CN107760197A - A kind of high folding LED packaging silicon rubber of high temperature resistant without cracking - Google Patents
A kind of high folding LED packaging silicon rubber of high temperature resistant without cracking Download PDFInfo
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- CN107760197A CN107760197A CN201710790866.0A CN201710790866A CN107760197A CN 107760197 A CN107760197 A CN 107760197A CN 201710790866 A CN201710790866 A CN 201710790866A CN 107760197 A CN107760197 A CN 107760197A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to a kind of high folding LED packaging silicon rubber of high temperature resistant without cracking, including component A and component B, the component A and component B weight ratio are 3：1；Wherein：Component A includes the raw material of following mass parts：Methyl ethylene MDQ silicones 50 60, methyl phenyl vinyl silicone oil 10 15, the hydrogeneous resin 5 10 of aminomethyl phenyl, hydrogeneous small molecule 20 40, chain extender 5 10, inhibitor 0.1~0.5, B component include the raw material of following mass parts：Methyl ethylene MDQ silicones 85 95, bonding agent 10 20, catalyst 0.1~0.5.High folding LED packaging silicon rubbers of the invention, in addition to new methyl ethylene MDQ silicones, add the chain extender containing methoxyl group and a kind of hydrogeneous small molecule, substantially increase the resistance to elevated temperatures of packaging silicon rubber again.
Description
Technical field
The invention belongs to encapsulating material field, is related to a kind of high temperature resistant, without cracking high index of refraction packaging silicon rubber and its preparation
Method.
Technical background
LED life is long, light efficiency is high, radiationless and low-power consumption, is widely used in various display screens, auto lamp and each
Backlight and illumination use of electronic product etc. are planted, the selection of its encapsulating material is most important to LED performance impact.But with
LED using more and more extensive, requirement to LED encapsulation material also more and more higher, especially high-power LED illuminating light source
Development, high caloric value to the bulk strength of encapsulating material, heat resistance, anti-light decline and cementability requirement also accordingly improves.
The content of the invention
It is an object of the invention to provide a kind of high temperature resistant, without cracking high index of refraction packaging silicon rubber and preparation method thereof.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：Described high folding LED packaging silicon rubbers include component A and
Component B, the component A and component B weight ratio are 3:1；Wherein：
The component A includes the raw material of following mass parts：
The B component includes the raw material of following mass parts：
Methyl ethylene MDQ silicones 85-95
Bonding agent 10-20
Catalyst 0.1~0.5
The beneficial effects of the invention are as follows：High index of refraction LED packaging silicon rubbers of the present invention are made up of A, B component, and component A is anti-
Resin, vinyl, crosslinking agent and the inhibitor of high strength heat resistant are provided in answering, B component provides chain extender, bonding agent and catalysis
Agent.High folding LED packaging silicon rubbers of the invention, in addition to new methyl ethylene MDQ silicones, add the expansion containing methoxyl group again
Chain agent and a kind of hydrogeneous small molecule, substantially increase the resistance to elevated temperatures of packaging silicon rubber.
Described methyl ethylene MDQ silicones is (ViMe selected from formula2SiO1/2)3(PhSiO3/2)7Silicones, its
Middle Me is methyl, and Ph is phenyl, and Vi is vinyl.Its structural formula is (1)：
The beneficial effect of MDQ silicones：The addition of wherein D chain links greatly strengthen the tightness degree of network structure resin,
Improve the high temperature resistant cracking performance of silica gel.
The hydrogeneous resin of described aminomethyl phenyl is (HMe selected from formula2SiO1/2)3(PhSiO3/2)7Silicones, wherein Me
For methyl, Ph is phenyl, and H is vinyl, and resin structure is similar with structure (1) structure.The selection hydrogeneous resin of aminomethyl phenyl has
Beneficial effect is：The crosslinking degree of resin is improved, increases the heat endurance of resin.
The methyl phenyl vinyl silicone oil is that end group is vinyl, and main chain is the vinyl silicone oil of silicon aminomethyl phenyl, its
Structural formula is (2)：
Wherein, n=1-10
Select the beneficial effect of methyl phenyl vinyl silicone oil：It is too high effectively to alleviate excessively internal stress caused by crosslinking,
Increase the overall performance of silica gel.
Described hydrogeneous small molecule is that end group is silicon hydrogen, and main chain is the hydrogeneous small molecule of silicon phenyl.The structure is (3)：
Wherein, n=1-5
Selecting the beneficial effect of hydrogeneous small molecule is：Increase crystallinity, balance silica gel whole synthesis performance.
The bonding agent is the coupling agent γ containing epoxy-functional-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane
(KH560), its structural formula is (4)：
It is as follows using the structural formula (5) of chain extender：
The catalyst is platinum group catalyst, is matched somebody with somebody selected from chloroplatinic acid in alcohol, platinum-methyl phenyl silicone, platinum-alkene
Any one or more than one in compound, wherein platinum content is 5ppm.
Described inhibitor is in ethynylcyclohexanol, 1,1,3- triphenyl -2- propine -1- alcohol, uncommon third fat of maleic acid two
Any one or more than one.
The preparation process of the component A：It is 50-60 methyl ethylene MDQ silicones, 5-15 mass parts first by mass parts
Base phenyl-vinyl silicon oil, the hydrogeneous resin of 5-10 mass parts aminomethyl phenyls, the hydrogeneous small molecule of 20-40 mass parts, 5-10 mass
Part chain extender, 0.1-0.5 mass parts inhibitor, are stirred using mechanical mixture, vacuumizing and defoaming, are filled with nitrogen, closed storage
Deposit, produce component A；
The preparation process of the B component：It is 85-95 methyl ethylene MDQ silicones, 10-20 mass parts by mass parts
The catalyst of bonding agent, 0.1-0.5 mass parts, is stirred using mechanical mixture, vacuumizing and defoaming, is filled with nitrogen, closed storage
Deposit, produce B component.
By A, B component according to mass ratio 3 during use:1 is well mixed, adds appropriate anti-settling powder and fluorescent material, vacuum
5~10min of deaeration, dispensing or encapsulating are on packaging part, condition of cure：80 DEG C, 1h+150 DEG C, 4h.
Embodiment
With reference to specific implementation case, the invention will be further described.
Embodiment 1
The preparation of component A：Accurately weigh 50g methyl ethylene MDQ silicones, 6.5g methyl phenyl vinyl silicone oil (its
In, n=1), the hydrogeneous resin of 6.5g crosslinking agent aminomethyl phenyls, the hydrogeneous small molecules of 30g (wherein, n=1), 6.5g chain extenders, 0.5g
Inhibitor ethynylcyclohexanol, is stirred using mechanical mixture, produces component A；
The preparation of B component：It is accurate weigh 87.5g methyl ethylene MDQ silicones, 12g bonding agents, 0.5g catalyst platinums-
Methyl phenyl silicone (platinum content 5ppm), is stirred using mechanical mixture, produces B component；
In use, by A, B component according to mass parts 3:1 is well mixed, vacuum defoamation 5min, and dispensing or encapsulating are in waiting to seal
In piece installing, 1h+150 DEG C of solidification 4h of 80 DEG C of solidifications.
Embodiment 2
The preparation of component A：Accurately weigh 55g methyl ethylene MDQ silicones, 5.5g methyl phenyl vinyl silicone oil (its
In, n=2), the hydrogeneous resin of 5.5g crosslinking agent aminomethyl phenyls, the hydrogeneous small molecules of 27g (wherein, n=2), 6.5g chain extenders, 0.5g
Inhibitor 1,1,3- triphenyl -2- propine -1- alcohol, is stirred using mechanical mixture, produces component A；
The preparation of B component：It is accurate weigh 87.5g methyl ethylene MDQ silicones, 12g bonding agents, 0.5g catalyst platinums-
Methyl phenyl silicone (platinum content 5ppm), is stirred using mechanical mixture, produces B component；
In use, by A, B component according to mass parts 1:1 is well mixed, vacuum defoamation 5min, and dispensing or encapsulating are in waiting to seal
In piece installing, 1h+150 DEG C of solidification 4h of 80 DEG C of solidifications.
Embodiment 3
The preparation of component A：Accurately weigh 60g methyl ethylene MDQ silicones, 6.5g methyl phenyl vinyl silicone oil (its
In, n=3), the hydrogeneous resin of 6.5g crosslinking agent aminomethyl phenyls, the hydrogeneous small molecules of 21g (wherein, n=3), 5.5g chain extenders, 0.5g
Inhibitor maleic acid two wishes the third fat, is stirred using mechanical mixture, produces component A；
The preparation of B component：It is accurate weigh 87.5g methyl ethylene MDQ silicones, 12g bonding agents, 0.5g catalyst platinums-
Olefin complex (platinum content 5ppm), is stirred using mechanical mixture, produces B component；
In use, by A, B component according to mass parts 1:1 is well mixed, vacuum defoamation 5min, and dispensing or encapsulating are in waiting to seal
In piece installing, 1h+150 DEG C of solidification 4h of 80 DEG C of solidifications.
Embodiment 4
The preparation of component A：Accurately weigh 57.5g methyl ethylene MDQ silicones, 6.5g methyl phenyl vinyl silicone oils
(wherein, n=4), the hydrogeneous resin of 6.5g crosslinking agent aminomethyl phenyls, the hydrogeneous small molecules of 22g (wherein, n=5), 7g chain extenders,
0.5g inhibitor maleic acid two wishes the third fat, is stirred using mechanical mixture, produces component A；
The preparation of B component：It is accurate weigh 87.5g methyl ethylene MDQ silicones, 12g bonding agents, 0.5g catalyst platinums-
Olefin complex (platinum content 5ppm), is stirred using mechanical mixture, produces B component；
In use, by A, B component according to mass parts 3:1 is well mixed, vacuum defoamation 5min, and dispensing or encapsulating are in waiting to seal
In piece installing, 1h+150 DEG C of solidification 4h of 80 DEG C of solidifications.
3W lamp beads are lighted under obtained LED packaging silicon rubbers 350mA in contrast above-described embodiment 1-4, in high temperature of 120 DEG C ring
1000h under border (environment temperature adds the radiating of lamp bead in itself, and section temperature can reach 180 DEG C) and under double 85 environment, LED lamp beads
Light decay degree, test result such as table 1：
Table 1：120 DEG C of embodiment, double 85 1000h light decays
From the test data in table 1 can be seen that the present invention prepare high index of refraction LED packaging silicon rubbers high temperature, double 85,
1000h light decays are respectively less than 10%, have excellent resistance to elevated temperatures, are encapsulated suitable for LED.
Contrast yellow and cracking situation of the obtained LED packaging silicon rubbers under 250 DEG C of 200h, contrast in examples detailed above 1-4
As a result such as table 2：
Table 2：200h yellowing index at 180 DEG C, 250 DEG C of embodiment
Note：Yellowing index b values represent silica gel yellowing, and b values are bigger, and yellow color is deeper
The high index of refraction LED packaging silicon rubber high temperature resistant yellows of the invention prepared are can be seen that from the test data in table 2
Excellent performance, and without cracking phenomena after 250 DEG C of 200h of high temperature.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (6)
1. high folding LED packaging silicon rubber of a kind of high temperature resistant without cracking, it is characterised in that including component A and component B, the component A
Weight ratio with component B is 3：1；Wherein：
The component A includes the raw material of following mass parts：
The B component includes the raw material of following mass parts：
Methyl ethylene MDQ silicones 85-95
Bonding agent 10-20
Catalyst 0.1~0.5
The methyl ethylene MDQ silicones formula is (ViMe2SiO1/2)3(PhSiO3/2)7Silicones, wherein Me is methyl,
Ph is phenyl, and Vi is vinyl；
The hydrogeneous small molecule is that end group is silicon hydrogen, and main chain is the hydrogeneous small molecule of silicon phenyl, and its structure is (3)：
Wherein, n=1-5；
The chain extender knot, its structural formula are (5)：
2. packaging silicon rubber according to claim 1, it is characterised in that the methyl phenyl vinyl silicone oil, its structural formula
For (2)：
Wherein, n=1-10；
The hydrogeneous resin of aminomethyl phenyl, formula are (HMe2SiO1/2)3(PhSiO3/2)7Silicones, wherein Me is methyl, Ph
For phenyl, H is vinyl.
3. packaging silicon rubber according to claim 1, it is characterised in that the bonding agent is γ-(2,3- the third oxygen of epoxy) third
Base trimethoxy silane.
4. packaging silicon rubber according to claim 1, it is characterised in that the catalyst is chloroplatinic acid in alcohol, platinum-methyl
One kind in phenyl polysiloxane, platinum-olefin complex, wherein platinum content are 5ppm.
5. packaging silicon rubber according to claim 1, it is characterised in that the inhibitor is ethynylcyclohexanol, 1,1,3-
Triphenyl -2- propine -1- alcohol, maleic acid two wish one kind in the third fat.
6. packaging silicon rubber according to claim 1, it is characterised in that preparation process includes：By the first that mass parts are 50-60
Base vinyl MDQ silicones, 5-15 mass parts methyl phenyl vinyl silicone oil, the hydrogeneous resin of 5-10 mass parts aminomethyl phenyls, 20-
The hydrogeneous small molecule of 40 mass parts, 5-10 parts chain extender, 0.1-0.5 part inhibitor, are stirred using mechanical mixture, vacuumized
Deaeration, nitrogen is filled with, sealed storage, produces component A；
The preparation process of the B component：It is 85-95 methyl ethylene MDQ silicones by mass parts, the bonding of 10-20 mass parts
Agent, the catalyst of 0.1-0.5 mass parts, are stirred using mechanical mixture, vacuumizing and defoaming, are filled with nitrogen, sealed storage, i.e.,
Obtain B component.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710790866.0A CN107760197A (en) | 2017-09-05 | 2017-09-05 | A kind of high folding LED packaging silicon rubber of high temperature resistant without cracking |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710790866.0A CN107760197A (en) | 2017-09-05 | 2017-09-05 | A kind of high folding LED packaging silicon rubber of high temperature resistant without cracking |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251723A (en) * | 2018-08-24 | 2019-01-22 | 烟台德邦先进硅材料有限公司 | A kind of Molding high folding LED packaging silicon rubber |
| CN113881395A (en) * | 2021-11-15 | 2022-01-04 | 湖南亿福照明科技有限公司 | Pouring sealant for LED packaging |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449551A (en) * | 2014-11-18 | 2015-03-25 | 烟台德邦先进硅材料有限公司 | LED packaging silica gel with high refractive index and yellowing resistance |
| CN106336849A (en) * | 2016-09-05 | 2017-01-18 | 烟台德邦先进硅材料有限公司 | High refractive LED packaging silica gel with high temperature resistance and low luminous decay |
-
2017
- 2017-09-05 CN CN201710790866.0A patent/CN107760197A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449551A (en) * | 2014-11-18 | 2015-03-25 | 烟台德邦先进硅材料有限公司 | LED packaging silica gel with high refractive index and yellowing resistance |
| CN106336849A (en) * | 2016-09-05 | 2017-01-18 | 烟台德邦先进硅材料有限公司 | High refractive LED packaging silica gel with high temperature resistance and low luminous decay |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251723A (en) * | 2018-08-24 | 2019-01-22 | 烟台德邦先进硅材料有限公司 | A kind of Molding high folding LED packaging silicon rubber |
| CN113881395A (en) * | 2021-11-15 | 2022-01-04 | 湖南亿福照明科技有限公司 | Pouring sealant for LED packaging |
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