CN103805127B - Preparation method for high-temperature-resisting epoxy organic silicon pouring sealant - Google Patents
Preparation method for high-temperature-resisting epoxy organic silicon pouring sealant Download PDFInfo
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- CN103805127B CN103805127B CN201410066556.0A CN201410066556A CN103805127B CN 103805127 B CN103805127 B CN 103805127B CN 201410066556 A CN201410066556 A CN 201410066556A CN 103805127 B CN103805127 B CN 103805127B
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Abstract
The invention provides a preparation method of a high-temperature-resisting epoxy organic silicon pouring sealant, relates to a preparation method of one pouring sealant, and aims to solve the problems that an existing pouring sealant cannot have good toughness, high heat resistance and good adhesion at the same time. The high-temperature-resisting epoxy organic silicon pouring sealant is prepared from epoxy organic silicon resin, active organic silicon fillers, a curing agent, a curing accelerator, a diluting agent and a de-foaming agent. The preparation method comprises the following steps: 1, preparing the epoxy organic silicon resin; 2, preparing the active organic silicon fillers; 3, weighing; and 4, mixing. According to the preparation method of the high-temperature-resisting epoxy organic silicon pouring sealant, the prepared epoxy organic silicon resin and the prepared active organic silicon fillers are used as raw materials and the prepared organic silicon pouring sealant has low adhesiveness and good wettability; and the cured product has toughness and heat resistance, and the quality of a pouring sealing piece is stable. According to the preparation method, the high-temperature-resisting epoxy organic silicon pouring sealant can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of joint sealant.
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 is that shrinking percentage is little, no coupling product, excellent electrical insulation capability, but is subject to the restriction of molecular structure itself, and toughness is poor and thermotolerance is not high.No coupling product release when add-on type liquid silicon rubber has crosslinked, shrinking percentage is little, and cross-linking density and the feature such as vulcanization rate is easy to control are also the conventional body materials of joint sealant.But addition-type silicon rubber is because molecule itself is in nonpolar, and cementability is poor, when using 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 every profession and trade to the performance of joint sealant is more and more higher, and existing joint sealant exists can not have good toughness, thermotolerance is high and cementability is good problem concurrently simultaneously.
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 preparation method of fire resistant epoxy organic silicon potting adhesive 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, epoxy silicone resin is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water, 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents by weight; First by 30 parts ~ 80 parts organosilicon sources and 10 parts ~ 40 parts water mixing, 1h ~ 5h is reacted at temperature is 50 DEG C ~ 100 DEG C, obtain mixed solution, then under temperature is 70 DEG C ~ 100 DEG C and pressure 1kPa ~ 10kPa, remove the alcohols material of water in mixed solution and generation, add 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents again, at temperature is 60 DEG C ~ 100 DEG C, react 2h ~ 4h, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane; Described solvent is the mixed solution of one or more in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is the mixture of one or more in bisphenol-A-type epoxy resin E-44, E-51 and E-54;
Two, active organosilicon filler is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water and 5 parts ~ 20 parts tetraethoxys by weight; 30 parts ~ 80 parts organosilicon sources taken and 10 parts ~ 40 parts water are mixed, at temperature is 50 DEG C ~ 100 DEG C, reacts 1h ~ 5h, naturally cools to 30 DEG C ~ 60 DEG C, then drip 5 parts ~ 20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h ~ 20h at 20 DEG C ~ 30 DEG C, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane;
Three, take: the active organosilicon filler that the epoxy silicone resin obtained by 100 parts ~ 150 parts steps one by weight, 10 parts ~ 55 parts step 2 obtain, 25 parts ~ 70 parts solidifying agent, 1 part ~ 3 parts curing catalysts, 10 parts ~ 50 parts thinners and 0.5 part ~ 3 parts defoamers;
Four, mix: the active organosilicon filler that the epoxy silicone resin that 100 parts that step one are taken ~ 150 parts steps one obtain, 10 parts ~ 55 parts step 2 obtain, 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, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is 1, the mixture of one or more in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1,6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether;
Defoamer described in step 3 is the model that German Di Gao company produces is the defoamer of airex 940.
Advantage of the present invention: the preparation method that, 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 DEG C ~ 410 DEG C, and 25 DEG C time, shearing resistance is 23MPa ~ 26MPa; Two, the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence combines by the present invention, the toughness in epoxy resin is increased by flexible silicone segment, simultaneously retaining ring epoxy resins and the good adhesiveproperties of base material, add active organosilicon filler again, 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 test one step one obtains.
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: the preparation method that, present embodiments provide for 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 DEG C ~ 410 DEG C, and 25 DEG C time, shearing resistance is 23MPa ~ 26MPa; Two, the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence combines by present embodiment, the toughness in epoxy resin is increased by flexible silicone segment, simultaneously retaining ring epoxy resins and the good adhesiveproperties of base material, add active organosilicon filler again, 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 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water, 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents by weight; First by 30 parts ~ 80 parts organosilicon sources and 10 parts ~ 40 parts water mixing, 1h ~ 5h is reacted at temperature is 50 DEG C ~ 100 DEG C, obtain mixed solution, then under temperature is 70 DEG C ~ 100 DEG C and pressure 1kPa ~ 10kPa, remove the alcohols material of water in mixed solution and generation, add 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents again, at temperature is 60 DEG C ~ 100 DEG C, react 2h ~ 4h, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane; Described solvent is the mixed solution of one or more in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is the mixture of one or more 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 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water and 5 parts ~ 20 parts tetraethoxys by weight; 30 parts ~ 80 parts organosilicon sources taken and 10 parts ~ 40 parts water are mixed, at temperature is 50 DEG C ~ 100 DEG C, reacts 1h ~ 5h, naturally cools to 30 DEG C ~ 60 DEG C, then drip 5 parts ~ 20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h ~ 20h at 20 DEG C ~ 30 DEG C, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl 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)s, methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methylnadic 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, the mixture of one or more in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1,6-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 model that German Di Gao company produces is the defoamer of airex 940.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, epoxy silicone resin is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water, 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents by weight; First by 30 parts ~ 80 parts organosilicon sources and 10 parts ~ 40 parts water mixing, 1h ~ 5h is reacted at temperature is 50 DEG C ~ 100 DEG C, obtain mixed solution, then under temperature is 70 DEG C ~ 100 DEG C and pressure 1kPa ~ 10kPa, remove the alcohols material of water in mixed solution and generation, add 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents again, at temperature is 60 DEG C ~ 100 DEG C, react 2h ~ 4h, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane; Described solvent is the mixed solution of one or more in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is the mixture of one or more in bisphenol-A-type epoxy resin E-44, E-51 and E-54;
Two, active organosilicon filler is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water and 5 parts ~ 20 parts tetraethoxys by weight; 30 parts ~ 80 parts organosilicon sources taken and 10 parts ~ 40 parts water are mixed, at temperature is 50 DEG C ~ 100 DEG C, reacts 1h ~ 5h, naturally cools to 30 DEG C ~ 60 DEG C, then drip 5 parts ~ 20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h ~ 20h at 20 DEG C ~ 30 DEG C, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of one or more in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane;
Three, take: the active organosilicon filler that the epoxy silicone resin obtained by 100 parts ~ 150 parts steps one by weight, 10 parts ~ 55 parts step 2 obtain, 25 parts ~ 70 parts solidifying agent, 1 part ~ 3 parts curing catalysts, 10 parts ~ 50 parts thinners and 0.5 part ~ 3 parts defoamers;
Four, mix: the active organosilicon filler that the epoxy silicone resin that 100 parts that step one are taken ~ 150 parts steps one obtain, 10 parts ~ 55 parts step 2 obtain, 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, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is 1, the mixture of one or more in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1,6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether;
Defoamer described in step 3 is the model that German Di Gao company produces is the defoamer of airex 940.
The advantage of present embodiment: the preparation method that, present embodiments provide for 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 DEG C ~ 410 DEG C, and 25 DEG C time, shearing resistance is 23MPa ~ 26MPa; Two, the adhesiveproperties of organosilyl high heat resistance and epoxy resin excellence combines by present embodiment, the toughness in epoxy resin is increased by flexible silicone segment, simultaneously retaining ring epoxy resins and the good adhesiveproperties of base material, add active organosilicon filler again, 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 difference 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)s, methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methylnadic 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, epoxy silicone resin is prepared: take 50 parts of organosilicon sources, 10 parts of water, 90 parts of epoxy resin and 50 parts of solvents by weight; First by 50 parts of organosilicon sources and 10 parts of water mixing, 5h is reacted at temperature is 80 DEG C, obtain mixed solution, then under temperature is 100 DEG C and pressure 1kPa, remove the alcohols material of water in mixed solution and generation, add 90 parts of epoxy resin and 50 parts of solvents again, at temperature is 90 DEG C, react 2h, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; 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, active organosilicon filler is prepared: take 40 parts of organosilicon sources, 15 parts of water and 5 parts of tetraethoxys by weight; The 40 parts of organosilicon sources taken and 15 parts of water are mixed, at temperature is 70 DEG C, reacts 5h, naturally cools to 40 DEG C, then drip 5 parts of tetraethoxys, obtain gel; By gel vacuum-drying 15h at 25 DEG C, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is the mixture of methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and vinyltriethoxysilane;
Three, take: the active organosilicon filler that the epoxy silicone resin obtained by 100 parts ~ 150 parts steps one by weight, 10 parts ~ 55 parts step 2 obtain, 25 parts ~ 70 parts solidifying agent, 1 part ~ 3 parts curing catalysts, 10 parts ~ 50 parts thinners and 0.5 part ~ 3 parts defoamers;
Four, mix: the active organosilicon filler that the epoxy silicone resin that 100 parts that step one are taken ~ 150 parts steps one obtain, 10 parts ~ 55 parts step 2 obtain, 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, 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 model that German Di Gao company produces is the defoamer of airex 940;
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).
Infrared spectrometer is used to test the epoxy silicone resin that test one step one obtains, as shown in Figure 1.Fig. 1 is the infrared spectrum of the epoxy silicone resin that test one step one obtains, 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 DEG C, shearing resistance 25 DEG C time is 24.3MPa, shearing resistance 250 DEG C time is 4.5MPa, and the shearing resistance 300 DEG C time is 2.3MPa, and the shearing resistance 350 DEG C time is 1.1MPa.
Claims (3)
1. a preparation method for fire resistant epoxy organic silicon potting adhesive, is characterized in that what a kind of preparation method of fire resistant epoxy organic silicon potting adhesive specifically completed according to the following steps:
One, epoxy silicone resin is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water, 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents by weight; First by 30 parts ~ 80 parts organosilicon sources and 10 parts ~ 40 parts water mixing, 1h ~ 5h is reacted at temperature is 50 DEG C ~ 100 DEG C, obtain mixed solution, then under temperature is 70 DEG C ~ 100 DEG C and pressure 1kPa ~ 10kPa, remove the alcohols material of water in mixed solution and generation, add 20 parts ~ 100 parts epoxy resin and 40 parts ~ 80 parts solvents again, at temperature is 60 DEG C ~ 100 DEG C, react 2h ~ 4h, underpressure distillation desolvation, obtains epoxy silicone resin; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is several mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane; Described solvent is the mixed solution of one or more in toluene, methylethylketone, ethyl acetate, ethanol, acetone, tetrahydrofuran (THF) and dimethylbenzene; Described epoxy resin is the mixture of one or more in bisphenol-A-type epoxy resin E-44, E-51 and E-54;
Two, active organosilicon filler is prepared: take 30 parts ~ 80 parts organosilicon sources, 10 parts ~ 40 parts water and 5 parts ~ 20 parts tetraethoxys by weight; 30 parts ~ 80 parts organosilicon sources taken and 10 parts ~ 40 parts water are mixed, at temperature is 50 DEG C ~ 100 DEG C, reacts 1h ~ 5h, naturally cools to 30 DEG C ~ 60 DEG C, then drip 5 parts ~ 20 parts tetraethoxys, obtain gel; By gel vacuum-drying 10h ~ 20h at 20 DEG C ~ 30 DEG C, obtain active organosilicon filler; Wherein, described organosilicon source is γ-aminopropyl triethoxysilane and organosilane monomer mixture composition; Described organosilane monomer mixture is several mixture in dimethyldiethoxysilane, Union carbide A-162, methyl triacetoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, diphenyl diethoxy silane and methyl triacetoxysilane;
Three, take: the active organosilicon filler that the epoxy silicone resin obtained by 100 parts ~ 150 parts steps one by weight, 10 parts ~ 55 parts step 2 obtain, 25 parts ~ 70 parts solidifying agent, 1 part ~ 3 parts curing catalysts, 10 parts ~ 50 parts thinners and 0.5 part ~ 3 parts defoamers;
Four, mix: the active organosilicon filler that the epoxy silicone resin that 100 parts that step one are taken ~ 150 parts steps one obtain, 10 parts ~ 55 parts step 2 obtain, 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, obtain fire resistant epoxy organic silicon potting adhesive;
Thinner described in step 3 is 1, the mixture of one or more in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, resorcinol diglycidyl ether, 1,6-hexanediol diglycidyl ether, o-tolyl glycidyl ether and neopentylglycol diglycidyl ether;
Defoamer described in step 3 is the model that German Di Gao company produces is the defoamer of airex 940.
2. the preparation method of a kind of fire resistant epoxy organic silicon potting adhesive according to claim 1, it is characterized in that 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.
3. the preparation method of a kind of fire resistant epoxy organic silicon potting adhesive according to claim 1, it is characterized in that the solidifying agent described in step 3 is 4,4-diaminodiphenyl oxide, 4,4-diaminodiphenylsulfone(DDS)s, methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride or methylnadic anhydride.
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| CN104231945B (en) * | 2014-09-12 | 2016-03-23 | 东莞市新懿电子材料技术有限公司 | A kind of liquid optical cement |
| CN105860081B (en) * | 2016-05-30 | 2018-08-10 | 哈尔滨工业大学 | Double cured silicone resins of a kind of photo-thermal and preparation method thereof |
| CN106519189B (en) * | 2016-11-05 | 2018-08-17 | 福州大学 | A kind of phosphorus-containing flame-retardant epoxy resin and preparation method thereof that epoxy silicon oil is modified |
| 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 |
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| CN103102857A (en) * | 2012-11-29 | 2013-05-15 | 广州市尤特新材料有限公司 | High-temperature resistant adhesive for glass and preparation method thereof |
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| CN103102857A (en) * | 2012-11-29 | 2013-05-15 | 广州市尤特新材料有限公司 | High-temperature resistant adhesive for glass and preparation method thereof |
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