CN101948610B - Low-viscosity bi-component epoxy resin potting adhesive and preparation method thereof - Google Patents
Low-viscosity bi-component epoxy resin potting adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-viscosity bi-component epoxy resin potting adhesive. The potting adhesive is characterized by consisting of a component A and a component B, wherein the component A comprises 70 to 120 weight parts of bisphenol A epoxy resin, 150 to 230 weight parts of filler, 0 to 15 weight parts of glycidol ether, 0.4 to 2.5 weight parts of organic silicon antifoaming agent and 0.2 to 1.5 weight parts of black pigment; the component B comprises 70 to 130 weight parts of acid anhydride and 1 to 4 weight parts of quaternary ammonium salt; and the mixture ratio of the component A to the component B is (2.5-4.0) to 1. The invention provides a preparation method of the low-viscosity bi-component epoxy resin potting adhesive. In the method, the low-viscosity bi-component epoxy resin potting adhesive formed by mixing the component A and the component B has the advantages of low viscosity, high fluidity, high permeability and low cost.
Description
Technical field
The present invention relates to can be applicable to the cast of electron and electrician product, the material of embedding, specifically, relate to a kind of low-viscosity double-component epoxy resin embedding adhesive and preparation method thereof.
Background technology
Epoxy resin embedding adhesive has excellent mechanical property, chemical mediator-resitant property, adhesiveproperties and electrical insulation capability, is widely used in cast, the embedding of machinery, electronic devices and components, X-former.
In fields such as electronic devices and components, outdoor transformer, lighter for ignitions, need carry out embedding to the fine gap on the product, thereby to the demands for higher performance of epoxy resin embedding adhesive.The viscosity of present most of epoxy resin embedding adhesive glues is big, mobile relatively poor; The not embedding of suitable fine gap; Therefore be necessary epoxy resin embedding adhesive is improved; Viscosity when reducing its actually operating improves its flowability, to adapt to above-mentioned needs carry out the product of embedding to fine gap needs.
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, and A component and B component mix that the epoxy resin embedding adhesive viscosity that the back forms is low, good fluidity, perviousness are strong.The technical scheme that adopts is following:
A kind of low-viscosity double-component epoxy resin embedding adhesive; It is characterized in that forming by A component and B component; By weight; The A component consist of 0.2～1.5 part of 70～120 parts of bisphenol A epoxide resins, 150～230 parts of fillers, 0～15 part of glycidyl ether, 0.4～2.5 part of silicone antifoam agent and mineral black, the B component consist of 70～130 parts on acid anhydrides, 1～4 part of quaternary ammonium salt, the blending ratio of A component and B component is (2.5～4.0): 1; Said filler is made up of crystalline silicon powder, treated carbonates and white lake, and its weight proportion is 140～220 parts of crystalline silicon powders, 0～50 part of treated carbonates, 10～60 parts in white lake.
Preferred above-mentioned bisphenol A epoxide 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 epoxy resin and the E-44 epoxy resin or both mixtures.
The mechanical property of above-mentioned filler ability reinforced epoxy joint sealant reduces the coefficient of expansion of epoxy resin embedding adhesive, and makes epoxy resin embedding adhesive have good heat-conducting effect, insulating property and flame retardant properties.The loading level of filler of the present invention is big, makes that the epoxy resin embedding adhesive viscosity is low, wellability good, epoxy resin embedding adhesive cured article superior.
Above-mentioned glycidyl ether is a reactive thinner; Preferred above-mentioned glycidyl ether is 1, a kind of or wherein multiple mixture in 4-butanediol diglycidyl ether, hexanediol diglycidyl ether, ethylene glycol diglycidylether, benzyl glycidyl ether and the butylglycidyl ether.Adopt glycidyl ether as reactive thinner; Can greatly reduce epoxy resin embedding adhesive system viscosity; Make epoxy resin embedding adhesive possess superior perviousness and flowability, help having the embedding of the product of fine gap, and when reducing viscosity, guarantee the thermotolerance of product again.
Above-mentioned silicone antifoam agent can be polysiloxane defoamers or organic silicon modified by polyether skimmer.But silicone antifoam agent has well the bubble defoaming effect the epoxy resin embedding adhesive system.
Above-mentioned mineral black plays pigmentation to joint sealant, can adopt the nano level 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 is as solidifying agent, make that the epoxy resin embedding adhesive viscosity is low, shrinking percentage is little, little to skin irritation, toxicity is low, solidifies the back good mechanical property, electric property is excellent.
Above-mentioned quaternary ammonium salt is as promotor.Preferred above-mentioned quaternary ammonium salt is a kind of or wherein multiple mixture in DTAC, tetradecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride and the two dodecyl dimethyl ammonium chloride.Adopt quaternary ammonium salt as promotor, can reduce the solidification value of epoxy resin embedding adhesive, make epoxy resin embedding adhesive have the long running time.
On the other hand, the present invention provides a kind of preparation method of above-mentioned low-viscosity double-component epoxy resin embedding adhesive, it is characterized in that comprising the steps:
(1) preparation A component: bisphenol A epoxide resin, glycidyl ether and silicone antifoam agent are mixed, and be stirred to and mix (preferred stirrer rotating speed is 1000～1500rpm, and churning time is 5～15 minutes); Add mineral black and filler (preferred stirrer rotating speed is 200～500rpm) while stirring then; After mineral black and filler all add, continue to stir (preferred stirrer rotating speed is 1500～2000rpm, and churning time is 20～30 minutes) again, bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler are mixed; Mixture to bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler carries out vacuum defoamation (preferred absolute pressure is below the 100pa) then, obtains the A component;
(2) preparation B component: quaternary ammonium salt 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); Mixture to quaternary ammonium salt and acid anhydrides carries out vacuum defoamation (preferred absolute pressure is below the 100pa) then, obtains the B component;
(3) preserve separately A component and B component; Preferably with A component and B component preserve separately 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 (2.5～4.0): 1 part by weight (is the A component: B component=(2.5～4.0): 1) mix; And be stirred to and mix and (preferably under the stirrer rotating speed is the situation of 200～400rpm, stirred 3～6 minutes earlier;, stirred 8～12 minutes the stirrer rotating speed under being the situation of 600～1000rpm again); Carry out vacuum defoamation (preferred absolute pressure is below the 100pa) then, obtain required low-viscosity double-component epoxy resin embedding adhesive.
Among the present invention; A component and B component mix that the low-viscosity double-component epoxy resin embedding adhesive viscosity that the back forms is low, good fluidity, perviousness are strong; Each item performance of low-viscosity double-component epoxy resin embedding adhesive is following: (1) viscosity: under 25 ℃ temperature≤and 2500 milli pascal seconds, under 60 ℃ temperature≤300 milli pascal seconds; (2) operable time: under 35 ℃ temperature>=5h (hour); (3) solidification value is 70～120 ℃; (4) set time be 3～5h (hour); (5) solidify back hardness: shore hardness>=88; (6) tensile strength>=50Mpa; (7) flexural strength>=90Mpa.In addition, the loading level of low-viscosity double-component epoxy resin embedding adhesive of the present invention is big, thereby cost is lower.
Embodiment
Embodiment 1
Prepare the low-viscosity double-component epoxy resin embedding adhesive by following step:
(1) preparation A component: 75 gram bisphenol A epoxide resins (being bisphenol A epoxide resin E 1), 6 are restrained glycidyl ethers, and (wherein ethylene glycol diglycidylether 4 restrains; Benzyl glycidyl ether 2 restrains) and 0.4 gram silicone antifoam agent (being ZGK 5) mixing; And be stirred to and mix (the stirrer rotating speed is 1000rpm, and churning time is 15 minutes); Add 0.2 gram mineral black (being carbon black) and 150 gram fillers (wherein crystalline silicon powder 140 restrains, white lake 10 grams) while stirring (the stirrer rotating speed is 500rpm) then; After mineral black and filler all add, continue again to stir (the stirrer rotating speed is 1800rpm, and churning time is 25 minutes), bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler are mixed; Mixture to bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler carries out vacuum defoamation (absolute pressure is 100pa) then, obtains the A component; The A component that obtains contains 75 gram bisphenol A epoxide resins, 6 gram glycidyl ethers, 0.4 gram silicone antifoam agent, 0.2 gram mineral black and 150 gram fillers;
(2) preparation B component: 1.2 gram quaternary ammonium salts (being DTAC) are joined in the 75 gram acid anhydrides (being methyl tetrahydrophthalic anhydride), and be stirred to and mix (the stirrer rotating speed is 1000rpm, and churning time is 8 minutes); Mixture to quaternary ammonium salt and acid anhydrides carries out vacuum defoamation (absolute pressure is 100pa) then, obtains the B component; The B component that obtains contains 1.2 gram quaternary ammonium salts and 75 gram acid anhydrides;
(3) with A component and B component preserve separately under dry, airy environment (ambient moisture is RH50%), envrionment temperature is 25 ℃;
(4) preparation of low-viscosity double-component 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 33 gram steps (2) obtain (is the A component: B component=100: 33) mix; And be stirred to and mix and (under the stirrer rotating speed is the situation of 300rpm, stirred 5 minutes earlier; Be to stir 12 minutes under the situation of 600rpm at the stirrer rotating speed again); Carry out vacuum defoamation (absolute pressure is 50pa) then, obtain 133 gram low-viscosity double-component 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 low-viscosity double-component epoxy resin embedding adhesive.
Embodiment 2
Prepare the low-viscosity double-component epoxy resin embedding adhesive by following step:
(1) preparation A component: (wherein bisphenol A epoxide resin E-51 is 70 grams with 110 gram bisphenol A epoxide resins; Bisphenol A epoxide resin E-44 is 40 grams) and 1.5 gram silicone antifoam agents (being organic silicon modified by polyether) mixing; And be stirred to and mix (the stirrer rotating speed is 1400rpm, and churning time is 6 minutes); Add 1.0 gram mineral blacks (being carbon black) and 213 gram fillers (wherein crystalline silicon powder 145 grams, lime carbonate 48 grams, white lake 20 grams) while stirring (the stirrer rotating speed is 300rpm) then; After mineral black and filler all add, continue again to stir (the stirrer rotating speed is 2000rpm, and churning time is 20 minutes), bisphenol A epoxide resin, silicone antifoam agent, mineral black and filler are mixed; Mixture to bisphenol A epoxide resin, silicone antifoam agent, mineral black and filler carries out vacuum defoamation (absolute pressure is 80pa) then, obtains the A component; The A component that obtains contains 110 gram bisphenol A epoxide resins, 1.5 gram silicone antifoam agents, 1.0 gram mineral blacks and 213 gram fillers;
(2) preparation B component: (wherein tetradecyl trimethyl ammonium chloride 2.0 restrains with 4.0 gram quaternary ammonium salts; Dodecyl benzyl dimethyl ammonium chloride 2.0 grams) join in the 126 gram acid anhydrides (being methylhexahydrophthalic anhydride); And be stirred to and mix (the stirrer rotating speed is 900rpm, and churning time is 12 minutes); Mixture to quaternary ammonium salt and acid anhydrides carries out vacuum defoamation (absolute pressure is 80pa) then, obtains the B component; The B component that obtains contains 4.0 gram quaternary ammonium salts and 126 gram acid anhydrides;
(3) with A component and B component preserve separately under dry, airy environment (ambient moisture is RH60%), envrionment temperature is 26 ℃;
(4) preparation of low-viscosity double-component 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 40 gram steps (2) obtain (is the A component: B component=100: 40) 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 8 minutes under the situation of 1000rpm at the stirrer rotating speed again); Carry out vacuum defoamation (absolute pressure is 40pa) then, obtain 140 gram low-viscosity double-component 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 low-viscosity double-component epoxy resin embedding adhesive.
Embodiment 3
Prepare the low-viscosity double-component epoxy resin embedding adhesive by following step:
(1) preparation A component: with 120 gram bisphenol A epoxide resins (being bisphenol A epoxide resin E-44), 15 gram glycidyl ethers (wherein 1; 4-butanediol diglycidyl ether 5 grams, hexanediol diglycidyl ether 5 grams, butylglycidyl ether 5 grams) and 2.4 gram silicone antifoam agents (being ZGK 5) mixing; And be stirred to and mix (the stirrer rotating speed is 1200rpm, and churning time is 10 minutes); Add 1.4 gram mineral blacks (being carbon black) and 230 gram fillers (wherein crystalline silicon powder 175 grams, white lake 55 grams) while stirring (the stirrer rotating speed is 200rpm) then; After mineral black and filler all add, continue again to stir (the stirrer rotating speed is 1500rpm, and churning time is 30 minutes), bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler are mixed; Mixture to bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler carries out vacuum defoamation (absolute pressure is 90pa) then, obtains the A component; The A component that obtains contains 120 gram bisphenol A epoxide resins, 15 gram glycidyl ethers, 2.4 gram silicone antifoam agents, 1.4 gram mineral blacks and 230 gram fillers;
(2) preparation B component: (wherein palmityl trimethyl ammonium chloride 1.5 restrains with 2.6 gram quaternary ammonium salts; Two dodecyl dimethyl ammonium chloride 1.1 grams) join in the 96 gram acid anhydrides (wherein methyl tetrahydrophthalic anhydride 30 grams, methylhexahydrophthalic anhydride 66 grams); And be stirred to and mix (the stirrer rotating speed is 800rpm, and churning time is 15 minutes); Mixture to quaternary ammonium salt and acid anhydrides carries out vacuum defoamation (absolute pressure is 90pa) then, obtains the B component; The B component that obtains contains 2.6 gram quaternary ammonium salts and 96 gram acid anhydrides;
(3) with A component and B component preserve separately 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 27 gram steps (2) obtain (is the A component: B component=100: 27) 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 900rpm at the stirrer rotating speed again), carry out vacuum defoamation (absolute pressure is 40pa) then, obtain 127 gram low-viscosity double-component 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 low-viscosity double-component epoxy resin embedding adhesive.
Claims (8)
1. low-viscosity double-component epoxy resin embedding adhesive; It is characterized in that forming by A component and B component; By weight; The A component consist of 0.2～1.5 part of 70～120 parts of bisphenol A epoxide resins, 150～230 parts of fillers, 0～15 part of glycidyl ether, 0.4～2.5 part of silicone antifoam agent and mineral black, the B component consist of 70～130 parts on acid anhydrides, 1～4 part of quaternary ammonium salt, the blending ratio of A component and B component is (2.5～4.0): 1; Said filler is made up of crystalline silicon powder, treated carbonates and white lake, and its weight proportion is 140～220 parts of crystalline silicon powders, 0～50 part of treated carbonates, 10～60 parts in white lake.
2. low-viscosity double-component epoxy resin embedding adhesive according to claim 1 is characterized in that: said bisphenol A epoxide resin is that oxirane value is 0.41～0.54 bisphenol A type epoxy resin.
3. low-viscosity double-component epoxy resin embedding adhesive according to claim 2 is characterized in that: said bisphenol A type epoxy resin is a kind of in E-51 epoxy resin and the E-44 epoxy resin or both mixtures.
4. low-viscosity double-component epoxy resin embedding adhesive according to claim 1; It is characterized in that: said glycidyl ether is 1, a kind of or wherein multiple mixture in 4-butanediol diglycidyl ether, hexanediol diglycidyl ether, ethylene glycol diglycidylether, benzyl glycidyl ether and the butylglycidyl ether.
5. low-viscosity double-component epoxy resin embedding adhesive according to claim 1 is characterized in that: said silicone antifoam agent is polysiloxane defoamers or organic silicon modified by polyether skimmer.
6. low-viscosity double-component epoxy resin embedding adhesive according to claim 1 is characterized in that: said acid anhydrides is a kind of in methyl tetrahydrophthalic anhydride and the methylhexahydrophthalic anhydride or both mixtures.
7. low-viscosity double-component epoxy resin embedding adhesive according to claim 1 is characterized in that: said quaternary ammonium salt is a kind of or wherein multiple mixture in DTAC, tetradecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride and the two dodecyl dimethyl ammonium chloride.
8. the preparation method of the described low-viscosity double-component epoxy resin embedding adhesive of claim 1 is characterized in that comprising the steps:
(1) preparation A component: bisphenol A epoxide resin, glycidyl ether and silicone antifoam agent are mixed, and be stirred to and mix; Add mineral black and filler while stirring then; After mineral black and filler all add, continue again to stir, bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler are mixed; Mixture to bisphenol A epoxide resin, glycidyl ether, silicone antifoam agent, mineral black and filler carries out vacuum defoamation then, obtains the A component;
(2) preparation B component: quaternary ammonium salt is joined in the acid anhydrides, and be stirred to and mix; Mixture to quaternary ammonium salt and acid anhydrides carries out vacuum defoamation then, obtains the B component;
(3) preserve separately 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 (2.5～4.0): 1 part by weight mixes; And be stirred to and mix, carry out vacuum defoamation then, obtain required low-viscosity double-component epoxy resin embedding adhesive.
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| CN102337003B (en) * | 2011-06-17 | 2012-11-14 | 莱州市顺利达电子材料有限公司 | Epoxy resin encapsulating material modified by organosilicon, its preparation method and its application |
| CN102515626B (en) * | 2012-01-06 | 2013-05-29 | 桂林理工大学 | High heat-conductivity epoxy casting material for dry power transformer and preparation method thereof |
| CN103050416B (en) * | 2012-12-07 | 2015-07-15 | 中国电子科技集团公司第十一研究所 | Bottom filling method and device for megapixel tellurium-cadmium-mercury hybrid chip |
| CN107189734A (en) * | 2017-05-27 | 2017-09-22 | 中昊(大连)化工研究设计院有限公司 | A kind of transparent, low halogen, color inhibition epoxy pouring sealant and preparation method thereof |
| CN107384278A (en) * | 2017-07-26 | 2017-11-24 | 合肥同佑电子科技有限公司 | A kind of mildew-proof flame retarded electron pouring sealant and preparation method thereof |
| CN110903796A (en) * | 2019-12-10 | 2020-03-24 | 南京工程学院 | High-toughness bridge reinforcing structure adhesive |
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