashby's catalyst, and prepare a reaction solution. S2-b: The reaction solution prepared in step S2-a is pre-reacted at 60~65℃ for more than 1 hour, and then the temperature is raised to 90~95℃ for more than 4.5 hours to obtain a reaction mixture. S2-c: The reaction mixture obtained in step S2-b is decolorized with activated carbon, then filtered to remove the activated carbon, and unreacted 4-vinylphenyl glycidyl ether is removed by vacuum distillation at 120~125℃ to obtain epoxy-modified silicone oil.

[0015] Further optionally, in step S2-a, the molar ratio of 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane is 2.2~2.4:1.

[0016] On the other hand, this application provides a method for preparing the above-mentioned heat-resistant multifunctional epoxy resin, comprising the following steps: S1. Preparation of epoxy-terminated polyphenylene ether; S2. Preparation of epoxy-modified silicone oil; S3. Weigh each component raw material precisely according to the formula, mix them and place them in a vacuum drying oven, cure at 95~105℃ for more than 1.5 hours to obtain a heat-resistant multifunctional epoxy resin.

[0017] In summary, the present invention has at least one of the following beneficial technical effects: 1. This application uses AFG-90 multifunctional epoxy resin as the main raw material, and adds a certain amount of epoxy-terminated polyphenylene ether and epoxy-modified silicone oil. Based on the different molecular weights of epoxy-terminated polyphenylene ether and epoxy-modified silicone oil, the crosslinking density of the epoxy resin can be effectively increased, thereby effectively improving the temperature resistance of the epoxy resin. In addition, this application introduces polyphenylene ether functional groups and specific organosilicon functional groups into the resin. The introduction of these functional groups can not only effectively improve the toughness and impact strength of the epoxy resin, but also effectively change the molecular structure of the epoxy resin. The introduction of many functional groups can effectively increase the glass transition temperature of the epoxy resin after curing.

[0018] 2. This application adds hydrophobic fumed silica to the epoxy resin system. In addition to acting as a filler and auxiliary agent, it can also introduce siloxane groups into the system, further increasing the glass transition temperature of the epoxy resin after curing.

[0019] 3. The epoxy resin of this application incorporates polyphenylene ether and organosilicon functional groups. While significantly improving the temperature resistance of the epoxy resin, the introduction of the above functional groups can greatly improve the hydrophobicity of the epoxy resin, thereby effectively reducing the moisture absorption rate of the epoxy resin after curing and significantly improving its moisture resistance. Detailed Implementation

[0020] The present application will be further described in detail below with reference to the embodiments.

[0021] This application provides a heat-resistant multifunctional epoxy resin, wherein the mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin includes: 100 parts of AFG-90 multifunctional epoxy resin, 20-40 parts of epoxy-terminated polyphenylene ether, 8-16 parts of epoxy-modified silicone oil, and 6-12 parts of hydrophobic fumed silica.

[0022] The preparation method of the above-mentioned heat-resistant multifunctional epoxy resin includes the following steps: S1. Preparation of epoxy-terminated polyphenylene ether; S2. Preparation of epoxy-modified silicone oil; S3. Weigh each component raw material precisely according to the formula, mix them and place them in a vacuum drying oven, cure at 95~105℃ for more than 1.5 hours to obtain a heat-resistant multifunctional epoxy resin.

[0023] Prior to this application, the heat-resistant epoxy resins prepared in the prior art were mainly polyphenolic functional group epoxy resins. The crosslinking density of the cured resin was increased by using multiple functional groups. The polyphenolic functional groups introduced a large number of benzene ring groups, which can effectively increase the glass transition temperature of the epoxy resin, thereby ensuring that it has better heat resistance.

[0024] However, the existing heat-resistant epoxy resins mentioned above lack sufficient high-temperature moisture resistance and exhibit some hygroscopicity at high temperatures, making them prone to various problems when used as epoxy encapsulation materials for electronic components. Although improving the curing agent can enhance its moisture resistance to some extent, the effect is limited and significantly increases the difficulty of the curing process.

[0025] The applicant designed a specific epoxy resin raw material ratio and introduced several new functional groups into the epoxy raw material, effectively solving the problems existing in the prior art.

[0026] The following are preparation examples and embodiments of this application.

[0027] The main raw materials used in the embodiments of this application are all commercially available.

[0028] Among them, the multifunctional epoxy resin, model AFG-90, was purchased from Shanghai Huayi Resin Co., Ltd.; hydrogen-terminated polydimethylsiloxane, purity 99%, was purchased from Hubei Shixing Chemical Co., Ltd.; 4-vinylphenyl glycidyl ether, purity 98%, was purchased from Wuhan Huahandingcheng New Material Technology Co., Ltd.; Ashby's catalyst, model PT-5000YC / PT-5000V, was purchased from Guangzhou Siyou New Material Technology Co., Ltd.; dihydroxyl-terminated polyphenylene ether, SABIC SA90, number average molecular weight 1700, was purchased from Dongguan Jin Granules Plastic Raw Material Co., Ltd.; epichlorohydrin, Jinan Chuangshi Chemical Co., Ltd.; 15-crown ether-5 catalyst, was purchased from Wuhan Jixin Yibang Biotechnology Co., Ltd.; and DDS curing agent, was purchased from Shenzhen Huiya New Material Technology Co., Ltd.

[0029] The following is a preparation example of this application.

[0030] Preparation Example 1 The preparation of the epoxy-terminated polyphenylene ether in this example includes the following steps: S1-a. Dihydroxy-terminated polyphenylene ether and epichlorohydrin are mixed in a mass ratio of 10:6.8. Toluene is added until the mixture is just completely dissolved. Then, 3% tetrabutylammonium bromide, 8% sodium hydroxide and 2% 15-crown ether-5 catalyst, which are the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin, are added to prepare a reaction solution. S1-b: The reaction solution prepared in step S1-a is reacted at 70~75℃ for 3 hours under nitrogen protection. After standing and cooling to room temperature, it is filtered through a nanofiltration membrane. Then, calcium oxide and aluminum oxide bimetallic oxide with a mass ratio of 3:1 and accounting for 200% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin are added. The solution is dechlorinated by applying 220V AC power for 5 minutes. The bimetallic oxide is then filtered out to obtain the filtrate. S1-c: The filtrate obtained in step S1-b is subjected to vacuum distillation at 100~105℃ to remove the 15-crown ether-5 catalyst, and then added to an equal volume of methanol and allowed to stand and cool to crystallize until no new crystals are formed. After filtering out the crystals, the solution is washed with water and vacuum dried to obtain epoxy-terminated polyphenylene ether.

[0031] Preparation Example 2 The preparation of the epoxy-terminated polyphenylene ether in this example includes the following steps: S1-a. Dihydroxy-terminated polyphenylene ether and epichlorohydrin are mixed in a mass ratio of 10:7, dissolved in toluene, and then tetrabutylammonium hydrogen sulfate (4% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin), sodium hydroxide (9% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin), and 15-crown ether-5 catalyst (3% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin) are added to prepare a reaction solution. S1-b: The reaction solution prepared in step S1-a is reacted at 70~75℃ for 3 hours under nitrogen protection. After standing and cooling to room temperature, it is filtered through a nanofiltration membrane. Then, calcium oxide and aluminum oxide bimetallic oxide with a mass ratio of 3:1 and accounting for 200% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin are added. The solution is dechlorinated by applying 220V AC power for 5 minutes. The bimetallic oxide is then filtered out to obtain the filtrate. S1-c: The filtrate obtained in step S1-b is subjected to vacuum distillation at 100~105℃ to remove the 15-crown ether-5 catalyst, and then added to an equal volume of methanol and allowed to stand and cool to crystallize until no new crystals are formed. After filtering out the crystals, the solution is washed with water and vacuum dried to obtain epoxy-terminated polyphenylene ether.

[0032] Preparation Example 3 The preparation of the epoxy-terminated polyphenylene ether in this example includes the following steps: S1-a. Dihydroxy-terminated polyphenylene ether and epichlorohydrin are mixed in a mass ratio of 10:7.2, dissolved in toluene, and then 5% triethylammonium chloride, 10% sodium hydroxide and 4% 15-crown ether-5 catalyst (based on the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin) are added to prepare a reaction solution. S1-b: The reaction solution prepared in step S1-a is reacted at 70~75℃ for 3 hours under nitrogen protection. After standing and cooling to room temperature, it is filtered through a nanofiltration membrane. Then, calcium oxide and aluminum oxide bimetallic oxide with a mass ratio of 3:1 and accounting for 200% of the total mass of dihydroxy-terminated polyphenylene ether and epichlorohydrin are added. The solution is dechlorinated by applying 220V AC power for 5 minutes. The bimetallic oxide is then filtered out to obtain the filtrate. S1-c: The filtrate obtained in step S1-b is subjected to vacuum distillation at 100~105℃ to remove the 15-crown ether-5 catalyst, and then added to an equal volume of methanol and allowed to stand and cool to crystallize until no new crystals are formed. After filtering out the crystals, the solution is washed with water and vacuum dried to obtain epoxy-terminated polyphenylene ether.

[0033] Preparation Example 4 The preparation of the epoxy-modified silicone oil in this example includes the following steps: S2-a. Mix 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane in a molar ratio of 2.1:1, and add Ashby's catalyst accounting for 2.5% of the total mass of 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane to prepare a reaction solution. S2-b: The reaction solution prepared in step S2-a is pre-reacted at 60~65℃ for 1h, and then the temperature is raised to 90~95℃ for 4.5h to obtain a reaction mixture. S2-c: The reaction mixture obtained in step S2-b is decolorized with activated carbon, then filtered to remove the activated carbon, and unreacted 4-vinylphenyl glycidyl ether is removed by vacuum distillation at 120~125℃ to obtain epoxy-modified silicone oil.

[0034] Preparation Example 5 The preparation of the epoxy-modified silicone oil in this example includes the following steps: S2-a. Mix 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane in a molar ratio of 2.2:1, and add Ashby's catalyst accounting for 2.5% of the total mass of 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane to prepare a reaction solution. S2-b: The reaction solution prepared in step S2-a is pre-reacted at 60~65℃ for 1.5h, and then the temperature is raised to 90~95℃ for 5h to obtain a reaction mixture. S2-c: The reaction mixture obtained in step S2-b is decolorized with activated carbon, then filtered to remove the activated carbon, and unreacted 4-vinylphenyl glycidyl ether is removed by vacuum distillation at 120~125℃ to obtain epoxy-modified silicone oil.

[0035] Preparation Example 6 The preparation of the epoxy-modified silicone oil in this example includes the following steps: S2-a. Mix 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane in a molar ratio of 2.4:1, add Ashby's catalyst accounting for 2.5% of the total mass of 4-vinylphenyl glycidyl ether and hydrogen-terminated polydimethylsiloxane, and prepare a reaction solution. S2-b: The reaction solution prepared in step S2-a is pre-reacted at 60~65℃ for 1.5h, and then the temperature is raised to 90~95℃ for 5.5h to obtain a reaction mixture. S2-c: The reaction mixture obtained in step S2-b is decolorized with activated carbon, then filtered to remove the activated carbon, and unreacted 4-vinylphenyl glycidyl ether is removed by vacuum distillation at 120~125℃ to obtain epoxy-modified silicone oil.

[0036] The following are embodiments of this application.

[0037] The method for preparing the heat-resistant multifunctional epoxy resin according to the embodiments of this application includes the following steps: S1. Select the epoxy-terminated polyphenylene ether corresponding to the preparation example; S2. Select the epoxy-modified silicone oil corresponding to the preparation example; S3. Weigh each component raw material precisely according to the formula, mix them and place them in a vacuum drying oven, cure at 95~105℃ for 1.5h to obtain a heat-resistant multifunctional epoxy resin. Example 1

[0038] The mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin in this embodiment includes: 100 parts of AFG-90 multifunctional epoxy resin, 20 parts of epoxy-terminated polyphenylene ether, 8 parts of epoxy-modified silicone oil, and 6 parts of hydrophobic fumed silica.

[0039] In this embodiment, the epoxy-terminated polyphenylene ether of Preparation Example 1 and the epoxy-modified silicone oil of Preparation Example 4 were selected. Example 2

[0040] The mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin in this embodiment includes: 100 parts of AFG-90 multifunctional epoxy resin, 40 parts of epoxy-terminated polyphenylene ether, 16 parts of epoxy-modified silicone oil, and 12 parts of hydrophobic fumed silica.

[0041] In this embodiment, the epoxy-terminated polyphenylene ether of Preparation Example 1 and the epoxy-modified silicone oil of Preparation Example 4 were selected. Example 3

[0042] The mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin in this embodiment includes: 100 parts of AFG-90 multifunctional epoxy resin, 24 parts of epoxy-terminated polyphenylene ether, 10 parts of epoxy-modified silicone oil, and 8 parts of hydrophobic fumed silica.

[0043] In this embodiment, the epoxy-terminated polyphenylene ether of Preparation Example 1 and the epoxy-modified silicone oil of Preparation Example 4 were selected. Example 4

[0044] The mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin in this embodiment includes: 100 parts of AFG-90 multifunctional epoxy resin, 28 parts of epoxy-terminated polyphenylene ether, 12 parts of epoxy-modified silicone oil, and 10 parts of hydrophobic fumed silica.

[0045] In this embodiment, the epoxy-terminated polyphenylene ether of Preparation Example 1 and the epoxy-modified silicone oil of Preparation Example 4 were selected. Example 5

[0046] The mass ratio of each raw material component of the heat-resistant multifunctional epoxy resin in this embodiment includes: 100 parts of AFG-90 multifunctional epoxy resin, 26 parts of epoxy-terminated polyphenylene ether, 11 parts of epoxy-modified silicone oil, and 9 parts of hydrophobic fumed silica.

[0047] In this embodiment, the epoxy-terminated polyphenylene ether of Preparation Example 1 and the epoxy-modified silicone oil of Preparation Example 4 were selected. Example 6

[0048] The difference between this embodiment and Example 5 is that this embodiment uses the epoxy-terminated polyphenylene ether from Preparation Example 2 and the epoxy-modified silicone oil from Preparation Example 5. Example 7

[0049] The difference between this embodiment and Example 5 is that this embodiment selects the epoxy-terminated polyphenylene ether of Preparation Example 3 and the epoxy-modified silicone oil of Preparation Example 6. Example 8

[0050] The difference between this embodiment and Example 5 is that this embodiment selects the epoxy-terminated polyphenylene ether from Preparation Example 2 and the epoxy-modified silicone oil from Preparation Example 6.

[0051] Comparative Example 1 EPPN-501 multifunctional epoxy resin from Nippon Kayaku Co., Ltd. was selected as Comparative Example 1.

[0052] Comparative Example 2 The difference between this comparative example and Example 8 is that hydrophobic fumed silica was not added.

[0053] Comparative Example 3 The difference between this comparative example and Example 8 is that an equal amount of AFG-90 multifunctional epoxy resin is used to replace the epoxy-terminated polyphenylene ether.

[0054] Comparative Example 4 The difference between this comparative example and Example 8 is that the epoxy-modified silicone oil is replaced with an equal amount of AFG-90 multifunctional epoxy resin.

[0055] The cured properties of the products from Examples 1-8 and Comparative Examples 1-4 were tested. DDS curing agent was used, with a resin-to-curing agent mass ratio of 100:55. The curing conditions were: 130℃ / 2h + 150℃ / 2h + 180℃ / 2h + 200℃ / 2h.

[0056] Tensile strength and impact strength were tested according to the methods described in GB / T 2567-2008; The glass transition temperature was tested according to the method described in GB / T 194667.2-2004; The moisture absorption rate was tested according to the method described in GB / T 1034-1998.

[0057] The results are shown in Table 1 below.

[0058] Table 1. Performance test results of Examples 1-8 and Comparative Examples 1-4 after curing. Tensile strength (MPa) <![CDATA[Impact strength (kJ / m 2 )]]> Glass transition temperature (°C) Moisture absorption rate (%) Example 1 94 55.8 249 0.18 Example 2 97 57.4 252 0.16 Example 3 103 57.9 258 0.12 Example 4 102 57.8 259 0.11 Example 5 105 58.1 261 0.10 Example 6 107 58.4 264 0.09 Example 7 108 58.7 265 0.08 Example 8 108 58.9 268 0.06 Comparative Example 1 92 50.2 238 2.92 Comparative Example 2 99 53.7 236 1.22 Comparative Example 3 87 49.6 217 2.38 Comparative Example 4 91 50.9 224 1.94 As can be seen from the data in Table 1, the epoxy resins prepared in Examples 1-8 of this application, after curing with the curing agent, have a glass transition temperature that is more than 10°C higher than that of the epoxy resin cured in Comparative Example 1, which is used in the prior art. Their temperature resistance is superior to that of existing multifunctional epoxy resins, their mechanical properties are also significantly better than those of the epoxy resin in Comparative Example 1, and their moisture absorption rate is significantly lower than that of the epoxy resin in Comparative Example 1. It is evident that the epoxy resins of this application have excellent temperature resistance and moisture resistance, and their performance is superb.

[0059] The data in Table 1, comparing the data of Examples 1 to 8, shows that after adjusting the raw material ratio, the various properties of the cured epoxy resin can be further improved. In addition, the epoxy resin of Example 8 has the best performance after curing, indicating that the higher the purity of the raw materials and the lower the impurity content, the better the performance of the resin.

[0060] As can be seen from the data in Table 1, comparing the data of Example 8 with those of Comparative Examples 2-4, the introduction of polyphenylene ether, organosilicon, and siloxy groups into this application allows the resin to possess both temperature resistance and moisture resistance. The absence of any one of these functional groups would disrupt the crosslinking system and functional group system designed in this application, resulting in a significant decrease in the resin's performance.

[0061] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A temperature resistant multifunctional epoxy resin, characterized by comprising: The mass ratio of each raw material component of the temperature-resistant multifunctional epoxy resin includes: 100 parts of AFG-90 multifunctional epoxy resin, 20-40 parts of epoxy-terminated polyphenyl ether, 8-16 parts of epoxy-modified silicone oil, and 6-12 parts of hydrophobic fumed silica.

2. The temperature-resistant multifunctional epoxy resin according to claim 1, characterized by, The mass ratio of each raw material component of the temperature-resistant multifunctional epoxy resin includes: 100 parts of AFG-90 multifunctional epoxy resin, 24-28 parts of epoxy-terminated polyphenyl ether, 10-12 parts of epoxy-modified silicone oil, and 8-10 parts of hydrophobic fumed silica.

3. The temperature resistant multifunctional epoxy resin according to claim 1, wherein The preparation of the epoxy-terminated polyphenyl ether includes the following steps: S1-a, mix the dihydroxyl-terminated polyphenyl ether and the epichlorohydrin at a mass ratio of 10:6.8-7.2, add toluene for dissolution, and then add the quaternary ammonium salt, sodium hydroxide and 15-crown-5 catalyst to prepare a reaction solution; S1-b, the reaction solution prepared in step S1-a is reacted at 70-75 DEG C for more than 3 hours under nitrogen protection, cooled to room temperature, filtered by nanofiltration membrane to obtain a filtrate; S1-c, the filtrate obtained in step S1-b is distilled at 100-105 DEG C under reduced pressure to remove the 15-crown-5 catalyst, and then added to methanol for crystallization, filtered to remove the crystals, washed with water and dried to obtain the epoxy-terminated polyphenyl ether.

4. The temperature resistant multifunctional epoxy resin according to claim 3, wherein In step S1-a, the amount of the quaternary ammonium salt added accounts for 3-5% of the total mass of the dihydroxyl-terminated polyphenyl ether and the epichlorohydrin.

5. The temperature resistant multifunctional epoxy resin according to claim 3, wherein In step S1-a, the amount of sodium hydroxide added accounts for 8-10% of the total mass of the dihydroxyl-terminated polyphenyl ether and the epichlorohydrin.

6. The temperature resistant multifunctional epoxy resin according to claim 3, wherein In step S1-a, the amount of 15-crown-5 catalyst added accounts for 2-4% of the total mass of the dihydroxyl-terminated polyphenyl ether and the epichlorohydrin.

7. The temperature resistant multifunctional epoxy resin according to claim 3, wherein In step S1-b, the filtrate after nanofiltration membrane filtration needs to be treated by double metal oxide dechlorination of calcium oxide and aluminum oxide.

8. The temperature resistant multifunctional epoxy resin according to claim 1, wherein The preparation of the epoxy-modified silicone oil includes the following steps: S2-a, mix the 4-vinylphenyl glycidyl ether and the hydrogen-terminated polydimethylsiloxane according to a molar ratio of not less than 2.1:1, add Ashby's catalyst to prepare a reaction solution; S2-b, the reaction solution prepared in step S2-a is pre-reacted at 60-65 DEG C for more than 1 hour, and then heated to 90-95 DEG C for reaction for more than 4.5 hours to obtain a reaction mixture; S2-c, the reaction mixture obtained in step S2-b is subjected to decolorization treatment by activated carbon, and then filtered to remove the activated carbon, and the unreacted 4-vinylphenyl glycidyl ether is removed by distillation at 120-125 DEG C under reduced pressure to obtain the epoxy-modified silicone oil.

9. The temperature resistant multifunctional epoxy resin according to claim 8, wherein In step S2-a, the molar ratio of the 4-vinylphenyl glycidyl ether and the hydrogen-terminated polydimethylsiloxane is 2.2-2.4:

1.

10. A method of preparing the temperature resistant multifunctional epoxy resin of claim 1, characterized by, The preparation includes the following steps: S1, preparing the epoxy-terminated polyphenyl ether; S2, preparing the epoxy-modified silicone oil; S3, accurately weighing each component raw material according to the ratio, mixing, and then placing in a vacuum drying oven for curing reaction at 95-105 DEG C for more than 1.5 hours to obtain the temperature-resistant multifunctional epoxy resin.