CN101372608A - Epoxy resin encapsulation adhesive and use thereof - Google Patents
Epoxy resin encapsulation adhesive and use thereof Download PDFInfo
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- CN101372608A CN101372608A CNA2007100124911A CN200710012491A CN101372608A CN 101372608 A CN101372608 A CN 101372608A CN A2007100124911 A CNA2007100124911 A CN A2007100124911A CN 200710012491 A CN200710012491 A CN 200710012491A CN 101372608 A CN101372608 A CN 101372608A
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- epoxy resin
- encapsulation adhesive
- antioxidant
- phosphorus
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Abstract
The invention relates to an encapsulation adhesive used for an electronic device, in particular to an epoxy resin encapsulation material for encapsulating a light emitting diode. The encapsulation adhesive has the advantages of good anti-optical weaken performance, short curing time, not getting yellow of the color of cured resin, good aging resistance, long operative time, etc. The encapsulation adhesive comprises two parts of component A and component B which are mixed to be used. The component A is A-typed bisphenol epoxy resin. The component B comprises methyl hexahydrophthalic anhydride, ethyl triphenyl iodo phosphonium, triphenylphosphine and beta-(3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid n-octadecanol antioxidant. The mass ratio of A to B is 1 to 0.8-1.
Description
Technical field
The present invention relates to a kind of encapsulating adhesive of electronic devices and components, particularly relate to the tackiness agent that can be used to the encapsulating light emitting diode.
Background technology
The encapsulating adhesive of electronic devices and components is to be mixed by a certain percentage by Resins, epoxy, solidifying agent, and for a change its performance makes it to satisfy different needs, suitably adds promotor, antioxidant etc. again.Select different materials for use or change the proportioning of various compositions, can influence the optical property of packaged material greatly.Particularly in light emitting diode packaged material field, need light transmission good, the light decay rate is low, the encapsulating adhesive that internal stress is little.Shortcomings such as present light-emitting diode packaging material mainly adopts the quaternary ammonium salt material as promotor, and material solidified Resins, epoxy easily produces yellow thus, and produces big internal stress in the solidification process, and it causes the product light transmission bad, and is easily aging.
Summary of the invention
The technical problem to be solved in the present invention provides that a kind of anti-light decay performance is good, and set time is shorter, the not flavescence of cured article color, and ageing resistance is good, the packaged material that operable time is long.
For this reason, a kind of Resins, epoxy is matrix with the bisphenol A type epoxy resin, selecting methyl hexahydrophthalic anhydride for use for the weathering resistance of giving the high translucidus of packaging plastic and get well is solidifying agent, because methyl hexahydrophthalic anhydride is originally as colourless transparent liquid, and compare with existing most of acid anhydrides, do not contain unsaturated link(age) among its molecular structure, increased the weathering resistance of cured resin for this reason; In order to give low internal stress of packaging plastic and high translucidus, the present invention has selected for use by ethyltriphenylphosphiodide iodide phosphorus, the composite promotor of triphenyl phosphorus, because of it has promoter action, antioxygenation concurrently, organophosphorus can also slow down the heat effect of solidification process in addition, can make encapsulating adhesive have the low and high advantage of light transmission of internal stress thus.
Be prepared into two kinds of components of A, B in advance.For example:
The preparation of A component: 42 gram bisphenol A type epoxy resin matrixes.
The preparation of B component: in the 40g methyl hexahydrophthalic anhydride, add an amount of (for example 0.42 gram) ethyltriphenylphosphiodide iodide phosphorus accelerant and 0.08 gram triphenyl phosphorus, add the β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid of 1.025 grams again.The B component is positioned in the oil bath pan under the certain temperature mixed stir about 30 minutes.
During use A, B component are mixed according to the ratio of mass ratio 1:1, the back that stirs is not more than in the vacuum drying oven of 10mm mercury column in vacuum tightness and both had been packaging plastic after 50 ℃ of deaerations.
Method for filling: place 130 ℃ baking oven preheating after 1 hour on the tetrafluoroethylene mould, spray into a small amount of remover, pour into packaging plastic, place 130 ℃ baking oven afterwards, be incubated after 50 minutes and take out, naturally cool to room temperature.
Above-mentioned consumption uses in the time of can being converted to following mass percent for the increasing consumption: the A component is bisphenol A type epoxy resin; Methyl hexahydrophthalic anhydride solidifying agent during preparation B component, ethyltriphenylphosphiodide iodide phosphorus, triphenyl phosphorus, β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid antioxidant accounts for 95%～98%, 0.8%～1.5% of B component total mass respectively, 0.15%～0.22%, 1%～3%.
Through experiment test, epoxy encapsulation glue provided by the invention has following performance:
Second-order transition temperature 〉=127 ℃
124 ℃ of heat-drawn wires
Shock strength 〉=4.87kJ/m
2
Flexural strength 〉=131MPa
Hardness 〉=97
Water-intake rate≤0.1%
Specific refractory power 1.55
Light decay≤15%
25 ℃ of (10kH of electrical insulating property
Z) 3.0
25 ℃ of (10kH of dielectric loss
Z) 0.011
Above-mentioned data show that characteristics of the present invention are that anti-light decay performance is good, and set time is shorter, the not flavescence of cured article color, and ageing resistance is good, and operable time is long.
Specific embodiment
Provide several preferred embodiments of epoxy encapsulation glue involved in the present invention below.Therefrom as can be seen: the quality of a composition that scales up wherein can not change the performance of packaging plastic yet.
Embodiment 1
The preparation of A component: 14.4 gram bisphenol A type epoxy resins.
The preparation of B component: in 14 gram methyl hexahydrophthalic anhydride solidifying agent, add the compound accelerant that an amount of (for example 0.115 gram) ethyltriphenylphosphiodide iodide phosphorus and 0.022 gram triphenyl phosphorus are formed, add 0.302 gram β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid antioxidant then.In 60 ℃ of oil baths, mix and stirred 30 minutes.
A, B component are mixed according to mass ratio 1:1, and the back that stirs is not more than 50 ℃ of deaerations in the vacuum drying oven of 10mm mercury column in vacuum tightness.
Method for filling: place 130 ℃ baking oven preheating after 1 hour on the tetrafluoroethylene mould, spray into a small amount of remover, pour into packaging plastic, place 130 ℃ baking oven afterwards, be incubated after 50 minutes and take out, naturally cool to room temperature.
Embodiment 2
The preparation of A component: with 72.6 gram bisphenol A type epoxy resins.
The preparation of B component: in 70 gram methyl hexahydrophthalic anhydride solidifying agent, add an amount of (for example 0.7 gram) ethyltriphenylphosphiodide iodide phosphorus and 0.14 gram triphenyl phosphorus promotor, add 1.71 gram β-positive octadecanol esters of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid then.In 60 ℃ of oil baths, mix and stirred 30 minutes.
A, B component are mixed according to mass ratio 1:1, and the back that stirs is not more than 50 ℃ of deaerations in the vacuum drying oven of 10mm mercury column in vacuum tightness.
Method for filling: place 130 ℃ baking oven preheating after 1 hour on the tetrafluoroethylene mould, spray into a small amount of remover, pour into packaging plastic, place 130 ℃ baking oven afterwards, be incubated after 50 minutes and take out, naturally cool to room temperature.
Embodiment 3
The preparation of A component: with 364.2 gram bisphenol A type epoxy resins.
The preparation of B component: in 350 gram methyl hexahydrophthalic anhydride solidifying agent, add an amount of (for example 4.2 grams) ethyltriphenylphosphiodide iodide phosphorus and 0.7 gram triphenyl phosphorus promotor, add 9.3 gram β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid antioxidants then.In 60 ℃ of oil baths, mix and stirred 30 minutes.
A, B component are mixed according to mass ratio 1:1, and the back that stirs is not more than 50 ℃ of deaerations in the vacuum drying oven of 10mm mercury column in vacuum tightness.
Method for filling: place 130 ℃ baking oven preheating after 1 hour on the tetrafluoroethylene mould, spray into a small amount of remover, pour into packaging plastic, place 130 ℃ baking oven afterwards, be incubated after 50 minutes and take out, naturally cool to room temperature.
Embodiment 4
The preparation of A component: with 2920 gram bisphenol A type epoxy resins.
The preparation of B component: in 2800 gram methyl hexahydrophthalic anhydride solidifying agent, add an amount of (for example 30 grams) ethyltriphenylphosphiodide iodide phosphorus and 6 gram triphenyl phosphorus promotor, add 82 gram β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid antioxidants then.In 60 ℃ of oil baths, mix and stirred 30 minutes.
A, B component are mixed according to mass ratio 1:1, and the back that stirs is not more than 50 ℃ of deaerations in the vacuum drying oven of 10mm mercury column in vacuum tightness.
Method for filling: place 130 ℃ baking oven preheating after 1 hour on the tetrafluoroethylene mould, spray into a small amount of remover, pour into packaging plastic, place 130 ℃ baking oven afterwards, be incubated after 50 minutes and take out, naturally cool to room temperature.
In the time of from above-mentioned four embodiment, can calculating preparation B component, methyl hexahydrophthalic anhydride solidifying agent, ethyltriphenylphosphiodide iodide phosphorus, triphenyl phosphorus, β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid antioxidant accounts for 95%～98% of B component total mass respectively, 0.8%～1.5%, 0.15%～0.22%, 1%～3%.
The performance test results such as following table to all packaging plastic samples:
| Embodiment | Second-order transition temperature (℃) | Heat-drawn wire (℃) | Shock strength (kJ/m 2) | Flexural strength (MPa) | Hardness | Water-intake rate (%) | Specific refractory power | Light decay (%) | 25 ℃ of 10kH of electrical insulating property Z | 25 ℃ of 10kH of dielectric loss Z |
| 1 | 127 | 123 | 4.88 | 131 | 97 | 0.89 | 1.52 | 14.2 | 3.06 | 0.010 |
| 2 | 128 | 124 | 4.90 | 133 | 99 | 0.95 | 1.53 | 13.4 | 3.12 | 0.009 |
| 3 | 128 | 125 | 4.88 | 132 | 98 | 0.88 | 1.56 | 13.7 | 3.16 | 0.013 |
| 4 | 127 | 124 | 4.87 | 131 | 97 | 0.93 | 1.59 | 14.5 | 3.08 | 0.011 |
Above-mentioned real result shows: characteristics of the present invention are that anti-light decay performance is good, and set time is shorter, the not flavescence of cured article color, and ageing resistance is good, and operable time is long.
Claims (3)
1. an epoxy resin encapsulation adhesive is made up of A, B two components, the A component is a Resins, epoxy, the B component is that solidifying agent, promotor, antioxidant are prepared from proportion in advance, then A, B two components are mixed the encapsulating adhesive that uses, it is characterized in that: the Resins, epoxy among the component A is bisphenol A type epoxy resin; Solidifying agent in the B component is that methyl hexahydrophthalic anhydride, promotor are ethyltriphenylphosphiodide iodide phosphorus and triphenyl phosphorus, methyl hexahydrophthalic anhydride, ethyltriphenylphosphiodide iodide phosphorus, triphenyl phosphorus, antioxidant account for total mass in B mass percent is respectively 95%～98%, 0.8%～1.5%, 0.15%～0.22%, 1%～3%; A, B component blended mass ratio are 1:0.8～1.
2. according to right 1 described epoxy resin encapsulation adhesive, it is characterized in that: the antioxidant in the B component is β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid, and its molecular formula is as follows:
3. any one described epoxy resin encapsulation adhesive is used for the encapsulation of photodiode in the right 1 to 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100124911A CN101372608A (en) | 2007-08-20 | 2007-08-20 | Epoxy resin encapsulation adhesive and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100124911A CN101372608A (en) | 2007-08-20 | 2007-08-20 | Epoxy resin encapsulation adhesive and use thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101372608A true CN101372608A (en) | 2009-02-25 |
Family
ID=40446995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100124911A Pending CN101372608A (en) | 2007-08-20 | 2007-08-20 | Epoxy resin encapsulation adhesive and use thereof |
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| CN (1) | CN101372608A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805577A (en) * | 2010-04-09 | 2010-08-18 | 东莞市天环科技有限公司 | Transparent epoxy resin packaging adhesive |
| CN101819953A (en) * | 2010-04-09 | 2010-09-01 | 东莞市天环科技有限公司 | Transparent epoxy resin packaging adhesive |
| CN101692473B (en) * | 2009-09-11 | 2011-03-30 | 中蓝晨光化工研究院有限公司 | Photocuring light-emitting diode encapsulation material |
| CN102977557A (en) * | 2012-12-11 | 2013-03-20 | 蓝星(北京)化工机械有限公司 | Room temperature curing epoxy resin composition and preparation method thereof |
| CN103382378A (en) * | 2013-07-23 | 2013-11-06 | 张运泉 | Weather-resistant epoxy adhesive |
| CN104031589A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | Heat stabilized type LED (Light Emitting Diode) sealant |
-
2007
- 2007-08-20 CN CNA2007100124911A patent/CN101372608A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692473B (en) * | 2009-09-11 | 2011-03-30 | 中蓝晨光化工研究院有限公司 | Photocuring light-emitting diode encapsulation material |
| CN101805577A (en) * | 2010-04-09 | 2010-08-18 | 东莞市天环科技有限公司 | Transparent epoxy resin packaging adhesive |
| CN101819953A (en) * | 2010-04-09 | 2010-09-01 | 东莞市天环科技有限公司 | Transparent epoxy resin packaging adhesive |
| CN101819953B (en) * | 2010-04-09 | 2011-10-26 | 东莞市天环科技有限公司 | Transparent epoxy resin packaging adhesive |
| CN102977557A (en) * | 2012-12-11 | 2013-03-20 | 蓝星(北京)化工机械有限公司 | Room temperature curing epoxy resin composition and preparation method thereof |
| CN102977557B (en) * | 2012-12-11 | 2015-11-18 | 蓝星(北京)化工机械有限公司 | A kind of room temperature curing epoxy composition and method of making the same |
| CN103382378A (en) * | 2013-07-23 | 2013-11-06 | 张运泉 | Weather-resistant epoxy adhesive |
| CN104031589A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | Heat stabilized type LED (Light Emitting Diode) sealant |
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Open date: 20090225 |