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CN103805127A - High-temperature-resisting epoxy organic silicon pouring sealant and preparation method thereof - Google Patents

High-temperature-resisting epoxy organic silicon pouring sealant and preparation method thereof Download PDF

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CN103805127A
CN103805127A CN201410066556.0A CN201410066556A CN103805127A CN 103805127 A CN103805127 A CN 103805127A CN 201410066556 A CN201410066556 A CN 201410066556A CN 103805127 A CN103805127 A CN 103805127A
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organic silicon
epoxy silicone
epoxy
silicone
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CN103805127B (en
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薛刚
张斌
孙明明
张绪刚
李坚辉
王磊
赵明
宋彩雨
李奇力
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Institute of Petrochemistry of Heilongjiang Academy of Sciences
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Abstract

一种耐高温环氧有机硅灌封胶及其制备方法,它涉及一种灌封胶及其制备方法。本发明的目的是要解决现有灌封胶存在的不能同时兼具韧性好、耐热性高和粘接性好的问题。一种耐高温环氧有机硅灌封胶由环氧有机硅树脂、活性有机硅填料,固化剂、固化促进剂、稀释剂和消泡剂制备而成;制备方法:一、制备环氧有机硅树脂;二、制备活性有机硅填料;三、称取;四、混合。提供了环氧有机硅树脂和活性有机硅填料的制备方法,将制备的环氧有机硅树脂和活性有机硅填料作为本发明的原料,制备的环氧有机硅灌封胶粘度低,浸润性好,固化产物兼具韧性和耐热性,灌封件的质量稳定。本发明可获得一种耐高温环氧有机硅灌封胶。

A high-temperature-resistant epoxy silicone potting glue and a preparation method thereof, which relate to a potting glue and a preparation method thereof. The purpose of the present invention is to solve the problem that the existing potting compound cannot simultaneously have good toughness, high heat resistance and good adhesion. A high temperature resistant epoxy silicone potting adhesive is prepared from epoxy silicone resin, active silicone filler, curing agent, curing accelerator, diluent and defoamer; preparation method: 1. Preparation of epoxy silicone Resin; 2. Preparation of active silicone filler; 3. Weighing; 4. Mixing. The preparation method of epoxy silicone resin and active silicone filler is provided, and the prepared epoxy silicone resin and active silicone filler are used as raw materials of the present invention, and the prepared epoxy silicone potting adhesive has low viscosity and wettability Well, the cured product has both toughness and heat resistance, and the quality of the potting parts is stable. The invention can obtain a high temperature resistant epoxy silicone potting glue.

Description

A kind of fire resistant epoxy organic silicon potting adhesive and preparation method thereof
Technical field
The present invention relates to a kind of joint sealant and preparation method thereof.
Background technology
Epoxy resin, organosilicon and urethane are most widely used three major types in joint sealant.Wherein the feature of epoxy resin encapsulated material be that shrinking percentage is little, no coupling product, good electrical insulation capability, but be subject to the restriction of molecular structure itself, toughness is poor and thermotolerance is not high.The features such as add-on type liquid silicon rubber has no coupling product when crosslinked and discharges, and shrinking percentage is little, and cross-linking density and vulcanization rate are easy to control are also the conventional body materials of joint sealant.But addition-type silicon rubber is because molecule itself is nonpolar, cementability is poor, and while use as Embedding Material, moisture can infiltrate device inside by the space between rubber and base material and cause corrosion and failure of insulation.
Along with the development of technology, the requirement of the performance of every profession and trade to joint sealant is more and more higher, and existing joint sealant exists and can not have good toughness, thermotolerance is high and cementability is good problem simultaneously concurrently.
Summary of the invention
The object of the invention is to solve that existing joint sealant exists can not have good toughness, thermotolerance is high and cementability is good problem concurrently simultaneously, and a kind of fire resistant epoxy organic silicon potting adhesive and preparation method thereof is provided.
A kind of fire resistant epoxy organic silicon potting adhesive is prepared from by 100 parts~150 parts epoxy silicone resins, 10 parts~55 parts active organosilicon fillers, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers by weight.
A kind of preparation method of fire resistant epoxy organic silicon potting adhesive specifically completes according to the following steps:
One, prepare epoxy silicone resin: take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water, 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents; First 30 parts~80 parts organosilicon sources and 10 parts~40 parts water are mixed, be to react 1h~5h at 50 ℃~100 ℃ in temperature, obtain mixed solution, then under being 70 ℃~100 ℃ and pressure 1kPa~10kPa, temperature removes water in mixed solution and the alcohols material of generation, add again 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents, be to react 2h~4h at 60 ℃~100 ℃ in temperature, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane; Described solvent is one or more the mixed solution in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is one or more the mixture in bisphenol-A type epoxy resin E-44, E-51 and E-54;
Two, prepare active organosilicon filler: take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water and 5 parts~20 parts tetraethoxys; 30 parts~80 parts organosilicon sources and 10 parts~40 parts water that take are mixed, and are to react 1h~5h at 50 ℃~100 ℃ in temperature, naturally cool to 30 ℃~60 ℃, then drip 5 parts~20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h~20h at 20 ℃~30 ℃, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane;
Three, take: the epoxy silicone resin being obtained by 100 parts~150 parts step 1 by weight, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers that step 2 obtains;
Four, mix: the epoxy silicone resin that 100 parts~150 parts step 1 that step 1 is taken obtain, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers mixing that step 2 obtains, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1, the mixture of one or more in 6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether;
Defoamer described in step 3 is the defoamer that model that German Di Gao company produces is airex940.
Advantage of the present invention: the preparation method who, the invention provides epoxy silicone resin and active organosilicon filler, using preparation epoxy silicone resin and active organosilicon filler as raw material of the present invention, epoxy organosilicon joint sealant viscosity prepared by the present invention is low, wetting property is good, cured product has toughness and thermotolerance concurrently, the steady quality of embedding part, initial decomposition temperature of the present invention is 393 ℃~410 ℃, in the time of 25 ℃, shearing resistance is 23MPa~26MPa; Two, the present invention combines the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence, increase the toughness in epoxy resin by flexible organosilicon segment, the good adhesiveproperties of retaining ring epoxy resins and base material simultaneously, add again active organosilicon filler, prepare and there is excellent toughness, simultaneously the fire resistant epoxy organic silicon potting adhesive of thermotolerance and adhesiveproperties excellence.
The present invention can obtain a kind of fire resistant epoxy organic silicon potting adhesive.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of the epoxy silicone resin that obtains of test one step 1.
Embodiment
Embodiment one: present embodiment is that a kind of fire resistant epoxy organic silicon potting adhesive is prepared from by 100 parts~150 parts epoxy silicone resins, 10 parts~55 parts active organosilicon fillers, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers by weight.
The advantage of present embodiment: one, present embodiment provides the preparation method of epoxy silicone resin and active organosilicon filler, using the epoxy silicone resin of preparation and active organosilicon filler as the raw material of present embodiment, epoxy organosilicon joint sealant viscosity prepared by present embodiment is low, wetting property is good, cured product has toughness and thermotolerance concurrently, the steady quality of embedding part, present embodiment initial decomposition temperature is 393 ℃~410 ℃, in the time of 25 ℃, shearing resistance is 23MPa~26MPa; Two, present embodiment combines the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence, increase the toughness in epoxy resin by flexible organosilicon segment, the good adhesiveproperties of retaining ring epoxy resins and base material simultaneously, add again active organosilicon filler, prepare and there is excellent toughness, simultaneously the fire resistant epoxy organic silicon potting adhesive of thermotolerance and adhesiveproperties excellence.
Present embodiment can obtain a kind of fire resistant epoxy organic silicon potting adhesive.
Embodiment two: present embodiment and embodiment one difference are: described epoxy silicone resin is prepared according to the following steps:
Take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water, 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents; First 30 parts~80 parts organosilicon sources and 10 parts~40 parts water are mixed, be to react 1h~5h at 50 ℃~100 ℃ in temperature, obtain mixed solution, then under being 70 ℃~100 ℃ and pressure 1kPa~10kPa, temperature removes water in mixed solution and the alcohols material of generation, add again 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents, be to react 2h~4h at 60 ℃~100 ℃ in temperature, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane; Described solvent is one or more the mixed solution in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is one or more the mixture in bisphenol-A type epoxy resin E-44, E-51 and E-54.Other steps are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: described active organosilicon filler is specifically prepared according to the following steps:
Take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water and 5 parts~20 parts tetraethoxys; 30 parts~80 parts organosilicon sources and 10 parts~40 parts water that take are mixed, and are to react 1h~5h at 50 ℃~100 ℃ in temperature, naturally cool to 30 ℃~60 ℃, then drip 5 parts~20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h~20h at 20 ℃~30 ℃, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane.Other steps are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: described solidifying agent is 4,4-diaminodiphenyl oxide, 4,4-diaminodiphenylsulfone(DDS), methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methyl carbic anhydride.Other steps are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: described curing catalyst is 2,4,6-tri-(dimethylamino methyl) phenol, Resorcinol, oxine, dimethyl benzylamine, 2-ethyl-4-methylimidazole or glyoxal ethyline.Other steps are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: described thinner is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1, the mixture of one or more in 6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether.Other steps are identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: described defoamer is the defoamer that model that German Di Gao company produces is airex940.Other steps are identical with embodiment one to six.
Embodiment eight: present embodiment is a kind of preparation method of fire resistant epoxy organic silicon potting adhesive, specifically completes according to the following steps:
One, prepare epoxy silicone resin: take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water, 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents; First 30 parts~80 parts organosilicon sources and 10 parts~40 parts water are mixed, be to react 1h~5h at 50 ℃~100 ℃ in temperature, obtain mixed solution, then under being 70 ℃~100 ℃ and pressure 1kPa~10kPa, temperature removes water in mixed solution and the alcohols material of generation, add again 20 parts~100 parts epoxy resin and 40 parts~80 parts solvents, be to react 2h~4h at 60 ℃~100 ℃ in temperature, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane; Described solvent is one or more the mixed solution in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is one or more the mixture in bisphenol-A type epoxy resin E-44, E-51 and E-54;
Two, prepare active organosilicon filler: take by weight 30 parts~80 parts organosilicon sources, 10 parts~40 parts water and 5 parts~20 parts tetraethoxys; 30 parts~80 parts organosilicon sources and 10 parts~40 parts water that take are mixed, and are to react 1h~5h at 50 ℃~100 ℃ in temperature, naturally cool to 30 ℃~60 ℃, then drip 5 parts~20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h~20h at 20 ℃~30 ℃, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is one or more the mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, phenylbenzene diethoxy silane and methyl triacetoxysilane;
Three, take: the epoxy silicone resin being obtained by 100 parts~150 parts step 1 by weight, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers that step 2 obtains;
Four, mix: the epoxy silicone resin that 100 parts~150 parts step 1 that step 1 is taken obtain, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers mixing that step 2 obtains, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1, the mixture of one or more in 6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether;
Defoamer described in step 3 is the defoamer that model that German Di Gao company produces is airex940.
The advantage of present embodiment: one, present embodiment provides the preparation method of epoxy silicone resin and active organosilicon filler, using the epoxy silicone resin of preparation and active organosilicon filler as the raw material of present embodiment, epoxy organosilicon joint sealant viscosity prepared by present embodiment is low, wetting property is good, cured product has toughness and thermotolerance concurrently, the steady quality of embedding part, present embodiment initial decomposition temperature is 393 ℃~410 ℃, in the time of 25 ℃, shearing resistance is 23MPa~26MPa; Two, present embodiment combines the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence, increase the toughness in epoxy resin by flexible organosilicon segment, the good adhesiveproperties of retaining ring epoxy resins and base material simultaneously, add again active organosilicon filler, prepare and there is excellent toughness, simultaneously the fire resistant epoxy organic silicon potting adhesive of thermotolerance and adhesiveproperties excellence.
Present embodiment can obtain a kind of fire resistant epoxy organic silicon potting adhesive.
Embodiment nine: present embodiment and embodiment eight differences are: the curing catalyst described in step 3 is 2,4,6-tri-(dimethylamino methyl) phenol, Resorcinol, oxine, dimethyl benzylamine, 2-ethyl-4-methylimidazole or glyoxal ethyline.Other steps are identical with embodiment eight.
Embodiment ten: one of present embodiment and embodiment eight or nine difference is: the solidifying agent described in step 3 is 4,4-diaminodiphenyl oxide, 4,4-diaminodiphenylsulfone(DDS), methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methyl carbic anhydride.Other steps are identical with embodiment eight or nine.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: a kind of preparation method of fire resistant epoxy organic silicon potting adhesive, specifically completes according to the following steps:
One, prepare epoxy silicone resin: take by weight 50 parts of organosilicon sources, 10 parts of water, 90 parts of epoxy resin and 50 parts of solvents; First 50 parts of organosilicon sources and 10 parts of water are mixed, be to react 5h at 80 ℃ in temperature, obtain mixed solution, then under being 100 ℃ and pressure 1kPa, temperature removes water in mixed solution and the alcohols material of generation, add again 90 parts of epoxy resin and 50 parts of solvents, be to react 2h at 90 ℃ in temperature, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is the mixture of dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane; Described solvent is ethyl acetate; Described epoxy resin is the mixture of bisphenol-A type epoxy resin E-44 and E-51;
Two, prepare active organosilicon filler: take by weight 40 parts of organosilicon sources, 15 parts of water and 5 parts of tetraethoxys; The 40 parts of organosilicon sources and the 15 parts of water that take are mixed, and are to react 5h at 70 ℃ in temperature, naturally cool to 40 ℃, then drip 5 parts of tetraethoxys, obtain gel; By gel vacuum-drying 15h at 25 ℃, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer compositions of mixtures; Described organosilane monomer mixture is the mixture of methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and vinyltriethoxysilane;
Three, take: the epoxy silicone resin being obtained by 100 parts~150 parts step 1 by weight, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers that step 2 obtains;
Four, mix: the epoxy silicone resin that 100 parts~150 parts step 1 that step 1 is taken obtain, 10 parts~55 parts active organosilicon filler, 25 parts~70 parts solidifying agent, 1 part~3 parts curing catalysts, 10 parts~50 parts thinners and 0.5 part~3 parts defoamers mixing that step 2 obtains, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is the mixture of BDDE and ethylene glycol diglycidylether;
Defoamer described in step 3 is the defoamer that model that German Di Gao company produces is airex940;
Curing catalyst described in step 3 is 2,4,6-tri-(dimethylamino methyl) phenol;
Solidifying agent described in step 3 is 4,4-diaminodiphenylsulfone(DDS).
Use infrared spectrometer to test the epoxy silicone resin of testing a step 1 and obtaining, as shown in Figure 1.Fig. 1 is the infrared spectrum of the epoxy silicone resin that obtains of test one step 1, from Fig. 1, at 3462cm -1, 3052cm -1, 1247cm -1, 916cm -1, 1130cm -1and 1035cm -1there is characteristic peak at place, at 3462cm -1for hydroxyl characteristic peak, be 3052cm -1, 1247cm -1, 916cm -1place is epoxide group characteristic peak, 1130cm -1and 1035cm -1place is siloxane bond characteristic peak.
The initial decomposition temperature of this test fire resistant epoxy organic silicon potting adhesive is 393.5 ℃, shearing resistance in the time of 25 ℃ is 24.3MPa, shearing resistance in the time of 250 ℃ is 4.5MPa, and the shearing resistance in the time of 300 ℃ is 2.3MPa, and the shearing resistance in the time of 350 ℃ is 1.1MPa.

Claims (10)

1.一种耐高温环氧有机硅灌封胶,其特征在于一种耐高温环氧有机硅灌封胶按重量份数由100份~150份环氧有机硅树脂、10份~55份活性有机硅填料、25份~70份固化剂、1份~3份固化促进剂、10份~50份稀释剂和0.5份~3份消泡剂制备而成。1. A high-temperature-resistant epoxy silicone potting glue is characterized in that a high-temperature-resistant epoxy silicone potting glue consists of 100 to 150 parts by weight of epoxy silicone resin, 10 to 55 parts of active It is prepared by silicone filler, 25-70 parts of curing agent, 1-3 parts of curing accelerator, 10-50 parts of diluent and 0.5-3 parts of defoamer. 2.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的环氧有机硅树脂是按以下步骤制备的:2. A kind of high temperature resistant epoxy silicone potting glue according to claim 1, characterized in that described epoxy silicone resin is prepared according to the following steps: 按重量份数称取30份~80份有机硅源、10份~40份水、20份~100份环氧树脂和40份~80份溶剂;首先将30份~80份有机硅源和10份~40份水混合,在温度为50℃~100℃下反应1h~5h,得到混合液,然后在温度为70℃~100℃和压力1kPa~10kPa下脱除混合液中的水和生成的醇类物质,再加入20份~100份环氧树脂和40份~80份溶剂,在温度为60℃~100℃下反应2h~4h,减压蒸馏脱除溶剂,得到环氧有机硅树脂;其中,所述的有机硅源为γ-氨丙基三乙氧基硅烷和有机硅单体混合物组成;所述的有机硅单体混合物为二甲基二乙氧基硅烷、甲基三乙氧基硅烷、甲基三乙酰氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、二苯基二乙氧基硅烷和甲基三乙酰氧基硅烷中的一种或几种的混合物;所述的溶剂为甲苯、甲乙酮、乙酸乙酯、乙醇、丙酮、四氢呋喃和二甲苯中的一种或几种的混合液;所述的环氧树脂为双酚-A型环氧树脂E-44、E-51和E-54中的一种或几种的混合物。Weigh 30 to 80 parts of organic silicon source, 10 to 40 parts of water, 20 to 100 parts of epoxy resin and 40 to 80 parts of solvent in parts by weight; first mix 30 to 80 parts of organic silicon source and 10 Mix 1 to 40 parts of water, react at a temperature of 50°C to 100°C for 1h to 5h to obtain a mixed solution, and then remove the water and produced Alcohols, then add 20-100 parts of epoxy resin and 40-80 parts of solvent, react at a temperature of 60°C-100°C for 2h-4h, and distill under reduced pressure to remove the solvent to obtain epoxy silicone resin; Wherein, the organosilicon source is composed of γ-aminopropyltriethoxysilane and organosilicon monomer mixture; the organosilicon monomer mixture is dimethyldiethoxysilane, methyltriethoxy ylsilane, methyltriacetoxysilane, γ-glycidyloxypropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, vinyltriethoxysilane, diphenyl A mixture of one or more of diethoxysilane and methyltriacetoxysilane; the solvent is one or more of toluene, methyl ethyl ketone, ethyl acetate, ethanol, acetone, tetrahydrofuran and xylene The mixed solution of the species; the epoxy resin is one or more mixtures of bisphenol-A epoxy resins E-44, E-51 and E-54. 3.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的活性有机硅填料具体是按以下步骤制备的:3. A high temperature resistant epoxy silicone potting compound according to claim 1, characterized in that the active silicone filler is specifically prepared according to the following steps: 按重量份数称取30份~80份有机硅源、10份~40份水和5份~20份正硅酸乙酯;将称取的30份~80份有机硅源和10份~40份水混合,在温度为50℃~100℃下反应1h~5h,自然冷却至30℃~60℃,再滴加5份~20份正硅酸乙酯,得到凝胶;将凝胶在20℃~30℃下真空干燥10h~20h,得到活性有机硅填料;其中,所述的有机硅源为γ-氨丙基三乙氧基硅烷和有机硅单体混合物组成;所述的有机硅单体混合物为二甲基二乙氧基硅烷、甲基三乙氧基硅烷、甲基三乙酰氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、二苯基二乙氧基硅烷和甲基三乙酰氧基硅烷中的一种或几种的混合物。Weigh 30-80 parts of organic silicon source, 10-40 parts of water and 5-20 parts of ethyl orthosilicate in parts by weight; weigh 30-80 parts of organic silicon source and 10-40 Mix parts of water, react at a temperature of 50°C to 100°C for 1h to 5h, cool naturally to 30°C to 60°C, and then add 5 to 20 parts of ethyl orthosilicate dropwise to obtain a gel; ℃~30℃ for 10h~20h to obtain active silicone filler; wherein, the organic silicon source is composed of γ-aminopropyltriethoxysilane and organic silicon monomer mixture; the organic silicon monomer The solid mixture is dimethyldiethoxysilane, methyltriethoxysilane, methyltriacetoxysilane, γ-glycidyl etheroxypropyltrimethoxysilane, γ-methacryloxypropyl One or a mixture of trimethoxysilane, vinyltriethoxysilane, diphenyldiethoxysilane and methyltriacetoxysilane. 4.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的固化剂为4,4-二氨基二苯醚、4,4-二氨基二苯砜、甲基四氢邻苯二甲酸酐、甲基六氢邻苯二甲酸酐、六氢邻苯二甲酸酐或甲基纳迪克酸酐。4. A high temperature resistant epoxy silicone potting compound according to claim 1, characterized in that said curing agent is 4,4-diaminodiphenyl ether, 4,4-diaminodiphenyl sulfone, Methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, or methylnadic anhydride. 5.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的固化促进剂为2,4,6-三(二甲胺基甲基)苯酚、间苯二酚、8-羟基喹啉、二甲基苄胺、2-乙基-4-甲基咪唑或2-甲基咪唑。5. A kind of high temperature resistant epoxy silicone potting compound according to claim 1, is characterized in that described curing accelerator is 2,4,6-tris(dimethylaminomethyl)phenol, m-benzene Diphenol, 8-hydroxyquinoline, dimethylbenzylamine, 2-ethyl-4-methylimidazole or 2-methylimidazole. 6.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的稀释剂为1,4-丁二醇二缩水甘油醚、乙二醇二缩水甘油醚、间苯二酚二缩水甘油醚、1,6-已二醇二缩水甘油醚、邻甲苯基缩水甘油醚和新戊二醇二缩水甘油醚中的一种或几种的混合物。6. A kind of high temperature resistant epoxy silicone potting compound according to claim 1, characterized in that said diluent is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, One or a mixture of resorcinol diglycidyl ether, 1,6-hexanediol diglycidyl ether, o-cresyl glycidyl ether and neopentyl glycol diglycidyl ether. 7.根据权利要求1所述的一种耐高温环氧有机硅灌封胶,其特征在于所述的消泡剂为德国迪高公司生产的型号为airex940的消泡剂。7. A high-temperature-resistant epoxy silicone potting compound according to claim 1, characterized in that said defoamer is airex940 produced by Tego, Germany. 8.一种耐高温环氧有机硅灌封胶的制备方法,其特征在于一种耐高温环氧有机硅灌封胶的制备方法具体是按以下步骤完成的:8. A preparation method of high temperature resistant epoxy silicone potting glue, characterized in that a kind of preparation method of high temperature resistant epoxy silicone potting glue is specifically completed according to the following steps: 一、制备环氧有机硅树脂:按重量份数称取30份~80份有机硅源、10份~40份水、20份~100份环氧树脂和40份~80份溶剂;首先将30份~80份有机硅源和10份~40份水混合,在温度为50℃~100℃下反应1h~5h,得到混合液,然后在温度为70℃~100℃和压力1kPa~10kPa下脱除混合液中的水和生成的醇类物质,再加入20份~100份环氧树脂和40份~80份溶剂,在温度为60℃~100℃下反应2h~4h,减压蒸馏脱除溶剂,得到环氧有机硅树脂;其中,所述的有机硅源为γ-氨丙基三乙氧基硅烷和有机硅单体混合物组成;所述的有机硅单体混合物为二甲基二乙氧基硅烷、甲基三乙氧基硅烷、甲基三乙酰氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、二苯基二乙氧基硅烷和甲基三乙酰氧基硅烷中的一种或几种的混合物;所述的溶剂为甲苯、甲乙酮、乙酸乙酯、乙醇、丙酮、四氢呋喃和二甲苯中的一种或几种的混合液;所述的环氧树脂为双酚-A型环氧树脂E-44、E-51和E-54中的一种或几种的混合物;1. Preparation of epoxy silicone resin: weigh 30 to 80 parts of organic silicon source, 10 to 40 parts of water, 20 to 100 parts of epoxy resin and 40 to 80 parts of solvent in parts by weight; Mix 1-80 parts of organosilicon source and 10-40 parts of water, react for 1h-5h at a temperature of 50°C-100°C to obtain a mixed solution, and then remove it at a temperature of 70°C-100°C and a pressure of 1kPa-10kPa In addition to the water and the generated alcohols in the mixed solution, add 20 to 100 parts of epoxy resin and 40 to 80 parts of solvent, react at a temperature of 60°C to 100°C for 2h to 4h, and remove it by distillation under reduced pressure Solvent to obtain epoxy silicone resin; wherein, the organic silicon source is composed of γ-aminopropyltriethoxysilane and organic silicon monomer mixture; the organic silicon monomer mixture is dimethyldiethyl Oxysilane, Methyltriethoxysilane, Methyltriacetoxysilane, γ-Glycidoxypropyltrimethoxysilane, γ-Methacryloxypropyltrimethoxysilane, Vinyl A mixture of one or more of triethoxysilane, diphenyldiethoxysilane and methyltriacetoxysilane; the solvent is toluene, methyl ethyl ketone, ethyl acetate, ethanol, acetone, tetrahydrofuran and one or more mixed solutions in xylene; the epoxy resin is a mixture of one or more of bisphenol-A epoxy resins E-44, E-51 and E-54; 二、制备活性有机硅填料:按重量份数称取30份~80份有机硅源、10份~40份水和5份~20份正硅酸乙酯;将称取的30份~80份有机硅源和10份~40份水混合,在温度为50℃~100℃下反应1h~5h,自然冷却至30℃~60℃,再滴加5份~20份正硅酸乙酯,得到凝胶;将凝胶在20℃~30℃下真空干燥10h~20h,得到活性有机硅填料;其中,所述的有机硅源为γ-氨丙基三乙氧基硅烷和有机硅单体混合物组成;所述的有机硅单体混合物为二甲基二乙氧基硅烷、甲基三乙氧基硅烷、甲基三乙酰氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、二苯基二乙氧基硅烷和甲基三乙酰氧基硅烷中的一种或几种的混合物;2. Preparation of active silicone filler: weigh 30 to 80 parts of organic silicon source, 10 to 40 parts of water and 5 to 20 parts of ethyl orthosilicate in parts by weight; weigh 30 to 80 parts Mix the organic silicon source with 10-40 parts of water, react at a temperature of 50°C-100°C for 1h-5h, cool naturally to 30°C-60°C, and then add 5-20 parts of ethyl orthosilicate dropwise to obtain Gel; vacuum-dry the gel at 20°C to 30°C for 10h to 20h to obtain an active silicone filler; wherein, the silicone source is a mixture of γ-aminopropyltriethoxysilane and silicone monomers Composition; the silicone monomer mixture is dimethyldiethoxysilane, methyltriethoxysilane, methyltriacetoxysilane, γ-glycidyl etheroxypropyltrimethoxysilane, γ -One or more mixtures of methacryloxypropyltrimethoxysilane, vinyltriethoxysilane, diphenyldiethoxysilane and methyltriacetoxysilane; 三、称取:按重量份数由100份~150份步骤一得到的环氧有机硅树脂、10份~55份步骤二得到的活性有机硅填料、25份~70份固化剂、1份~3份固化促进剂、10份~50份稀释剂和0.5份~3份消泡剂;3. Weighing: 100-150 parts by weight of epoxy silicone resin obtained in step 1, 10-55 parts of active silicone filler obtained in step 2, 25-70 parts of curing agent, 1- 3 parts of curing accelerator, 10 to 50 parts of diluent and 0.5 to 3 parts of defoamer; 四、混合:将步骤一称取的100份~150份步骤一得到的环氧有机硅树脂、10份~55份步骤二得到的活性有机硅填料、25份~70份固化剂、1份~3份固化促进剂、10份~50份稀释剂和0.5份~3份消泡剂混合,得到耐高温环氧有机硅灌封胶;4. Mixing: Weigh 100-150 parts of epoxy silicone resin obtained in step 1, 10-55 parts of active silicone filler obtained in step 2, 25-70 parts of curing agent, 1- 3 parts of curing accelerator, 10 to 50 parts of diluent and 0.5 to 3 parts of defoamer are mixed to obtain high temperature resistant epoxy silicone potting glue; 步骤三所述的稀释剂为1,4-丁二醇二缩水甘油醚、乙二醇二缩水甘油醚、间苯二酚二缩水甘油醚、1,6-已二醇二缩水甘油醚、邻甲苯基缩水甘油醚和新戊二醇二缩水甘油醚中的一种或几种的混合物;The diluent described in step three is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, resorcinol diglycidyl ether, 1,6-hexanediol diglycidyl ether, ortho One or more mixtures of cresyl glycidyl ether and neopentyl glycol diglycidyl ether; 步骤三所述的消泡剂为德国迪高公司生产的型号为airex940的消泡剂。The defoamer described in step 3 is the defoamer of the model airex940 produced by Tego, Germany. 9.根据权利要求8所述的一种耐高温环氧有机硅灌封胶的制备方法,其特征在于步骤三所述的固化促进剂为2,4,6-三(二甲胺基甲基)苯酚、间苯二酚、8-羟基喹啉、二甲基苄胺、2-乙基-4-甲基咪唑或2-甲基咪唑。9. The preparation method of a kind of high temperature resistant epoxy silicone potting compound according to claim 8, it is characterized in that the curing accelerator described in step 3 is 2,4,6-tris(dimethylaminomethyl ) phenol, resorcinol, 8-hydroxyquinoline, dimethylbenzylamine, 2-ethyl-4-methylimidazole or 2-methylimidazole. 10.根据权利要求8所述的一种耐高温环氧有机硅灌封胶的制备方法,其特征在于步骤三所述的固化剂为4,4-二氨基二苯醚、4,4-二氨基二苯砜、甲基四氢邻苯二甲酸酐、甲基六氢邻苯二甲酸酐、六氢邻苯二甲酸酐或甲基纳迪克酸酐。10. A method for preparing a high temperature resistant epoxy silicone potting compound according to claim 8, characterized in that the curing agent described in step three is 4,4-diaminodiphenyl ether, 4,4-diphenyl ether Aminodiphenylsulfone, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methylnadic anhydride.
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CN106753205B (en) * 2017-01-11 2020-05-22 湖南博翔新材料有限公司 Epoxy modified organic silicon pouring sealant with low viscosity and high heat conductivity and application thereof
CN109880561A (en) * 2017-12-06 2019-06-14 上海本诺电子材料有限公司 A kind of epoxy resin embedding adhesive composition and preparation method thereof
CN110229585A (en) * 2019-06-18 2019-09-13 刘涛 A kind of heat treatment can quick selfreparing coating and preparation method thereof
CN116693810A (en) * 2023-07-04 2023-09-05 嘉兴南洋万事兴化工有限公司 High heat-resistant epoxy curing agent for LED packaging, preparation method and epoxy pouring sealant prepared by using high heat-resistant epoxy curing agent

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