CN102965069B - A kind of resistance to sulfuration LED silica gel - Google Patents
A kind of resistance to sulfuration LED silica gel Download PDFInfo
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- CN102965069B CN102965069B CN201210465914.6A CN201210465914A CN102965069B CN 102965069 B CN102965069 B CN 102965069B CN 201210465914 A CN201210465914 A CN 201210465914A CN 102965069 B CN102965069 B CN 102965069B
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- vinyl
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- silicone oil
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Abstract
The present invention relates to the LED silica gel of a kind of LED silica gel, particularly resistance to sulfuration, belong to field of adhesive technology.Described resistance to sulfuration LED silica gel comprises component A and B component, and the weight ratio of described component A and B component is 1:1; Wherein, described component A comprises the raw material of following weight part: methyl phenyl vinyl silicone oil 50 ~ 60 parts, methyl vinyl MQ resin 30 ~ 60 parts, platinum group catalyst 0.1 ~ 0.3 part, caking agent 3 ~ 5 parts; Described B component comprises the raw material of following weight part: methyl phenyl vinyl silicone oil 40 ~ 50 parts, vinyl MQ resin 30 ~ 50 parts, linking agent 5 ~ 15 parts, 0.1 ~ 0.3 part, inhibitor.LED silica gel of the present invention has sticking power such as silver, PPA, glass excellent, transmittance more than 98%, and because introduce containing phenyl functional group, branched ethylene base and improve vinyl MQ resin consumption, improves cross-linking density, solidification hardness, thus improve the sulfidation-resistance energy of encapsulation glue-line.
Description
Technical field
The present invention relates to the LED silica gel of a kind of LED silica gel particularly resistance to sulfuration, belong to field of adhesive technology.
Background technology
The current packaged material used of LED has epoxy resin, polymethylmethacrylate, glass, the contour transparent material of organosilicon, its epoxy resin and organosilicon material are as main packaged material, epoxy resin internal stress is excessive, xanthochromia, high and low temperature resistance is poor, loss of properties on aging, and current organosilicon material, internal stress is little, high and low temperature resistance is good, non yellowing, transmittance is also higher than epoxy resin, therefore rapid substituted epoxy resin, be widely used in LED field, but organosilicon material is low-refraction organosilicon material particularly, because use the end-vinyl polydimethylsiloxane of long-chain, molecular chain length, contents of ethylene is low, cause cross-linking density low, cause glue-line ventilation property good, under sulfurous gas effect, meeting partial penetration silica gel packaging material, react at silica gel interface and silver layer, generate silver sulfide, silver layer is caused to turn black, light decay improves rapidly.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides the LED silica gel of a kind of LED silica gel particularly resistance to sulfuration.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: described resistance to sulfuration LED silica gel comprises component A and B component, and the weight ratio of described component A and B component is 1:1; Wherein,
Described component A comprises the raw material of following weight part: methyl phenyl vinyl silicone oil 50 ~ 60 parts, methyl vinyl MQ resin 30 ~ 60 parts, platinum group catalyst 0.1 ~ 0.3 part, caking agent 3 ~ 5 parts;
Described B component comprises the raw material of following weight part: methyl phenyl vinyl silicone oil 40 ~ 50 parts, methyl vinyl MQ resin 30 ~ 50 parts, linking agent 5 ~ 15 parts, 0.1 ~ 0.3 part, inhibitor.
The invention has the beneficial effects as follows: LED silica gel of the present invention is made up of A, B component, component A provides phenyl and polyfunctionality vinyl and caking agent in the reaction, B component provides phenyl, polyfunctionality vinyl and linking agent, LED silica gel of the present invention has sticking power such as silver, PPA, glass excellent, transmittance is more than 98%, and because introduce containing phenyl functional group, branched ethylene base and improve vinyl MQ resin consumption, improve cross-linking density, solidification hardness, thus improve the sulfidation-resistance energy of encapsulation glue-line.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the viscosity of described methyl phenyl vinyl silicone oil is 1000 ~ 20000 centipoises, and structural formula is:
Wherein, Me is methyl, and Vi is vinyl, n
1=20 ~ 50, n
2=25 ~ 55, n
3=10 ~ 30
The beneficial effect of above-mentioned further scheme is adopted to be: as matrix resin, contrast end-vinyl polydisiloxane, phenyl containing part, do not affect the consistency with other low-refraction raw materials, the ventilation property of silica gel material is reduced after introducing phenyl solidification, and end group, side base all contain vinyl, improve crosslinked density, different viscosity can also be adjusted.
Further, the structural formula of described methyl vinyl MQ resin is: (Me
3siO
0.5)
a(ViMe
2siO
0.5)
b(SiO
2), wherein, Me is methyl, and Vi is vinyl, a=06 ~ 0.8, b=0.1 ~ 0.2.
The beneficial effect of above-mentioned further scheme is adopted to be: adding of methyl vinyl MQ resin, to improve cross-linking density and the intensity of whole silica gel, reduce the ventilation property of silica gel.
Further, it is 3-5% that the molar mass of described methyl vinyl MQ resin medium vinyl accounts for content.
Further, described caking agent contains epoxy-functional, and its structural formula is:
Structural formula one;
Or,
Structural formula two
Further, described linking agent is polymethyl hydrogen siloxane.
Further, described platinum group catalyst is any one in the alcoholic solution of Platinic chloride, platinum-vinyl siloxane title complex, platinum-olefin(e)complex.
Further, the preferred platinum-vinyl siloxane title complex of described platinum group catalyst, the mass content of platinum is 3000 ~ 7000ppm.
Further, described inhibitor is any one in ethynylcyclohexanol, t etram-ethyltetravinylcyclotetrasiloxane or benzotriazole.
Further, ethynylcyclohexanol elected as by described inhibitor.
The preparation side of resistance to sulfuration LED silica gel of the present invention comprises the preparation process of component A and the preparation process of B component; Wherein, the preparation process of described component A is as follows: be the methyl phenyl vinyl silicone oil of 50 ~ 60 parts, methyl vinyl MQ resin 30 ~ 60 parts, catalyzer 0.1 ~ 0.3 part, caking agent 3 ~ 5 parts by parts by weight, add successively in stirrer, mixing and stirring, obtain described component A;
The preparation process of described B component is as follows: methyl phenyl vinyl silicone oil 40 ~ 50 parts, methyl vinyl MQ resin 30 ~ 50 parts, and linking agent 5 ~ 15 parts, 0.1 ~ 0.3 part, inhibitor, add successively in stirrer, mixing and stirring, obtain described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 ~ 40 minutes, point glue or encapsulating are on to be packaged, first heat 0.5 ~ 1.5 hour at 80 ~ 100 DEG C of temperature, then 100 ~ 200 DEG C of heating 1.5 ~ 4 hours, solidify.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
The preparation of component A: take methyl phenyl vinyl silicone oil 50g, methyl vinyl MQ resin 44.9g, caking agent 5g(and structure above one), catalyst platinum-vinyl siloxane complex 0.1g, the wherein mass content 7000ppm of platinum, add successively in stirrer, mixing and stirring, obtain described component A;
The preparation of B component: take methyl phenyl vinyl silicone oil 50g, methyl vinyl MQ resin 34.8g linking agent polymethyl hydrogen siloxane 15g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, be that the proportioning of 1: 1 mixes by weight by described component A, B component, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first 90 DEG C of heating 1 hour, then heat 3 hours at 150 DEG C.
Embodiment 2
The preparation of component A: take methyl phenyl vinyl silicone oil 60g, methyl vinyl MQ resin 36.7g, caking agent 3g(and structure above two), catalyst platinum-vinyl siloxane complex 0.3g, wherein the mass content of platinum is 7000ppm, add successively in stirrer, mixing and stirring, obtain described component A;
The preparation of B component: take methyl phenyl vinyl silicone oil 40g, methyl vinyl MQ resin 50g, linking agent polymethyl hydrogen siloxane 9.8g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
Embodiment 3
The preparation of component A: take methyl phenyl vinyl silicone oil 53.9g, methyl vinyl MQ resin 42g, caking agent 4g(structural formula one), catalyst platinum-vinyl siloxane complex 0.1g, the wherein mass content 5000ppm of platinum, add successively in stirrer, mixing and stirring, obtain described component A;
The preparation of B component: take methyl phenyl vinyl silicone oil 45g, methyl vinyl MQ resin 41g, linking agent polymethyl hydrogen siloxane 13.8g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
Comparative example 1
The preparation of component A: take end-vinyl polydisiloxane 50g, methyl vinyl MQ resin 44.9g, caking agent 5g(structural formula one), catalyst platinum-vinyl siloxane complex 0.1g, the mass content 7000ppm of platinum, add in stirrer successively, mixing and stirring, obtains described component A;
The preparation of B component: take end-vinyl polydisiloxane 50g, methyl vinyl MQ resin 34.8g, linking agent polymethyl hydrogen siloxane 15g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
Comparative example 2
The preparation of component A: take end-vinyl polydisiloxane 98.8g, caking agent 2g(structural formula two), catalyst platinum-vinyl siloxane complex 0.2g, the mass content 5000ppm of platinum, add in stirrer, mixing and stirring successively, obtains described component A;
The preparation of B component: take vinyl polydisiloxane 89.8g, linking agent polymethyl hydrogen siloxane 10g, inhibitor ethynylcyclohexanol 0.2g, mixing and stirring, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
The A of embodiment 1,2,3 and comparative example 1,2, B component are weighed by weight the ratio of 1:1, then mix, deaeration 30 minutes, one is by mixing object point glue to treated 3528LED support; Two is require to make sheet material, by mixture levelling in mould according to GB/T528-2009 respectively.Condition of cure: first 90 DEG C of heating 1 hour, then 150 DEG C of heating 3 hours.Test one: the sample after solidification is carried out transmittance test; Test two: the sample of the LED chip (3528) after cure package silica gel is carried out the experiment of sulfuration light decay, sample is positioned in 100ml closed glass jar, place 0.2g powder sulphur in bottle, under 60 DEG C of air tight conditions, place 24h, and to decline tester test light decay by LED light; Test three: require to make dumbbell shaped silica gel exemplar according to GB/T528-2009, use puller system test tensile strength; Test four: by the hardness of silica gel after Shore A durometer test solidification, testing method is according to GB/T2411-2008.
Table 1 performance index table
Can be found out by table 1, embodiment 1 compares can find out with comparative example 1, increase, thus hardness and intensity obviously increases containing phenyl branched ethylene base silicone oil than cross-linking density after the solidification of end-vinyl polydisiloxane; Embodiment 1,2,3 adds containing phenyl branched ethylene base silicone oil and methyl vinyl MQ resin, compares with comparative example 1 and 2, and cross-linking density increases, and hardness, intensity are high, and after sulfuration test, light decay obviously reduces, and meets and has the client of cures requirements to use
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a resistance to sulfuration LED silica gel, is characterized in that, prepares by the following method:
The preparation of component A: take methyl phenyl vinyl silicone oil 50g, methyl vinyl MQ resin 44.9g, caking agent 5g shown in structural formula one, catalyst platinum-vinyl siloxane complex 0.1g, the wherein mass content 7000ppm of platinum, adds in stirrer, mixing and stirring successively, obtain described component A
The preparation of B component: take methyl phenyl vinyl silicone oil 50g, methyl vinyl MQ resin 34.8g linking agent polymethyl hydrogen siloxane 15g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
2. a resistance to sulfuration LED silica gel, is characterized in that, prepares by the following method:
The preparation of component A: take methyl phenyl vinyl silicone oil 60g, methyl vinyl MQ resin 36.7g, caking agent 3g shown in structural formula two, catalyst platinum-vinyl siloxane complex 0.3g, wherein the mass content of platinum is 7000ppm, adds successively in stirrer, mixing and stirring, obtain described component A
The preparation of B component: take methyl phenyl vinyl silicone oil 40g, methyl vinyl MQ resin 50g, linking agent polymethyl hydrogen siloxane 9.8g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
3. a resistance to sulfuration LED silica gel, is characterized in that, prepares by the following method:
The preparation of component A: take methyl phenyl vinyl silicone oil 53.9g, methyl vinyl MQ resin 42g, caking agent 4g shown in structural formula one, catalyst platinum-vinyl siloxane complex 0.1g, the wherein mass content 5000ppm of platinum, adds in stirrer, mixing and stirring successively, obtain described component A
The preparation of B component: take methyl phenyl vinyl silicone oil 45g, methyl vinyl MQ resin 41g, linking agent polymethyl hydrogen siloxane 13.8g, inhibitor ethynylcyclohexanol 0.2g, adds in stirrer, mixing and stirring successively, obtains described B component;
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 20 minutes, some glue or encapsulating, on to be packaged, first heat 1 hour at 90 DEG C, then 150 DEG C of heating 3 hours.
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