CN104788899A - A highly-heat-resistant anti-yellowing thermosetting epoxy composition - Google Patents
A highly-heat-resistant anti-yellowing thermosetting epoxy composition Download PDFInfo
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- CN104788899A CN104788899A CN201510019294.7A CN201510019294A CN104788899A CN 104788899 A CN104788899 A CN 104788899A CN 201510019294 A CN201510019294 A CN 201510019294A CN 104788899 A CN104788899 A CN 104788899A
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Abstract
A highly-heat-resistant anti-yellowing thermosetting epoxy composition is disclosed. The composition is prepared by mixing following components by mass: 5-20% of epoxy resin having a molecule structure shown as a formula I, 5-25% of a curing agent, 0.2-1.2% of a curing accelerator, 0.01-2% of an internal releasing agent, 50-88% of pigment-filler, 0.01-2% of a coupling agent and 0.01-2.3% of an antioxidant, wherein the pigment-filler comprises an inorganic filler and white pigment according to a mass ratio of 1-4:1. The composition has higher heat resistance and excellent anti-yellowing performance, and can allow photosemiconductor LEDs to maintain high reflection rates and reliability in long-term high-temperature working.
Description
Technical field
The present invention relates to a kind of for photosemiconductor LED reflection body material, particularly one high heat-resistant xanthochromia thermoset epoxy composition.
Background technology
Along with technology is showing improvement or progress day by day, photosemiconductor LED and electron device are applied to increasing field, along with the needs that development and the user of photosemiconductor technology constantly promote, the power of photosemiconductor LED continues to increase, volume is also diminishing gradually, this to the stability of material and the requirement of reliability more and more higher.
The polyphthalamide PPA material that traditional technology uses, because it exists high temperature resistance difference, uvioresistant ability is weak, the problem of easy xanthochromia, and exist and metal bonding power poor, the shortcoming of easy water suction, can not ensure that component element long period is reliable and stable, therefore only with for lower than 1 watt of power component.And PCT material is the thermoplasticity light reflector base material of new generation developed on its basis, although strengthen to some extent than PPA material property in heat-resistant xanthochromia, at more high performance components, as more than 2 watts use time, stability still can not meet the demands.
Summary of the invention
The object of the present invention is to provide a kind of high heat-resistant xanthochromia thermoset epoxy composition, there is higher thermotolerance and excellent yellowing resistance energy, photosemiconductor LED reflection matrix can be improved under long-time hot operation, keep high-reflectivity and reliability.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of high heat-resistant xanthochromia thermoset epoxy composition, is mixed by the component of following mass percent:
Molecular formula is the epoxy resin 5-20% shown in formula I, solidifying agent 5-25%, curing catalyst 0.2%-1.2%, inner pattern releasing agent applicable 0.01%-2%, color stuffing 50-88%, coupling agent 0.01%-2%, oxidation inhibitor 0.01%-2.3%, wherein color stuffing is by mineral filler and white pigment the forming of mass ratio according to 1-4:1;
For the defect of current material, first the present invention improves base resin, the epoxy resin shown in specific formula I is selected to be matrix resin, epoxy resin shown in formula I has saturated carbon azepine ring, the thermostability that resin is good can be provided, the color and luster of resin is colourless or faint yellow simultaneously, can prepare the material that reflectivity is high, and not easy to change after being heated.Have selected specific solidifying agent material to improve the thermotolerance of material, after coordinating like this, the yellowing resistance of material can be good simultaneously.
As preferably, described solidifying agent is hydrogenating methyl carbic anhydride.Hydrogenating methyl carbic anhydride is saturated polynary ring, and the ring texture of molecule own has rigidity, and selective hydrogenation methylnadic anhydride is the resistance toheat that solidifying agent can improve product.
As preferably, described curing catalyst is selected from one or more in 1,8-diaza-two ring (5,4,0) undecylene-7,2-ethyl-4 Methylimidazole, triphenyl phosphorus.
As preferably, described inner pattern releasing agent applicable is selected from one or more in stearic acid, calcium stearate, Zinic stearas, aluminum stearate, oxidized polyethlene wax, palm wax.
As preferably, described mineral filler is selected from crystalline silicon powder, fusion silicon powder, ball-shaped silicon micro powder, calcium carbonate, aluminium hydroxide, magnesium hydroxide, wollastonite, barium carbonate, hydrotalcite the combination choosing one or more, and the size controlling of mineral filler is at 0.01-50 micron.
As preferably, described white pigment is selected from one or more in titanium dioxide, zinc oxide, aluminum oxide, magnesium oxide, zinc sulphide, and the size controlling of white pigment is at 0.01-8 micron.
As preferably, described coupling agent is selected from the one in silane resin acceptor kh-550, silane coupling agent KH-560, vinyltrimethoxy silane, titanic acid ester, Al-Ti-diffused steel.
As preferably, described oxidation inhibitor is selected from one or more in 2,6 ditertiary butyl p cresol, triphenyl phosphite, diphenylalkyl phosphites.
The preparation method of high heat-resistant xanthochromia thermoset epoxy composition, comprises the steps:
(1) mineral filler, white pigment, part oxidation inhibitor and coupling agent are turned/min mixing 5-10min at high-speed mixer high speed 2000-2200, at a slow speed 500-600 turn/min mixing obtains front batch mixing in 20-30 minute, the temperature of mixing process controls at 50 DEG C-130 DEG C;
Due in high-speed mixer, there is the problem of local superheating in powder friction, and therefore while interpolation coupling agent, adding portion oxidation inhibitor is protected coupling agent, prevents powder xanthochromia, thus improves the quality of product.Temperature controls at 50 DEG C-130 DEG C, more preferably 70 DEG C-110 DEG C, can not react not lower than 50 DEG C of coupling agent activity, can produce xanthochromia higher than 130 DEG C of powders; Mixing process first tells that rear low speed can prevent amount of localized heat too high, and the xanthochromia problem caused, the too short coupling agent of mixing time can not fully react, the oxidized xanthochromia of long then coupling agent.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable;
(3) undertaken mediating 10-30 minute to obtain Procuring thing 100 DEG C of-120 DEG C of Procuring by after epoxy resin, partially cured dose and curing catalyst mixing;
Epoxy resin is carried out Procuring by this step, advantage is: because the reactive behavior of hydrogenating methyl carbic anhydride is lower, therefore the prepolymer of the epoxy resin shown in preparation formula I and solidifying agent hydrogenating methyl carbic anhydride can reduce the machine-shaping cycle, and can also reduce small-molecule substance causes flash and mold fouling simultaneously.
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 60-100 DEG C of melting mixing, pulverize after cooling.
As preferably, oxidation inhibitor in step (1): the mass ratio=1:12.5-20 of coupling agent; In step (3), the consumption of solidifying agent is the 8-20% of the total consumption of solidifying agent.Oxidation inhibitor is preferably with colourless triphenyl phosphite, and oxidation inhibitor: the mass ratio=1:12.5-20 of coupling agent, oxidation inhibitor addition is very few can not play a protective role, and addition too much affects the activity of coupling agent.
The invention has the beneficial effects as follows: there is higher thermotolerance and excellent yellowing resistance energy, photosemiconductor LED reflection matrix can be improved under long-time hot operation, keep high-reflectivity and reliability, c material is under 460nm optical wavelength is irradiated, initially there is the reflectivity of more than 90%, and after placing 1000 hours by 150 DEG C of high temperature, keep more than 70% reflectivity.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment 1
A kind of high heat-resistant xanthochromia thermoset epoxy composite formula:
Be mixed by the component of following mass percent:
Molecular formula is the epoxy resin 5% (commercially available) shown in formula I:
Solidifying agent 5% (hydrogenating methyl carbic anhydride),
Curing catalyst 0.2% (2-ethyl-4 Methylimidazole),
Inner pattern releasing agent applicable 0.01% (calcium stearate),
Color stuffing 88%, wherein by mineral filler, (ball-shaped silicon micro powder+aluminium hydroxide presses the mass ratio combination of 5:1 to color stuffing, the size controlling of mineral filler is at 0.01-50 micron) with the composition of white pigment (titanium dioxide+zinc oxide mass ratio of pressing 1:1 combines, and the size controlling of white pigment is at 0.01-8 micron) according to the mass ratio of 1:1;
Coupling agent 1.5% (vinyltrimethoxy silane),
Oxidation inhibitor 0.29% (triphenyl phosphite).
Preparation method comprises the steps:
(1) by mineral filler, white pigment, part oxidation inhibitor and coupling agent at high-speed mixer high speed 2000 turns/min mixing 10min, 500 turns/min mixes 30 minutes and obtains front batch mixing at a slow speed, and the temperature of mixing process controls at 50 DEG C.Wherein oxidation inhibitor: the mass ratio=1:20 of coupling agent.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable.
(3) by epoxy resin, partially cured dose and curing catalyst input kneader, Procuring thing is mediated 30 minutes to obtain 100 DEG C of Procuring.The consumption of this step solidifying agent is 8% of the total consumption of solidifying agent.
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 60 DEG C of melting mixing, pulverize after cooling, compressing tablet.
Embodiment 2
A kind of high heat-resistant xanthochromia thermoset epoxy composite formula:
Be mixed by the component of following mass percent:
Molecular formula is the epoxy resin 20% (commercially available) shown in formula I:
Solidifying agent 25% (hydrogenating methyl carbic anhydride),
Curing catalyst 1.2% (2-ethyl-4 Methylimidazoles+triphenyl phosphorus presses the mass ratio combination of 1:1),
Inner pattern releasing agent applicable 2% (calcium stearate+oxidized polyethlene wax presses the mass ratio combination of 1:1),
Color stuffing 50%, wherein color stuffing is by mineral filler (ball-shaped silicon micro powder, the size controlling of mineral filler is at 0.01-50 micron) with white pigment (titanium dioxide, the size controlling of white pigment is at 0.01-8 micron) according to the composition of the mass ratio of 4:1;
Coupling agent 0.01% (silane coupling agent KH-560),
Oxidation inhibitor 1.79% (triphenyl phosphite).
Preparation method comprises the steps:
(1) by mineral filler, white pigment, part oxidation inhibitor and coupling agent at high-speed mixer high speed 2200 turns/min mixing 5min, 600 turns/min mixes 20 minutes and obtains front batch mixing at a slow speed, and the temperature of mixing process controls at 130 DEG C.Wherein oxidation inhibitor: the mass ratio=1:12.5 of coupling agent.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable.
(3) by epoxy resin, partially cured dose and curing catalyst input kneader, Procuring thing is mediated 10 minutes to obtain 120 DEG C of Procuring.The consumption of this step solidifying agent is 20% of the total consumption of solidifying agent.
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 100 DEG C of melting mixing, pulverize after cooling, compressing tablet.
Embodiment 3
A kind of high heat-resistant xanthochromia thermoset epoxy composite formula:
Be mixed by the component of following mass percent:
Molecular formula is the epoxy resin 10% (commercially available) shown in formula I:
Solidifying agent 10% (hydrogenating methyl carbic anhydride),
Curing catalyst 0.5% (triphenyl phosphorus),
Inner pattern releasing agent applicable 0.5% (oxidized polyethlene wax),
Color stuffing 74.7%, wherein color stuffing is by mineral filler (ball-shaped silicon micro powder, the size controlling of mineral filler is at 0.01-50 micron) with white pigment (aluminum oxide, the size controlling of white pigment is at 0.01-8 micron) according to the composition of the mass ratio of 3:1;
Coupling agent 2% (titanic acid ester),
Oxidation inhibitor 2.3% (triphenyl phosphite+diphenylalkyl phosphites is according to the combination of the mass ratio of 1:1).
Preparation method comprises the steps:
(1) by mineral filler, white pigment, part oxidation inhibitor and coupling agent at high-speed mixer high speed 2000 turns/min mixing 8min, 500 turns/min mixes 25 minutes and obtains front batch mixing at a slow speed, and the temperature of mixing process controls at 80 DEG C.Wherein oxidation inhibitor: the mass ratio=1:15 of coupling agent.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable.
(3) by epoxy resin, partially cured dose and curing catalyst input kneader, Procuring thing is mediated 20 minutes to obtain 110 DEG C of Procuring.The consumption of this step solidifying agent is 15% of the total consumption of solidifying agent.
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 80 DEG C of melting mixing, pulverize after cooling, compressing tablet.
Embodiment 4
A kind of high heat-resistant xanthochromia thermoset epoxy composite formula:
Be mixed by the component of following mass percent:
Molecular formula is the epoxy resin 15% (commercially available) shown in formula I:
Solidifying agent 20% (hydrogenating methyl carbic anhydride),
Curing catalyst 1% (2-ethyl-4 Methylimidazole+DBU presses the mass ratio combination of 1:1),
Inner pattern releasing agent applicable 1.95% (Zinic stearas),
Color stuffing 62%, wherein color stuffing is by mineral filler (ball-shaped silicon micro powder, the size controlling of mineral filler is at 0.01-50 micron) with white pigment (titanium dioxide, the size controlling of white pigment is at 0.01-8 micron) according to the composition of the mass ratio of 2:1;
Coupling agent 0.04% (silane coupling agent KH-560),
Oxidation inhibitor 0.01% (triphenyl phosphite).
Preparation method comprises the steps:
(1) by mineral filler, white pigment, part oxidation inhibitor and coupling agent at high-speed mixer high speed 2000 turns/min mixing 10min, 500 turns/min mixes 25 minutes and obtains front batch mixing at a slow speed, and the temperature of mixing process controls at 70 DEG C.Wherein oxidation inhibitor: the mass ratio=1:20 of coupling agent.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable.
(3) by epoxy resin, partially cured dose and curing catalyst input kneader, Procuring thing is mediated 20 minutes to obtain 110 DEG C of Procuring.The consumption of this step solidifying agent is 10% of the total consumption of solidifying agent.
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 90 DEG C of melting mixing, pulverize after cooling, compressing tablet.
Comparative example 1
A kind of high heat-resistant xanthochromia thermoset epoxy composite formula:
Be mixed by the component of following mass percent:
Bisphenol A epoxide resin 10%:
Solidifying agent 10% (methyl hexahydrophthalic anhydride),
Curing catalyst 0.5% (2-ethyl-4 Methylimidazole),
Inner pattern releasing agent applicable 0.5% (oxidized polyethlene wax),
Color stuffing 74.7%, wherein color stuffing is by mineral filler (ball-shaped silicon micro powder, the size controlling of mineral filler is at 0.01-50 micron) with white pigment (aluminum oxide, the size controlling of white pigment is at 0.01-8 micron) according to the composition of the mass ratio of 3:1;
Coupling agent 2% (titanic acid ester),
Oxidation inhibitor 2.3% (triphenyl phosphite+diphenylalkyl phosphites is according to the combination of the mass ratio of 1:1).
Preparation method comprises the steps:
(1) by mineral filler, white pigment and coupling agent at high-speed mixer high speed 2000 turns/min mixing 8min, 500 turns/min mixes 25 minutes and obtains front batch mixing at a slow speed, and the temperature of mixing process controls at 80 DEG C.
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable.
(3) after Preblend, epoxy resin, solidifying agent and curing catalyst, oxidation inhibitor being mixed, be heated to 80 DEG C of melting mixing, pulverize after cooling, compressing tablet.
Testing method:
Reflectivity test method:
Embodiment and comparative example each resin combination sample are made the square piece of long 60*100*3mm, by under original state and 150 DEG C 1000 hours aging after print, the reflectance test under using HunterLab ColorQuest XE to carry out 460nm wavelength.
CTE (thermal expansivity) and Tg testing method:
CTE and Tg is tested according to the 5.6th article of linear expansivity of SJ/T11197-1999 and second-order transition temperature.
Flexural strength testing method:
Flexural strength is tested according to GB 1042-1979 plastics bend test method.
The each embodiment of table 1 and properties of sample
1000 h heat aging time at * 150 DEG C
As seen from Table 1, example 1-4 employs I formula epoxy resin and novel process, can reach claim under 460nm optical wavelength is irradiated, initially there is the reflectivity of more than 90%, and after placing 500 hours by 150 DEG C of high temperature, keep more than 70% reflectivity.
From comparative example 1, use general purpose epoxy resin and solidifying agent, Tg drops to less than 130 DEG C, aging reflectivity also fails to reach 70%, this causes because the thermostability of bisphenol A type epoxy resin is not high, in addition, technique is not optimized to cause also be the reason that reflectivity and flexural strength are lower.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (10)
1. a high heat-resistant xanthochromia thermoset epoxy composition, is characterized in that, be mixed by the component of following mass percent:
Molecular formula is the epoxy resin 5-20% shown in formula I, solidifying agent 5-25%, curing catalyst 0.2%-1.2%, inner pattern releasing agent applicable 0.01%-2%, color stuffing 50-88%, coupling agent 0.01%-2%, oxidation inhibitor 0.01%-2.3%, wherein color stuffing is by mineral filler and white pigment the forming of mass ratio according to 1-4:1;
2. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, is characterized in that: described solidifying agent is hydrogenating methyl carbic anhydride.
3. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, it is characterized in that: described curing catalyst is selected from 1, one or more in 8-diaza-two ring (5,4,0) undecylene-7,2-ethyl-4 Methylimidazole, triphenyl phosphorus.
4. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, is characterized in that: described inner pattern releasing agent applicable is selected from one or more in stearic acid, calcium stearate, Zinic stearas, aluminum stearate, oxidized polyethlene wax, palm wax.
5. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, it is characterized in that: described mineral filler is selected from crystalline silicon powder, fusion silicon powder, ball-shaped silicon micro powder, calcium carbonate, aluminium hydroxide, magnesium hydroxide, wollastonite, barium carbonate, hydrotalcite the combination choosing one or more, and the size controlling of mineral filler is at 0.01-50 micron.
6. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, it is characterized in that: described white pigment is selected from one or more in titanium dioxide, zinc oxide, aluminum oxide, magnesium oxide, zinc sulphide, the size controlling of white pigment is at 0.01-8 micron.
7. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, is characterized in that: described coupling agent is selected from the one in silane resin acceptor kh-550, silane coupling agent KH-560, vinyltrimethoxy silane, titanic acid ester, Al-Ti-diffused steel.
8. one according to claim 1 high heat-resistant xanthochromia thermoset epoxy composition, is characterized in that: described oxidation inhibitor is selected from one or more in 2,6 ditertiary butyl p cresol, triphenyl phosphite, diphenylalkyl phosphites.
9. the preparation method of high heat-resistant xanthochromia thermoset epoxy composition as claimed in claim 1, is characterized in that, comprise the steps:
(1) mineral filler, white pigment, part oxidation inhibitor and coupling agent are turned/min mixing 5-10min at high-speed mixer high speed 2000-2200, at a slow speed 500-600 turn/min mixing obtains front batch mixing in 20-30 minute, the temperature of mixing process controls at 50 DEG C-130 DEG C;
(2) front batch mixing is mixed to obtain Preblend with inner pattern releasing agent applicable;
(3) undertaken mediating 10-30 minute to obtain Procuring thing 100 DEG C of-120 DEG C of Procuring by after epoxy resin, partially cured dose and curing catalyst mixing;
(4) after Preblend, Procuring thing, remaining oxidation inhibitor, remaining solidifying agent and curing catalyst being mixed, be heated to 60-100 DEG C of melting mixing, pulverize after cooling.
10. preparation method according to claim 9, is characterized in that: oxidation inhibitor in step (1): the mass ratio=1:12.5-20 of coupling agent; In step (3), the consumption of solidifying agent is the 8-20% of the total consumption of solidifying agent.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108017879A (en) * | 2016-11-04 | 2018-05-11 | 无锡创达新材料股份有限公司 | A kind of preparation of high-power LED encapsulation white epoxy moulding compound |
| CN111205796A (en) * | 2019-12-27 | 2020-05-29 | 科化新材料泰州有限公司 | Light-colored anti-yellowing epoxy resin composition for semiconductor packaging |
| CN111393069A (en) * | 2020-03-25 | 2020-07-10 | 深圳绿景环保再生资源有限公司 | Preparation method of epoxy mortar of modified powder and graded sand and epoxy mortar |
| CN112029458A (en) * | 2020-08-17 | 2020-12-04 | 南京施瓦乐新材料科技有限公司 | Adhesive for temperature-controlled color-changing glass and preparation method thereof |
| CN112391034A (en) * | 2019-08-13 | 2021-02-23 | 北京科化新材料科技有限公司 | Epoxy resin composite material and preparation method and application thereof |
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| CN102649868A (en) * | 2011-02-24 | 2012-08-29 | 日东电工株式会社 | Resin composition for optical semiconductor element housing package, and optical semiconductor light-emitting device obtained using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108017879A (en) * | 2016-11-04 | 2018-05-11 | 无锡创达新材料股份有限公司 | A kind of preparation of high-power LED encapsulation white epoxy moulding compound |
| CN112391034A (en) * | 2019-08-13 | 2021-02-23 | 北京科化新材料科技有限公司 | Epoxy resin composite material and preparation method and application thereof |
| CN112391034B (en) * | 2019-08-13 | 2022-12-09 | 北京科化新材料科技有限公司 | Epoxy resin composite material and preparation method and application thereof |
| CN111205796A (en) * | 2019-12-27 | 2020-05-29 | 科化新材料泰州有限公司 | Light-colored anti-yellowing epoxy resin composition for semiconductor packaging |
| CN111205796B (en) * | 2019-12-27 | 2022-08-05 | 江苏科化新材料科技有限公司 | Light-colored anti-yellowing epoxy resin composition for semiconductor packaging |
| CN111393069A (en) * | 2020-03-25 | 2020-07-10 | 深圳绿景环保再生资源有限公司 | Preparation method of epoxy mortar of modified powder and graded sand and epoxy mortar |
| CN111393069B (en) * | 2020-03-25 | 2021-09-21 | 深圳绿景环保再生资源有限公司 | Preparation method of epoxy mortar of modified powder and graded sand and epoxy mortar |
| CN112029458A (en) * | 2020-08-17 | 2020-12-04 | 南京施瓦乐新材料科技有限公司 | Adhesive for temperature-controlled color-changing glass and preparation method thereof |
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