CN101508825B - Epoxy resin embedding glue and method for producing the same - Google Patents
Epoxy resin embedding glue and method for producing the same Download PDFInfo
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- CN101508825B CN101508825B CN2009101197980A CN200910119798A CN101508825B CN 101508825 B CN101508825 B CN 101508825B CN 2009101197980 A CN2009101197980 A CN 2009101197980A CN 200910119798 A CN200910119798 A CN 200910119798A CN 101508825 B CN101508825 B CN 101508825B
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Abstract
The invention relates to an epoxy resin potting adhesive which consists of component A and component B. By weight portion, the component A consists of 90-130 portions of bisphenol A type epoxy resin, 240-320 portions of filling, 15-25 portions of thinner, 10-25 portions of toughener, 1-2.5 portions of defoamer and 0.8-2 portions of black pigment, and the component B consists of 60-130 portions of estolide and 1-3 portions of imidazole accelerator. The mixing proportion of the component A and the component B is (3-5):1. The invention also provides a preparation method of the epoxy resin potting adhesive. The epoxy resin potting adhesive provided by the invention has low cost and long resting period; after being mixed, the component A and the component B have low viscidity, good wetting quality, good heat resistance, good defoaming performance, good fluidity and long operating time and are solidified between 70 DEG C and 160 DEG C; a product after solidifying has bright surface, good mechanical performance and insulating performance and high glass transition temperature; and the quality of a potting component is stable.
Description
Technical field
The present invention relates to a kind of epoxy resin embedding adhesive and preparation method thereof, this epoxy resin embedding adhesive can be applicable to the embedding of motor vehicle spark coil.
Background technology
Resins, epoxy is a kind of thermosetting resin, has excellent cementability, physical strength and electrical insulating property, thereby is widely used in cast, the embedding of devices such as electronic devices and components, transformer.But because pure epoxy resin has high crosslinking structure, thus have that matter is crisp, shortcomings such as fatiguability, thermotolerance are good inadequately, toughness difference.For the reliability that guarantees the embedding device, good heat dissipation ability and excellent electric performance, be necessary Resins, epoxy is carried out the modification of aspects such as toughness reinforcing, heat-resisting, fire-retardant and reduction internal stress.
Summary of the invention
Technical problem to be solved by this invention provides a kind of epoxy resin embedding adhesive and preparation method thereof, this epoxy resin embedding adhesive is a double-component epoxy resin embedding adhesive, has that viscosity is low, a good heat resistance, second-order transition temperature (Tg) is high, the shelf-time is long, the applicable time is long advantage.The technical scheme that adopts is as follows:
A kind of epoxy resin embedding adhesive, it is characterized in that forming by A component and B component, by weight, the A component consist of 90～130 parts of bisphenol A type epoxy resins, 240～320 parts of fillers, 15～25 parts of thinners, 10～25 parts of toughner, 1～2.5 part of defoamer, 0.8～2 part of mineral black, the B component consist of 60～130 parts on acid anhydrides, 1～3 part of imidazoles promotor, the blending ratio of A component and B component is (3～5): 1; Described filler is made up of active micro silicon powder, lime carbonate and aluminium hydroxide, and its weight proportion is 180～280 parts of active micro silicon powders, 20～60 parts in lime carbonate, 10～50 parts in aluminium hydroxide.
Preferred above-mentioned bisphenol A type epoxy resin is that oxirane value is 0.41～0.54 bisphenol A type epoxy resin; More preferably above-mentioned bisphenol A type epoxy resin is a kind of in E-51 Resins, epoxy and the E-44 Resins, epoxy or both mixtures.
Above-mentioned filler can the reinforced epoxy joint sealant mechanical property, reduce the coefficient of expansion of epoxy resin embedding adhesive, and make the insulation of epoxy resin embedding adhesive and flame retardant properties good.The loading level of filler of the present invention is big, and viscosity is low, and wetting property is good, cured article mechanical property excellence.Because high filler loading level, make the product line coefficient of expansion very low, and cost reduce greatly, help improving product competitiveness.
Preferred above-mentioned thinner is multi-functional reactive thinner, more preferably thinner is a kind of or wherein multiple mixture in glycerol triglycidyl ether, 1,4 one butanediol diglycidyl ether, hexanediol diglycidyl ether and the TriMethylolPropane(TMP) glycidyl ether.Adopt multi-functional reactive thinner, can under the situation that reduces system viscosity, guarantee the thermotolerance of product simultaneously again.
Preferred above-mentioned toughner is polyurethanes toughner (" strange scholar " toughner that for example can buy on the market), it is a kind of polymeric blends that has the different activities end group, different types of segment is tied by ester bond or ammonia ester bond, this toughner is respond well, and is very little to the influence of product second-order transition temperature.
Preferred above-mentioned defoamer is a silicone antifoam agent, as polysiloxane.But defoamer has well the bubble defoaming effect the epoxy resin embedding adhesive system.
Above-mentioned mineral black can adopt carbon black.
Above-mentioned acid anhydrides is a liquid anhydride.Preferred above-mentioned acid anhydrides is a kind of in methyl tetrahydrophthalic anhydride and the methylhexahydrophthalic anhydride or both mixtures.Acid anhydrides makes the epoxy resin embedding adhesive viscosity low as solidifying agent, shrink little, hypotoxicity, it is good to solidify the back electric property.Adopt liquid anhydride to mix, make that epoxy resin embedding adhesive viscosity is little, little to skin irritation, instillation process is good, shrinking percentage is little, cured article good mechanical property, electric property excellence with Resins, epoxy.
Preferred above-mentioned imidazoles promotor is a kind of or wherein multiple mixture in 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole and the 1-cyanoethyl-2-ethyl-4-methylimidazole.Adopt imidazoles promotor, can reduce the solidification value of epoxy resin embedding adhesive, make epoxy resin embedding adhesive have the long operating time.
On the other hand, the invention provides a kind of preparation method of above-mentioned epoxy resin embedding adhesive, this preparation method comprises the steps:
(1) prepares the A component: bisphenol A type epoxy resin, thinner, toughner and defoamer are mixed and be stirred to mixing (preferred stirrer rotating speed is 1000～1400rpm, and churning time is 5～15 minutes); Add mineral black and filler (preferred stirrer rotating speed is 100～300rpm) while stirring then; Continue again after mineral black and filler all add to stir (preferred stirrer rotating speed is 1500～2000rpm, and churning time is 20～30 minutes), bisphenol A type epoxy resin, thinner, toughner, defoamer, mineral black and filler are mixed; Carry out vacuum defoamation (preferred vacuum tightness is more than the 100pa) then, obtain the A component;
(2) preparation B component: imidazoles promotor is joined in the acid anhydrides, and be stirred to and mix (preferred stirrer rotating speed is 800～1000rpm, and churning time is 8～15 minutes); Carry out vacuum defoamation (preferred vacuum tightness is more than the 100pa) then, obtain the B component;
(3) separated deposit A component and B component; Preferably with A component and B component separated deposit under dry, airy environment (preferred ambient humidity is RH70% below), envrionment temperature is below 30 ℃, in case the A component and the B component moisture absorption go bad;
(4) preparation of epoxy resin embedding adhesive: in the time of need carrying out embedding, with A component and B component according to (3～5): 1 part by weight (is the A component: B component=(3～5): 1) mix, and be stirred to and mix and (preferably under the stirrer rotating speed is the situation of 100～400rpm, stirred 4～8 minutes earlier, under being the situation of 1000～1600rpm, stirred 10～15 minutes the stirrer rotating speed again), carry out vacuum defoamation (preferred vacuum tightness is more than the 100pa) then, obtain epoxy resin embedding adhesive.
The loading level of epoxy resin embedding adhesive filler provided by the invention is big, and cost is lower; A component and B component are separately deposited, and the shelf-time is long; A component and B component mix back viscosity low (mix that initial viscosity＜10Pa.s), wetting property is good, good heat resistance, antifoam performance is good, good fluidity has the long applicable time (under 25 ℃ temperature,＞6 hours), is cured between 70 ℃～160 ℃; The solidified after-product surface-brightening, mechanical property and insulating property good (tensile strength＞60MPa, flexural strength＞100MPa), second-order transition temperature height (＞100 ℃), the steady quality of embedding part.This epoxy resin embedding adhesive can be applicable to the embedding of the electronic apparatus materials such as spark coil of motor vehicle (as automobile, motorcycle).
Embodiment
Embodiment 1
Prepare epoxy resin embedding adhesive by following step:
(1) preparation A component: with 95 gram bisphenol A type epoxy resin E-51,16 gram thinners (glycerol triglycidyl ether 8.5 grams, 1 wherein, 4-butanediol diglycidyl ether 7.5 gram), 11 grams polyurethane toughened dose (" strange scholar " toughner that adopts can buy on the market) and 1.1 restrain defoamers (being polysiloxane) and mix and be stirred to and mix (the stirrer rotating speed is 1000rpm, and churning time is 15 minutes); Add 0.9 gram carbon black and 240 gram fillers (wherein active micro silicon powder 190 grams, lime carbonate 40 restrain, aluminium hydroxide 10 grams) while stirring (the stirrer rotating speed is 120rpm) then; Continue again after carbon black and filler all add to stir (the stirrer rotating speed is 1800rpm, and churning time is 25 minutes), bisphenol A type epoxy resin E-51, thinner, polyurethane toughened dose, defoamer, carbon black and filler are mixed; Carry out vacuum defoamation (vacuum tightness is 100pa) then, obtain the A component; The A component that obtains contains 95 gram bisphenol A type epoxy resin E-51,16 gram thinners, polyurethane toughened dose of 11 grams, 1.1 gram defoamers, 0.9 gram carbon black and 240 gram fillers;
(2) preparation B component: 2 gram imidazoles promotor (wherein 2-ethyl imidazol(e) 0.5 gram, 1-cyanoethyl-2-ethyl-4-methylimidazole 1.5 grams) are joined in the 61 gram methyl tetrahydrophthalic anhydrides, and be stirred to and mix (the stirrer rotating speed is 1000rpm, and churning time is 8 minutes); Carry out vacuum defoamation (vacuum tightness is 100pa) then, obtain the B component; The B component that obtains contains 2 gram imidazoles promotor and 61 gram methyl tetrahydrophthalic anhydrides;
(3) with A component and B component separated deposit under dry, airy environment (ambient moisture is RH50%), envrionment temperature is 25 ℃;
(4) preparation of epoxy resin embedding adhesive: in the time of need carrying out embedding, getting the B component that the 100 A components that obtain of gram steps (1) and 26 gram steps (2) obtain (is the A component: B component=100: 26) mix, and be stirred to and mix and (under the stirrer rotating speed is the situation of 150rpm, stirred 8 minutes earlier, be to stir 12 minutes under the situation of 1200rpm at the stirrer rotating speed again), carry out vacuum defoamation (vacuum tightness is 50pa) then, obtain 126 gram epoxy resin embedding adhesives.
During batch process, prepare A component and B component according to above-mentioned part by weight; And by above-mentioned part by weight preparation epoxy resin embedding adhesive.
Embodiment 2
Prepare epoxy resin embedding adhesive by following step:
(1) preparation A component: 130 gram bisphenol A type epoxy resins (wherein 90 grams are bisphenol A type epoxy resin E-44 for bisphenol A type epoxy resin E-51,40 grams), 20 gram thinners (wherein TriMethylolPropane(TMP) glycidyl ether 12.5 grams, hexanediol diglycidyl ether 7.5 grams), 18 grams polyurethane toughened dose (" strange scholar " toughner that adopts can buy on the market) and 1.5 are restrained defoamers (being polysiloxane) mix and be stirred to and mix (the stirrer rotating speed is 1400rpm, and churning time is 6 minutes); Add 1.5 gram carbon blacks and 318 gram fillers (wherein active micro silicon powder 220 grams, lime carbonate 58 grams, aluminium hydroxide 40 grams) while stirring (the stirrer rotating speed is 300rpm) then; Continue again after carbon black and filler all add to stir (the stirrer rotating speed is 2000rpm, and churning time is 20 minutes), bisphenol A type epoxy resin, thinner, polyurethane toughened dose, defoamer, carbon black and filler are mixed; Carry out vacuum defoamation (vacuum tightness is 80pa) then, obtain the A component; The A component that obtains contains 130 gram bisphenol A type epoxy resins, 20 gram thinners, polyurethane toughened dose of 18 grams, 1.5 gram defoamers, 1.5 gram carbon blacks and 318 gram fillers;
(2) preparation B component: 1.1 gram imidazoles promotor (wherein 2-ethyl imidazol(e) 0.5 gram, 2-ethyl-4-methylimidazole 0.6 gram) are joined in the 105 gram methylhexahydrophthalic anhydrides, and be stirred to and mix (the stirrer rotating speed is 900rpm, and churning time is 12 minutes); Carry out vacuum defoamation (vacuum tightness is 80pa) then, obtain the B component; The B component that obtains contains 1.1 gram imidazoles promotor and 105 gram methylhexahydrophthalic anhydrides;
(3) with A component and B component separated deposit under dry, airy environment (ambient moisture is RH60%), envrionment temperature is 26 ℃;
(4) preparation of epoxy resin embedding adhesive: in the time of need carrying out embedding, getting the B component that the 100 A components that obtain of gram steps (1) and 32 gram steps (2) obtain (is the A component: B component=100: 32) mix, and be stirred to and mix and (under the stirrer rotating speed is the situation of 250rpm, stirred 6 minutes earlier, be to stir 15 minutes under the situation of 1000rpm at the stirrer rotating speed again), carry out vacuum defoamation (vacuum tightness is 40pa) then, obtain 132 gram epoxy resin embedding adhesives.
During batch process, prepare A component and B component according to above-mentioned part by weight; And by above-mentioned part by weight preparation epoxy resin embedding adhesive.
Embodiment 3
Prepare epoxy resin embedding adhesive by following step:
(1) preparation A component: 115 gram bisphenol A type epoxy resin E-44,25 gram thinners (wherein hexanediol diglycidyl ether 10 grams, glycerol triglycidyl ether 15 grams), 25 grams polyurethane toughened dose (" strange scholar " toughner that adopts can buy on the market) and 2.4 are restrained defoamers (being polysiloxane) mix and be stirred to and mix (the stirrer rotating speed is 1200rpm, and churning time is 10 minutes); Add 2 gram carbon blacks and 295 gram fillers (wherein active micro silicon powder 250 grams, lime carbonate 20 grams, aluminium hydroxide 25 grams) while stirring (the stirrer rotating speed is 200rpm) then; Continue again after carbon black and filler all add to stir (the stirrer rotating speed is 1500rpm, and churning time is 30 minutes), bisphenol A type epoxy resin E-44, thinner, polyurethane toughened dose, defoamer, carbon black and filler are mixed; Carry out vacuum defoamation (vacuum tightness is 90pa) then, obtain the A component; The A component that obtains contains 115 gram bisphenol A type epoxy resin E-44,25 gram thinners, polyurethane toughened dose of 25 grams, 2.4 gram defoamers (polysiloxane), 2 gram carbon blacks and 295 gram fillers;
(2) preparation B component: 2.8 gram imidazoles promotor (wherein 2-ethyl imidazol(e) 0.8 gram, 2-ethyl-4-methylimidazole 1 gram, 1-cyanoethyl-2-ethyl-4-methylimidazole 1 gram) are joined in the 128 gram acid anhydrides (wherein methyl tetrahydrophthalic anhydride 88 grams, methylhexahydrophthalic anhydride 40 grams), and be stirred to and mix (the stirrer rotating speed is 800rpm, and churning time is 15 minutes); Carry out vacuum defoamation (vacuum tightness is 90pa) then, obtain the B component; The B component that obtains contains 2.8 gram imidazoles promotor and 128 gram acid anhydrides;
(3) with A component and B component separated deposit under dry, airy environment (ambient moisture is RH60%), envrionment temperature is 25 ℃;
(4) preparation of epoxy resin embedding adhesive: in the time of need carrying out embedding, getting the B component that the 100 A components that obtain of gram steps (1) and 20 gram steps (2) obtain (is the A component: B component=100: 20) mix, and be stirred to and mix and (under the stirrer rotating speed is the situation of 400rpm, stirred 4 minutes earlier, be to stir 10 minutes under the situation of 1500rpm at the stirrer rotating speed again), carry out vacuum defoamation (vacuum tightness is 40pa) then, obtain 120 gram epoxy resin embedding adhesives.
During batch process, prepare A component and B component according to above-mentioned part by weight; And by above-mentioned part by weight preparation epoxy resin embedding adhesive.
Claims (9)
1. epoxy resin embedding adhesive, it is characterized in that forming by A component and B component, by weight, the A component consist of 90～130 parts of bisphenol A type epoxy resins, 240～320 parts of fillers, 15～25 parts of thinners, 10～25 parts of toughner, 1～2.5 part of defoamer, 0.8～2 part of mineral black, the B component consist of 60～130 parts on acid anhydrides, 1～3 part of imidazoles promotor, the blending ratio of A component and B component is (3～5): 1; Described filler is made up of active micro silicon powder, lime carbonate and aluminium hydroxide, and its weight proportion is 180～280 parts of active micro silicon powders, 20～60 parts in lime carbonate, 10～50 parts in aluminium hydroxide.
2. epoxy resin embedding adhesive according to claim 1 is characterized in that: described bisphenol A type epoxy resin is that oxirane value is 0.41～0.54 bisphenol A type epoxy resin.
3. epoxy resin embedding adhesive according to claim 2 is characterized in that: described bisphenol A type epoxy resin is a kind of in E-51 Resins, epoxy and the E-44 Resins, epoxy or both mixtures.
4. epoxy resin embedding adhesive according to claim 1, it is characterized in that: described thinner is a glycerol triglycidyl ether, 1, a kind of or wherein multiple mixture in 4-butanediol diglycidyl ether, hexanediol diglycidyl ether and the TriMethylolPropane(TMP) glycidyl ether.
5. epoxy resin embedding adhesive according to claim 1 is characterized in that: described toughner is polyurethanes toughner.
6. epoxy resin embedding adhesive according to claim 1 is characterized in that: described defoamer is a polysiloxane.
7. epoxy resin embedding adhesive according to claim 1 is characterized in that: described acid anhydrides is a kind of in methyl tetrahydrophthalic anhydride and the methylhexahydrophthalic anhydride or both mixtures.
8. epoxy resin embedding adhesive according to claim 1 is characterized in that: described imidazoles promotor is a kind of or wherein multiple mixture in 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole and the 1-cyanoethyl-2-ethyl-4-methylimidazole.
9. the preparation method of the described epoxy resin embedding adhesive of claim 1 is characterized in that comprising the steps:
(1) prepares the A component: bisphenol A type epoxy resin, thinner, toughner and defoamer are mixed and be stirred to mixing; Add mineral black and filler while stirring then; Continue again after mineral black and filler all add to stir, bisphenol A type epoxy resin, thinner, toughner, defoamer, mineral black and filler are mixed; Carry out vacuum defoamation then, obtain the A component;
(2) preparation B component: imidazoles promotor is joined in the acid anhydrides, and be stirred to and mix; Carry out vacuum defoamation then, obtain the B component;
(3) separated deposit A component and B component;
(4) preparation of epoxy resin embedding adhesive: in the time of need carrying out embedding, with A component and B component according to (3～5): 1 part by weight mixes, and is stirred to and mixes, and carries out vacuum defoamation then, obtains epoxy resin embedding adhesive.
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2009
- 2009-03-30 CN CN2009101197980A patent/CN101508825B/en active Active
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| CN104559892A (en) * | 2014-11-17 | 2015-04-29 | 南京艾布纳密封技术有限公司 | Novel epoxy resin sealant adhesive and preparation method thereof |
| CN106634752A (en) * | 2016-12-30 | 2017-05-10 | 上海嘉尔成汽车部件有限公司 | Special epoxy resin potting adhesive for ignition coils and preparation method thereof |
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