CN102702682A - Liquid epoxy resin composition for packaging LED (Light Emitting Diode) - Google Patents
Liquid epoxy resin composition for packaging LED (Light Emitting Diode) Download PDFInfo
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- CN102702682A CN102702682A CN2012101720424A CN201210172042A CN102702682A CN 102702682 A CN102702682 A CN 102702682A CN 2012101720424 A CN2012101720424 A CN 2012101720424A CN 201210172042 A CN201210172042 A CN 201210172042A CN 102702682 A CN102702682 A CN 102702682A
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Abstract
The invention discloses a liquid epoxy resin composition for packaging an LED (Light Emitting Diode). The liquid epoxy resin composition consists of an agent A and an agent B, wherein the agent A comprises 97-99 percent by weight of epoxy resin composition and 1-3 percent by weight of defoaming agent; the agent B comprises 94-97 percent by weight of alicyclic anhydride, 0.02-0.1 percent by weight of antioxidant, 0.02-0.1 percent by weight of ultraviolet absorber, 2-5 percent by weight of toughening modifier and 0.5-1.5 percent by weight of accelerator; and the weight ratio of the agent A to the agent B is 100:(100-105). The epoxy resin composition in the agent A is bisphenol-A epoxy resin and 3,4-epoxy cyclohexylmethyl and 3,4-epoxycyclohexyl carboxylate; and the alicyclic anhydride in the agent B is at least one of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and hexahydrophthalic anhydride; and the toughening modifier is neopentyl glycol. The neopentyl glycol has a structure of a branched chain, so that the flexibility and the cracking resistance of the cured epoxy resin are remarkably improved.
Description
Technical field
The present invention relates to be used for the liquid resin of LED encapsulation usefulness, liquid epoxy resin composition is used in a kind of LED encapsulation.
Background technology
Common LED encapsulation is difficult to satisfy the requirement of high-powered LED lamp with liquid epoxies viscosity high (being more than the 10000CPS under the room temperature), second-order transition temperature low (about 110 ℃).
Chinese patent CN201010166012 discloses a kind of composition epoxy resin, is made up of A glue and B glue, and A glue comprises epoxy resin composition, mill base and skimmer, and wherein epoxy resin composition is mixed by cycloaliphatic epoxy resin and bisphenol-type epoxy resin; B glue comprises anhydride curing agent, and curing catalyst solidifies modifying agent and inhibitor, and wherein solidifying modifying agent employing structural formula is OH-(CH
2) the glycols organic cpds of n-OH (n=2-12).This composition epoxy resin has lower viscosity before solidifying, and higher glass transition temperature is arranged after the curing, and is still relatively poor at the snappiness and the resistance to cracking of cured article, also needs to improve.
Summary of the invention
The present invention is intended to propose a kind of snappiness and liquid epoxy resin composition is used in resistance to cracking LED encapsulation preferably.
This LED encapsulation is made up of A agent and B agent two portions with liquid epoxy resin composition; The composition of A agent is 97 ~ 99wt% epoxy resin composition and 1 ~ 3wt% skimmer; The composition of B agent is alicyclic acid anhydrides, 0.02 ~ 0.1wt% oxidation inhibitor, 0.02 ~ 0.1wt% uv-absorbing agent, 2 ~ 5w1% plasticized modifier and the 0.5 ~ 1.5wt% promotor of 94 ~ 97wt%, and the weight ratio of A agent and B agent is 100: 100 ~ 105.Epoxy resin composition in the A agent is bisphenol A type epoxy resin and 3; 4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate, wherein 3,4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate accounts for 10 ~ 20wt% of epoxy resin total amount, and bisphenol A type epoxy resin accounts for 80 ~ 90wt% of epoxy resin total amount.Alicyclic acid anhydrides in the B agent is at least a in methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, the hexahydrophthalic anhydride, and described plasticized modifier is a NSC 6366.
This LED encapsulation uses liquid epoxy resin composition to adopt NSC 6366 to be plasticized modifier, owing to NSC 6366 has the structure of side chain snappiness and resistance to cracking behind the epoxy resin cure is improved significantly.
Embodiment
Liquid epoxy resin composition is used in this LED encapsulation; Form by A agent and B agent two portions; The composition of A agent is 97 ~ 99wt% epoxy resin composition and 1 ~ 3wt% skimmer; The composition of B agent is alicyclic acid anhydrides, 0.02 ~ 0.1wt% oxidation inhibitor, 0.02 ~ 0.1wt% uv-absorbing agent, 2 ~ 5wt% plasticized modifier and the 0.5 ~ 1.5wt% promotor of 94 ~ 97wt%, and the weight ratio of A agent and B agent is 100: 100 ~ 105.
Epoxy resin composition in the A agent is bisphenol A type epoxy resin and 3; 4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate, wherein 3,4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate accounts for 10 ~ 20wt% of epoxy resin total amount, and bisphenol A type epoxy resin accounts for 80 ~ 90wt% of epoxy resin total amount.The structural formula of bisphenol A type epoxy resin is:
The epoxy equivalent (weight) of bisphenol A type epoxy resin is best about 200g ∕ eq, because the modest viscosity of this epoxy resin at 150-300g ∕ eq especially.
3,4-epoxycyclohexyl methyl 3, the structural formula of 4-epoxycyclohexyl manthanoate is:
Alicyclic acid anhydrides in the B agent is at least a in methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, the hexahydrophthalic anhydride, and described plasticized modifier is a NSC 6366.
In the anhydride curing agent in anhydride group and the epoxy resin equivalence ratio of epoxide group be 0.8 ~ 1.2.
Promotor can be adopted imidazoles, at least a in liquid amine and the solid ammonium salt.Oxidation inhibitor can be in Hinered phenols antioxidant, phosphorous acid ester, the thioesters at least a.Uv-absorbing agent can adopt at least a in benzotriazole, the Benzophenones.
Introduce embodiment below.
Analytical procedure and comparative approach are:
1, the mensuration of viscosity: adopt homemade NDJ-97 type viscometer determining, 40 ℃ of water temperatures.
2, gelation is measured: adopt the HG-B type gel time determinator of Tianjin brilliance instrument plant, measure 150 ℃ of temperature.
3, flexural strength is measured: the electronic universal experimental machine that adopts Jilin Hua Yang plant and instrument factory.
4, voltage breakdown adopts the voltage breakdown experiment instrument of Jilin Hua Yang plant and instrument factory.
5, second-order transition temperature (Tg) is measured, the DSC method.
6, the mensuration of transmittance adopts 722 type spectrophotometers, measures the transmittance of cured article 400nm, and sample is the transparent cured thing of thickness 2mm, in mirror surface mould, solidifies.
7, water-intake rate is measured, and φ 50 * 3mm solidified sample is put into 100 ℃ of boiling water boil 2H, and the weight before and after record is put into is respectively W1 and W2, and then water-intake rate is (W2-W1)/11 * 100%.
8, cracking behavior experiment; After adopting the metal washer of external diameter φ 12 packaged, sample number is N=5, with 50 ℃/30 minutes+0 ℃/30 minutes as a circulation; The contact site of observing metal washer and resin has or not cracking phenomena to take place, and writes down the cycle number of passing through.
Synthetic example 1 (A agent 1): in the stainless steel cauldron of the 5L of charged heating and vacuum unit, add 1800 gram bisphenol A type epoxy resins (Mitsui Chemicals manufacturing R139S, epoxy equivalent (weight) 190g/eq); Heat rise to 80 ℃ after, add 200 grams 3,4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate (Hubei Xinjing New Material Co., Ltd., epoxy equivalent (weight) 130g/eq), skimmer 2 grams (moral modest chemical 5300); Be warming up to 110 ℃ after stirring; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Synthetic example 2 (A agent 2): in the stainless steel cauldron of the 5L of charged heating and vacuum unit, add 1600 and restrain bisphenol A type epoxy resins (Mitsui Chemicals system R139S, epoxy equivalent (weight) 190g/eq); Heat rise to 80 ℃ after, add 400 grams 3,4-epoxycyclohexyl methyl 3; 4-epoxycyclohexyl manthanoate (Hubei Xinjing New Material Co., Ltd., epoxy equivalent (weight) 130g/eq), skimmer 2 grams (moral modest chemical 5300); Be warming up to 110 ℃ after stirring; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Synthetic example 3 (B agent 1): in the stainless steel cauldron of the 5L of charged heating and vacuum unit; Add 1930 gram methylhexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system MEHHPA), heat rise to 80 ℃ after, add 10 and restrain N; N-dimethyl benzylamine (the newer chemical industry manufacturing in Changzhou); NSC 6366 50 grams (Korea S LG chemistry system), oxidation inhibitor 2,6-di-t-butyl-4-sylvan 1 gram (Jinan Genesis chemical industry system); Uv-absorbing agent 2-hydroxyl-4-methoxy benzophenone 1 gram (Xiangfan City's gold is translated into fine chemistry industry system) warming while stirring to 100 ℃; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Iorr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Synthetic example 4 (B agent 2): in the stainless steel cauldron of the 5L of charged heating and vacuum unit; Add 1900 gram methylhexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system MEHHPA), heat rise to 80 ℃ after, add 20 and restrain N; N-dimethyl benzylamine (the newer chemical industry manufacturing in Changzhou); NSC 6366 80 grams (Korea S LG chemistry system), oxidation inhibitor 2,6-di-t-butyl-4-sylvan 1 gram (Jinan Genesis chemical industry system); Uv-absorbing agent 2-hydroxyl-4-methoxy benzophenone 1 gram (Xiangfan City's gold is translated into fine chemistry industry system) warming while stirring to 100 ℃; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
5 (the B agent 3) of synthetic example: in the stainless steel cauldron of the 5L of charged heating and vacuum unit, add 1960 and restrain methylhexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system MEHHPA), heat rise to 80 ℃ after; Add 20 gram N; N-dimethyl benzylamine (the newer chemical industry manufacturing in Changzhou), 20 grams 1,4-butyleneglycol (manufacturing of Huidong, Shanghai chemical industry); Oxidation inhibitor 2; 6-di-t-butyl-4-sylvan 1 gram (Jinan Genesis chemical industry system), uv-absorbing agent 2-hydroxyl-4-methoxy benzophenone 1 gram (Xiangfan City's gold is translated into fine chemistry industry system) warming while stirring to 100 ℃ keeps temperature; Vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Synthetic example 6 (B agent 4): in the stainless steel cauldron of the 5L of charged heating and vacuum unit; Add 1500 gram methylhexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system MEHHPA) and 400 gram hexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system HHPA), heat rise to 80 ℃ after, adding 20 restrains N; N-methylbenzylamine (the newer chemical industry manufacturing in Changzhou); NSC 6366 80 grams (Korea S LG chemistry system), oxidation inhibitor 2,6-di-t-butyl-4-sylvan 1 gram (Jinan Genesis chemical industry system); Uv-absorbing agent 2-hydroxyl-4-methoxy benzophenone 1 gram (Xiangfan City's gold is translated into fine chemistry industry system) warming while stirring to 100 ℃; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Synthetic example 7 (B agent 5): in the stainless steel cauldron of the 5L of charged heating and vacuum unit; Add 1300 gram methylhexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system MEHHPA) and 600 gram hexahydrophthalic anhydrides (Zhejiang platinum promise chemical industry system HHPA), heat rise to 80 ℃ after, adding 20 restrains N; N-dimethyl benzylamine (the newer chemical industry manufacturing in Changzhou); NSC 6366 80 grams (Korea S LG chemistry system), oxidation inhibitor 2,6-di-t-butyl-4-sylvan 1 gram (Jinan Genesis chemical industry system); Uv-absorbing agent 2-hydroxyl-4-methoxy benzophenone 1 gram (Xiangfan City's gold is translated into fine chemistry industry system) warming while stirring to 100 ℃; Keep temperature, vacuumize while stirring (vacuum tightness is to 3Torr) more than 30 minutes, be cooled to 60 ℃ after blowing.
Embodiment:
The A agent that synthetic example 1 and synthetic example 2 are made mixes the final vacuum deaeration with synthetic example 3 ~ synthetic example 7 prepared B agent respectively according to a certain ratio, inject in the metal die with the appearance cup in, be cured condition of cure: 90 ℃/2H+130 ℃/3H.Make the sample of embodiment 1 ~ 7 and reference examples.The gained sample is tested, and the result lists in the table 1, wherein synthetic example 2 and the reference examples that is combined as of synthesizing example 5.
Table 1
Can be known that by table 1 the LED encapsulation that obtains with method of the present invention is mixing low, the easy deaeration of back viscosity with liquid epoxy resin composition, cured article is of light color, intensity is high, and resistance to cracking can have greatly improved.
Claims (1)
1. liquid epoxy resin composition is used in a LED encapsulation; Be made up of A agent and B agent two portions, the composition of A agent is 97 ~ 99wt% epoxy resin composition and 1 ~ 3wt% skimmer, and the composition of B agent is alicyclic acid anhydrides, 0.02 ~ 0.1wt% oxidation inhibitor, 0.02 ~ 0.1wt% uv-absorbing agent, 2 ~ 5wt% plasticized modifier and the 0.5 ~ 1.5wt% promotor of 94 ~ 97wt%; The weight ratio of A agent and B agent is 100: 100 ~ 105; It is characterized in that the epoxy resin composition in the described A agent is bisphenol A type epoxy resin and 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate; Wherein 3; 4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate accounts for 10 ~ 20wt% of epoxy resin total amount, and bisphenol A type epoxy resin accounts for 80 ~ 90wt% of epoxy resin total amount; Alicyclic acid anhydrides in the described B agent is at least a in methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, the hexahydrophthalic anhydride, and described plasticized modifier is a NSC 6366.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103937159A (en) * | 2014-03-25 | 2014-07-23 | 佛山市南海新丝路绝缘材料有限公司 | High-performance heat-resisting epoxy resin compound for LED packaging |
| CN104031356A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | LED (light-emitting diode) pouring sealant |
| CN106674895A (en) * | 2016-12-13 | 2017-05-17 | 安徽兆利光电科技有限公司 | LED lamp flexible glue sealing resin |
| CN106700997A (en) * | 2016-12-27 | 2017-05-24 | 苏州兴创源新材料科技有限公司 | High temperature resistant packaging adhesive for large-power LED illuminating lamp and preparation method of high temperature resistant packaging adhesive |
| CN106700420A (en) * | 2016-12-13 | 2017-05-24 | 安徽兆利光电科技有限公司 | Polystyrene package resin of LED lamp |
| CN109321184A (en) * | 2018-10-08 | 2019-02-12 | 盐城东山精密制造有限公司 | A kind of packaging method of LED light source packaging plastic and indoor display screen |
| CN109825232A (en) * | 2019-02-27 | 2019-05-31 | 华南理工大学 | A kind of epoxy packages glue and preparation method thereof for LED |
| CN111471420A (en) * | 2020-04-09 | 2020-07-31 | 北京康美特科技股份有限公司 | Packaging adhesive and preparation method and application thereof |
| CN112341976A (en) * | 2019-08-07 | 2021-02-09 | 北京科化新材料科技有限公司 | Solid epoxy resin packaging material and preparation method and application thereof |
| CN113214602A (en) * | 2021-05-06 | 2021-08-06 | 厦门市宜帆达新材料有限公司 | Insulating resin composite material, high-voltage insulating sleeve and preparation method and application thereof |
| CN114163613A (en) * | 2020-09-10 | 2022-03-11 | 北京科化新材料科技有限公司 | Packaging material and preparation method and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103937159A (en) * | 2014-03-25 | 2014-07-23 | 佛山市南海新丝路绝缘材料有限公司 | High-performance heat-resisting epoxy resin compound for LED packaging |
| CN104031356A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | LED (light-emitting diode) pouring sealant |
| CN106674895A (en) * | 2016-12-13 | 2017-05-17 | 安徽兆利光电科技有限公司 | LED lamp flexible glue sealing resin |
| CN106700420A (en) * | 2016-12-13 | 2017-05-24 | 安徽兆利光电科技有限公司 | Polystyrene package resin of LED lamp |
| CN106700997A (en) * | 2016-12-27 | 2017-05-24 | 苏州兴创源新材料科技有限公司 | High temperature resistant packaging adhesive for large-power LED illuminating lamp and preparation method of high temperature resistant packaging adhesive |
| CN109321184A (en) * | 2018-10-08 | 2019-02-12 | 盐城东山精密制造有限公司 | A kind of packaging method of LED light source packaging plastic and indoor display screen |
| CN109825232A (en) * | 2019-02-27 | 2019-05-31 | 华南理工大学 | A kind of epoxy packages glue and preparation method thereof for LED |
| CN112341976A (en) * | 2019-08-07 | 2021-02-09 | 北京科化新材料科技有限公司 | Solid epoxy resin packaging material and preparation method and application thereof |
| CN111471420A (en) * | 2020-04-09 | 2020-07-31 | 北京康美特科技股份有限公司 | Packaging adhesive and preparation method and application thereof |
| CN114163613A (en) * | 2020-09-10 | 2022-03-11 | 北京科化新材料科技有限公司 | Packaging material and preparation method and application thereof |
| CN114163613B (en) * | 2020-09-10 | 2024-03-12 | 北京科化新材料科技有限公司 | Packaging material, preparation method and application thereof |
| CN113214602A (en) * | 2021-05-06 | 2021-08-06 | 厦门市宜帆达新材料有限公司 | Insulating resin composite material, high-voltage insulating sleeve and preparation method and application thereof |
| CN113214602B (en) * | 2021-05-06 | 2023-09-22 | 厦门市宜帆达新材料有限公司 | Insulating resin composite material, high-voltage insulating sleeve, and preparation methods and applications thereof |
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Application publication date: 20121003 |