CN102850988A - Epoxy resin pouring sealant and usage method - Google Patents

Epoxy resin pouring sealant and usage method Download PDF

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Publication number
CN102850988A
CN102850988A CN201210364115XA CN201210364115A CN102850988A CN 102850988 A CN102850988 A CN 102850988A CN 201210364115X A CN201210364115X A CN 201210364115XA CN 201210364115 A CN201210364115 A CN 201210364115A CN 102850988 A CN102850988 A CN 102850988A
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epoxy resin
embedding adhesive
resin embedding
sio
pouring sealant
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CN102850988B (en
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卢安贤
罗志伟
刘学峰
陈兴军
瞿高
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Central South University
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Central South University
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Abstract

The invention relates to an epoxy resin pouring sealant and a usage method. The epoxy resin pouring sealant is composed of an o-cresol-formaldehude epoxy resin matrix, a methylhexahydrophthalic anhydride curing agent, an electronic grade torispherical silica micro powder filler, a diluent and an antifoaming agent, wherein the composition ratio of the epoxy resin matrix to the curing agent is 1: (0.6-1.4), and the composition ratio of the epoxy resin matrix to the filler is 1: (0.3-2.4). According to the epoxy resin pouring sealant, a curing process is that pre-curing is performed at the temperature of 90 DEG C for 0.5-1 hour, and curing is performed at the temperature of 150 DEG C for 2-3 hours. The epoxy resin pouring sealant has the advantages of being low in toxicity, density, thermal expansivity coefficient and water absorption rate, high in bending strength and compressive strength and good in application prospect and can be widely applied to electronic controllers, sensors, aerospace components and the like.

Description

A kind of epoxy resin embedding adhesive and using method
Technical field
The present invention relates to epoxy resin embedding adhesive and the using method of a kind of epoxy resin embedding adhesive and using method, particularly low thermal coefficient of expansion, high bending resistance and ultimate compression strength.Belong to the production of adhesive technical field.
Background technology
Joint sealant claims again electronic pastes, is a widely address.Be used for the bonding of electronic devices and components, sealing, embedding and coating protection.It is liquid that joint sealant belongs to before uncured, has flowability, and the glue viscosity is according to the difference of the material of product, performance, production technique and to some extent difference.Could realize its use value after joint sealant solidifies fully, can play waterproof and dampproof, dustproof, insulation, heat conduction after the curing, maintain secrecy, protection against corrosion, heatproof, shockproof effect.Along with the expansion of range of application, the over-all properties of joint sealant material is had higher requirement.
Particularly abroad to the existing more report of epoxy resin embedding adhesive material, the more application example is arranged also both at home and abroad.Application number is the preparation method that 200610150880.6 Chinese patent has been reported modified phenolic resins in low viscosity, fire resistant joint sealant and this glue, mainly is the application for high temperature resistant element.Application number is that 200710138788.2 Chinese patent has been reported acid resistance epoxy resin embedding adhesive and preparation method thereof, and what solved mainly that lead acid cell often occurs climbs acid, leaks the problems such as acid.Application number is that 200910059237.6 Chinese patent has been reported a kind of low density, high impact properties epoxy resin embedding adhesive and preparation method thereof, lay particular emphasis on the shock resistance of material, the material of its acquisition is applicable to the embedding of the electric elements under miniaturization, lightweight, the shock resistance condition.Application number is that 200680018614.6 Chinese patent has been reported a kind of resin combination and goods prepared therefrom with low thermal coefficient of expansion, and the thermal expansivity of this material is about 10 ~ 50 * 10 -6/ ℃, but do not relate to the performance of the aspects such as bending strength or ultimate compression strength.Polymkeric substance in its chemical constitution is the resin combinations such as polyimide, polyester-imide, and packing material is graphite, and the preparation method is powder compression, compression molding, basic molding etc., is mainly used in wear ring or packing ring.Above-mentioned patent special emphasis separately is all not identical.The epoxy resin encapsulated material that satisfies simultaneously low thermal coefficient of expansion, high bending resistance and ultimate compression strength not yet has report.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and provide a kind of reasonable mixture ratio of components, curing process simple, lower-cost low thermal coefficient of expansion, bending resistance, epoxy resin embedding adhesive and using method that ultimate compression strength is high.
A kind of epoxy resin embedding adhesive of the present invention comprises that following component forms by weight:
Figure BDA00002193204700021
Described Resins, epoxy is solid-state o-cresol formaldehyde epoxy resin, 200 mesh sieves; Described solidifying agent is liquid methylhexahydrophthalic anhydride; Described filler is SiO 2Micro mist, described SiO 2Micro mist is the electronic-grade torispherical, SiO 2The SiO of content 〉=98.5% 2Micro mist is crossed 400 mesh sieves.Described thinner is a kind of in dimethylbenzene, ethanol or the acetone; Described defoamer is the emulsion paint defoamer, and described emulsion paint is produced by good this specialization of Changzhou worker company limited with defoamer, and product type is: the SPA-200 defoamer.
The using method of a kind of epoxy resin embedding adhesive of the present invention is sketched in lower:
Weight part by the epoxy resin embedding adhesive component that designs is got each component, at first, Resins, epoxy, filler, mixing diluents is stirred, then, under whipped state, add solidifying agent and be heated to 90 ℃, after thing to be mixed dissolves into liquid state, add defoamer, continue to stir 10-30 minute, after stirring is finished, it can be coated in by embedding thing surface, room temperature places vacuum drying oven after leaving standstill Procuring in 0.5-1 hour, 150 ℃, constant temperature 2 ~ 3 hours fully solidifies.
The present invention has carried out the optimization of a large amount of Composition Design and curing process to the epoxy resin encapsulated material, through comparison and screening repeatedly, prepared the epoxy resin encapsulated material of low thermal coefficient of expansion, high bending resistance and ultimate compression strength.
The present invention is owing to adopting the said components proportioning, selecting the lower o-cresol formaldehyde epoxy resin of thermal expansivity is matrix, selecting liquid heat-curing type anhydrides methyl hexahydrophthalic anhydride is solidifying agent, has that fusing point title complex viscosity low, that form with cycloaliphatic epoxy resin is low, working life long, the thermotolerance of cured article is high, electrical properties in high temperatures good; The torispherical silicon powder of introducing electronic-grade is weighting agent, and the internal friction of torispherical silicon powder in resin or colloidal sol is little, can reduce the viscosity of mixture systems, improves the filling ratio of silicon powder; And can improve the dispersed and mobile of mixture system, increase the intensity of material, thereby strengthen physical strength, Young's modulus, the ageing-resistant performance of cured product, corrosion resistance etc.The present invention is by the optimization design to main ingredient, and the density of the epoxy resin embedding adhesive material that obtains is lower, and thermal linear expansion coefficient is lower, between-10.04 ~ 35.24 (10 -6/ K) between, even be negative value at the thermal expansivity of some temperature range, this result will widen the range of application of epoxy resin embedding adhesive material greatly.The bending strength of material reaches as high as 187MPa, ultimate compression strength reaches as high as 683MPa, and (25 ℃ of lower water-intake rates, water-bath 48h), make the over-all properties of epoxy resin embedding adhesive material obtain larger improvement, over-all properties is higher than the epoxy resin embedding adhesive material of domestic and international similar system far away.This epoxy resin embedding adhesive material preparation method is simple, and curing process is simple, and production cost is lower.And this Embedding Material has the characteristic of low toxicity, low density, low thermal coefficient of expansion, low water absorption and high bending resistance and ultimate compression strength, can be widely used in electronic regulator, sensor, space flight element etc., and application prospect is good.
Description of drawings
Accompanying drawing 1 is the thermal expansivity curve after the epoxy resin embedding adhesive of the embodiment of the invention 3 preparations solidifies.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
Embodiment 1:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700031
Embodiment 2: the epoxy resin embedding adhesive material of the low thermal coefficient of expansion that the present invention relates to, high bending resistance and ultimate compression strength, the content of each component is
Figure BDA00002193204700032
Embodiment 3:
The epoxy resin embedding adhesive of preparation, the content of each component is
Embodiment 4:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700034
Embodiment 5:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700041
Embodiment 6:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700042
Embodiment 7:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700043
Embodiment 8:
The epoxy resin embedding adhesive of preparation, the content of each component is
Figure BDA00002193204700044
The chemical constitution of the epoxy resin embedding adhesive material of each embodiment preparation is different, but using method is close, detailed process is: the weight part by the epoxy resin embedding adhesive component that designs is got each component, at first, with Resins, epoxy, filler, mixing diluents stirs, and then, adds solidifying agent and be heated to 90 ℃ under whipped state, after thing to be mixed dissolves into liquid state, add defoamer, continue to stir 10-30 minute, after stirring is finished, it can be coated in by embedding thing surface, room temperature places vacuum drying oven after leaving standstill Procuring in 0.5-1 hour, 150 ℃, constant temperature 2 ~ 3 hours fully solidifies.
Performance index after the epoxy resin embedding adhesive of each specific embodiment preparation of the present invention solidifies are listed in the table 1.
Table 1
Figure BDA00002193204700051

Claims (7)

1. epoxy resin embedding adhesive comprises that following component forms by weight:
Figure FDA00002193204600011
2. epoxy resin embedding adhesive according to claim 1, it is characterized in that: described Resins, epoxy is solid-state o-cresol formaldehyde epoxy resin, crosses 200 mesh sieves.
3. epoxy resin embedding adhesive according to claim 1 is characterized in that: described solidifying agent is liquid methylhexahydrophthalic anhydride.
4. epoxy resin embedding adhesive according to claim 1, it is characterized in that: described filler is SiO 2Micro mist, described SiO 2Micro mist is the electronic-grade torispherical, SiO 2The SiO of content 〉=98.5% 2Micro mist is crossed 400 mesh sieves.
5. epoxy resin embedding adhesive according to claim 1 is characterized in that: described thinner is a kind of in dimethylbenzene, ethanol or the acetone.
6. epoxy resin embedding adhesive according to claim 1, it is characterized in that: described defoamer is the emulsion paint defoamer.
7. the using method of the described epoxy resin embedding adhesive of any one according to claim 1-6, to get each component by the weight part of the epoxy resin embedding adhesive component that designs, at first, with Resins, epoxy, filler, mixing diluents stirs, then, under whipped state, add solidifying agent and be heated to 90 ℃, after thing to be mixed dissolves into liquid state, add defoamer, continue to stir 10-30 minute, after stirring is finished, it can be coated in by embedding thing surface, after room temperature leaves standstill Procuring in 0.5-1 hour, place vacuum drying oven, 150 ℃, constant temperature 2 ~ 3 hours fully solidifies.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103468193A (en) * 2013-09-17 2013-12-25 广州聚合电子材料有限公司 Low-halogen low-smell epoxy resin pouring sealant and preparation process thereof
CN106867438A (en) * 2017-03-06 2017-06-20 固德电材系统(苏州)股份有限公司 A kind of epoxy resin embedding adhesive and its application method
CN107556701A (en) * 2017-09-14 2018-01-09 江山海维科技有限公司 A kind of sensor epoxy resin manufacturing process
CN108165179A (en) * 2017-12-27 2018-06-15 惠州市杜科新材料有限公司 A kind of speaker voice coil high temperature resistant coating binder
WO2018121048A1 (en) * 2016-12-27 2018-07-05 苏州兴创源新材料科技有限公司 Heat-resistant packaging adhesive for high-power led and manufacturing method thereof
CN108774382A (en) * 2018-08-11 2018-11-09 甘肃恒路交通勘察设计院有限公司 A kind of preparation of sensor package material and method for testing performance
CN109385240A (en) * 2018-10-10 2019-02-26 广州聚合新材料科技股份有限公司 A kind of epoxy resin embedding adhesive and its preparation method and application
CN111684010A (en) * 2018-12-06 2020-09-18 浙江华飞电子基材有限公司 Liquid casting resin composition for ultrahigh-voltage device
CN113708002A (en) * 2021-09-29 2021-11-26 远景能源有限公司 Battery box and energy storage battery

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070293603A1 (en) * 2006-06-19 2007-12-20 Ashland Licensing And Intellectual Property Llc Epoxy adhesive composition and use thereof
CN102559115A (en) * 2011-12-22 2012-07-11 烟台德邦科技有限公司 Chip-level bottom filling adhesive and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070293603A1 (en) * 2006-06-19 2007-12-20 Ashland Licensing And Intellectual Property Llc Epoxy adhesive composition and use thereof
CN102559115A (en) * 2011-12-22 2012-07-11 烟台德邦科技有限公司 Chip-level bottom filling adhesive and preparation method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103468193B (en) * 2013-09-17 2016-05-18 广州聚合新材料科技股份有限公司 Epoxy resin embedding adhesive and the preparation technology thereof of the low smell of low halogen
CN103468193A (en) * 2013-09-17 2013-12-25 广州聚合电子材料有限公司 Low-halogen low-smell epoxy resin pouring sealant and preparation process thereof
WO2018121048A1 (en) * 2016-12-27 2018-07-05 苏州兴创源新材料科技有限公司 Heat-resistant packaging adhesive for high-power led and manufacturing method thereof
CN106867438A (en) * 2017-03-06 2017-06-20 固德电材系统(苏州)股份有限公司 A kind of epoxy resin embedding adhesive and its application method
CN107556701B (en) * 2017-09-14 2020-04-03 江山海维科技有限公司 Manufacturing process of epoxy resin for sensor
CN107556701A (en) * 2017-09-14 2018-01-09 江山海维科技有限公司 A kind of sensor epoxy resin manufacturing process
CN108165179A (en) * 2017-12-27 2018-06-15 惠州市杜科新材料有限公司 A kind of speaker voice coil high temperature resistant coating binder
CN108774382A (en) * 2018-08-11 2018-11-09 甘肃恒路交通勘察设计院有限公司 A kind of preparation of sensor package material and method for testing performance
CN109385240A (en) * 2018-10-10 2019-02-26 广州聚合新材料科技股份有限公司 A kind of epoxy resin embedding adhesive and its preparation method and application
CN109385240B (en) * 2018-10-10 2021-05-28 广州聚合新材料科技股份有限公司 Epoxy resin pouring sealant and preparation method and application thereof
CN111684010A (en) * 2018-12-06 2020-09-18 浙江华飞电子基材有限公司 Liquid casting resin composition for ultrahigh-voltage device
CN111684010B (en) * 2018-12-06 2023-08-04 浙江华飞电子基材有限公司 Liquid casting resin composition for ultrahigh-voltage device
CN113708002A (en) * 2021-09-29 2021-11-26 远景能源有限公司 Battery box and energy storage battery

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