CN103087665B - High-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and preparation method thereof - Google Patents
High-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and a preparation method thereof. The pouring sealant comprises a component A and a component B, wherein the component A is prepared by blending an epoxy resin, a reactive diluent, an antifoaming agent and an inorganic heat conductivity filler which is treated by a silane coupling agent; and the component B is a curing agent. According to the pouring sealant, aluminum oxide and zinc oxide are adopted to provide high heat conductivity and insulation properties, the heat conductivity coefficient can be 1.75-2.23W.m.K, the volume resistivity is 3.25-5.91*10<15>omega/cm, the viscosity of the pouring sealant is greatly reduced by adopting the reactive diluent containing a plurality of active end groups, and the viscosity of the pouring sealant is 19,800-29,800mPa.s (25 DEG C), so that the pouring sealant is beneficial for pouring; and by using a modified acid anhydride as the curing agent, the operable time of the pouring sealant at 25 DEG C can be more than 8h.
Description
Technical field
The present invention relates to a kind of High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant and preparation method thereof, belong to polymer composite Application Areas.
Background technology
Epoxy resin (EP) has good physical and chemical performance, excellent bonding strength, good dielectric properties; And cure shrinkage is little, product size good stability, hardness is high, and snappiness is better, to alkali and most of solvent-stable, is widely used in national defence, each department of national economy.
Along with the development of microelectronics and large-scale integrated circuit, circuit components high concentration, the heat radiation of components and parts becomes distinct issues.Common epoxy resin embedding adhesive because of heat conductivility poor, cannot meet the cooling requirements of some occasion, the epoxy resin embedding adhesive researching and developing high heat conduction is very necessary, generally takes the method for filling conducting filler in epoxy resin to improve its heat conductivility.
The thermal conductivity of the epoxy casting material that patent CN102515626A takes filling aluminum oxide, aluminium nitride, the inorganic heat conductive filler of boron nitride to obtain is 1.1 ~ 1.3W/ (m.K), still can not meet the radiating requirements of some large-scale integrated circuit.Patent CN101974302A takes to fill ball-aluminium oxide to improve the thermal conductivity of epoxy resin, and the thermal conductivity of joint sealant reaches 1.2 ~ 1.8 W/ (m.K), but the cost of the ball-aluminium oxide used is high.Heat-conduction epoxy resin joint sealant also exists that the fast operable time of gel is short in addition, the shortcoming of viscosity greatly not easily embedding.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, propose a kind of good heat conductivity, viscosity is little, gel is slow, High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant that operable time is longer and preparation method thereof.
High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant of the present invention, comprises component A and B component that mass ratio is 100: 5 ~ 8; The quality group of described A component becomes: epoxy resin 100 parts, reactive thinner 20 ~ 30 parts, defoamer 2 ~ 3 parts, through the inorganic heat conductive filler of silane coupling agent surface-treated 1000 ~ 1300 parts, described inorganic heat conductive filler is aluminum oxide and/or zinc oxide; Described B component is modified anhydride solidifying agent.
Described epoxy resin is preferably E-51 type epoxy resin.
Described reactive thinner is preferably at least one in Isosorbide-5-Nitrae-hexanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether and 1,2-cylohexanediol diglycidyl ether.
Described defoamer is preferably at least one in polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxypropylene amidogen ether and polyoxyethylene polyoxypropylene glyceryl ether.
Described silane coupling agent is preferably at least one in glycidyl ether oxygen propyl trimethoxy silicane, 3-aminopropyl triethoxysilane and dodecyltrimethoxysilane.
Described modified anhydride solidifying agent is preferably 1-methyl hexahydrophthalic anhydride or 4-methyl tetrahydro phthalic anhydride.
Described inorganic heat conductive filler is preferably the composition of aluminum oxide and zinc oxide, and the two mass ratio is 3:1 ~ 4:1, and described aluminum oxide median size is preferably 4 ~ 6 μm; Described zinc oxide median size is preferably 1 ~ 3 μm, is preferably 2 μm.
Described aluminum oxide is preferably the composition that median size is the aluminum oxide of 6 μm and median size 4 μm, and the two mass ratio is 3:2 ~ 5:3.
The preparation method of High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant of the present invention, comprises the steps:
(1) 100 parts of inorganic heat conductive fillers are taken in 100 DEG C of dry 2h by mass parts; Get 1 part of silane coupling agent, 3 parts of dehydrated alcohols and 0.33 part of distilled water By Hydrolysis At Room Temperature 20min; 110 DEG C of high-speed mixing 30min in high-speed mixer by the hydrolyzed solution of silane coupling agent and dried inorganic heat conductive filler, take out mixture, 120 DEG C of dry 2h, namely obtain through the inorganic heat conductive filler of silane coupling agent surface-treated;
(2) take epoxy resin, reactive thinner and defoamer and stir 20 ~ 30min in high speed dispersor; Add through the inorganic heat conductive filler of silane coupling agent surface-treated again, continue stirring 20 ~ 40min after reinforced and namely obtain component A;
(3) component A is taken with B component and after mixing, namely vacuum defoamation obtains High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant.
The present invention utilizes aluminum oxide, zinc oxide provides high heat conduction and insulating property, and thermal conductivity can reach 1.75 ~ 2.23W/m.K, and volume specific resistance is 3.25 ~ 5.91 × 10
15Ω/cm; Adopt the reactive thinner containing multiple active end group significantly to reduce the viscosity of joint sealant, joint sealant viscosity is at 19800 ~ 29800mPa.s(25 DEG C), be beneficial to embedding, take modified anhydride as solidifying agent, when 25 DEG C, the operable time of joint sealant reaches more than 8h.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be appreciated that, these embodiments only for illustration of the present invention, and are not intended to limit the scope of the invention.The improvement made according to the present invention of technician and adjustment, still belong to protection scope of the present invention in actual applications.If no special instructions, in embodiment number all by mass parts.
embodiment 1
Take 100 parts of E-51 type epoxy resin, 23 part 1,4-hexanediol diglycidyl ether, 2.5 parts of polyoxyethylene polyoxypropylene tetramethylolmethane ethers stir 20min in high speed dispersor, add the inorganic heat conductive filler through glycidyl ether oxygen propyl trimethoxy silicane process successively: the zinc oxide of the aluminum oxide of the aluminum oxide of 450 parts of median sizes 6 μm, 300 parts of median sizes 4 μm, 250 parts of median sizes 2 μm, reinforced complete continuations stirring 20min obtains component A.
Take 100 parts of component A to mix with 7.1 parts of 1-methyl hexahydrophthalic anhydride solidifying agent, vacuum defoamation 30min, the viscosity of joint sealant is 20800mPa.s(25 DEG C); Joint sealant 100 DEG C solidification 3h, thermal conductivity is 1.76 W/m.K, and volume specific resistance is 5.43 × 10
15Ω/cm.
embodiment 2
Take 100 parts of E-51 type epoxy resin, 27 part 1,6-hexanediol diglycidyl ether, 2.7 parts of polyoxyethylene polyoxypropylene glyceryl ethers stir 25min in high speed dispersor, add the inorganic heat conductive filler through the process of 3-aminopropyl triethoxysilane successively: the zinc oxide of the aluminum oxide of the aluminum oxide of 495 parts of median sizes 6 μm, 330 parts of median sizes 4 μm, 275 parts of median sizes 2 μm, reinforced complete continuations stirring 25min obtains component A.
Take 100 parts of component A to mix with 6.4 parts of 4-methyl tetrahydro phthalic anhydride solidifying agent, vacuum defoamation 30min, the viscosity of joint sealant is 24500mPa.s(25 DEG C); Joint sealant 100 DEG C solidification 3h, thermal conductivity is 1.93 W/m.K, and volume specific resistance is 4.12 × 10
15Ω/cm.
embodiment 3
Take 100 parts of E-51 type epoxy resin, 29 part 1,2-cylohexanediol diglycidyl ether, 2.9 parts of polyoxyethylene polyoxypropylene amidogen ethers stir 20min in high speed dispersor, add the inorganic heat conductive filler through dodecyltrimethoxysilane process successively: the zinc oxide of the aluminum oxide of the aluminum oxide of 585 parts of median sizes 6 μm, 390 parts of median sizes 4 μm, 325 parts of median sizes 2 μm, reinforced complete continuations stirring 25min obtains component A.
Take 100 parts of component A to mix with 5.6 parts of 1-methyl hexahydrophthalic anhydride solidifying agent, vacuum defoamation 30min, the viscosity of joint sealant is 29800mPa.s(25 DEG C); Joint sealant 100 DEG C solidification 3h, thermal conductivity is 2.22 W/m.K, and volume specific resistance is 3.47 × 10
15Ω/cm.
Claims (7)
1. a High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant, is characterized in that, comprises component A and B component that mass ratio is 100: 5 ~ 8; The quality group of described A component becomes: epoxy resin 100 parts, reactive thinner 20 ~ 30 parts, defoamer 2 ~ 3 parts, through the inorganic heat conductive filler of silane coupling agent surface-treated 1000 ~ 1300 parts, described inorganic heat conductive filler is the composition of aluminum oxide and zinc oxide, and the two mass ratio is 3:1 ~ 4:1; Described aluminum oxide median size is 4 ~ 6 μm; Described zinc oxide median size is 1 ~ 3 μm; Described silane coupling agent is at least one in glycidyl ether oxygen propyl trimethoxy silicane, 3-aminopropyl triethoxysilane and dodecyltrimethoxysilane; Described B component is modified anhydride solidifying agent.
2. High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to claim 1, it is characterized in that, described epoxy resin is E-51 type epoxy resin.
3. High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to claim 1, it is characterized in that, described reactive thinner is Isosorbide-5-Nitrae-hexanediol diglycidyl ether, 1, at least one in 6-hexanediol diglycidyl ether and 1,2-cylohexanediol diglycidyl ether.
4. High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to claim 1, it is characterized in that, described defoamer is at least one in polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxypropylene amidogen ether and polyoxyethylene polyoxypropylene glyceryl ether.
5. High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to claim 1, it is characterized in that, described modified anhydride solidifying agent is 1-methyl hexahydrophthalic anhydride or 4-methyl tetrahydro phthalic anhydride.
6. High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to claim 1, is characterized in that, described aluminum oxide is the composition of the aluminum oxide of median size 6 μm and median size 4 μm, and the two mass ratio is 3:2 ~ 5:3.
7. the preparation method of High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant according to any one of claim 1 ~ 6, is characterized in that, comprise the steps:
(1) 100 parts of inorganic heat conductive fillers are taken in 100 DEG C of dry 2h by mass parts; Get 1 part of silane coupling agent, 3 parts of dehydrated alcohols and 0.33 part of distilled water By Hydrolysis At Room Temperature 20min; 110 DEG C of high-speed mixing 30min in high-speed mixer by the hydrolyzed solution of silane coupling agent and dried inorganic heat conductive filler, take out mixture, 120 DEG C of dry 2h, namely obtain through the inorganic heat conductive filler of silane coupling agent surface-treated;
(2) take epoxy resin, reactive thinner and defoamer and stir 20 ~ 30min in high speed dispersor; Add through the inorganic heat conductive filler of silane coupling agent surface-treated again, continue stirring 20 ~ 40min after reinforced and namely obtain component A;
(3) component A is taken with B component and after mixing, namely vacuum defoamation obtains High-heat-conductiviinsulation insulation low-viscosity epoxy resin joint sealant.
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| CN112126393B (en) * | 2020-09-28 | 2021-07-20 | 杭州应星新材料有限公司 | Phase-change heat storage pouring sealant and preparation method thereof |
| CN113308121B (en) * | 2021-07-14 | 2022-06-07 | 合肥工业大学 | Insulating high-thermal-conductivity gel filled with composite thermal-conductive filler based on chemical bond assembly |
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| CN115595104A (en) * | 2022-10-27 | 2023-01-13 | 佛山清立新材料科技有限公司（Cn） | Epoxy packaging adhesive and preparation method and application thereof |
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