CN104893310A - Polysilsesquioxane-contained liquid silicone rubber for LED packaging and preparation method of polysilsesquioxane-contained liquid silicone rubber - Google Patents
Polysilsesquioxane-contained liquid silicone rubber for LED packaging and preparation method of polysilsesquioxane-contained liquid silicone rubber Download PDFInfo
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Abstract
The invention relates to liquid silicone rubber for LED packaging, in particular to a polysilsesquioxane-contained liquid silicone rubber for LED packaging and a preparation method of the polysilsesquioxane-contained liquid silicone rubber. The silicone rubber comprises, by weight, 20-130 parts of polysiloxane with a functional-group vinyl polysilsesquioxane structure, 1-50 parts of polysiloxane with a functional-group hydrogen polysilsesquioxane structure, 30-150 parts of dendritic organopolysiloxane with unsaturated bonds, 0.001-0.5 part of platinum complex catalyst, 0.01-0.05 part of inhibitor and 0.5-3 parts of tackifier. Lateral groups of the silicone rubber contain functional-group polysilsesquioxane, and the cured silicone rubber can form concentrated crosslinking points, so that product tensile strength, tearing strength and elongation at break are improved greatly, high product thermostability and cohesiveness are achieved, and light transmittance is larger than or equal to 99%; the preparation method is simple in technology and easy to implement.
Description
Technical field
The present invention relates to a kind of LED liquid silastic, be specifically related to a kind of LED liquid silastic containing polysilsesquioxane and preparation method thereof.
Background technology
Photodiode (Light Emitting Diode, be called for short LED), have efficiency high, photochromic pure, energy consumption is little, the life-span is long, respond the advantages such as fast, pollution-free, all solid state, is a kind of novel illumination light source, be called as green " solid-state illumination ".LED organosilicon material is normally linking agent by vinyl polysiloxane, hydrogen containing siloxane, under platinum catalyst, the transparent three-dimensional reticulate body of certain mechanical strength is sulfided into by addition reaction of silicon with hydrogen, this organosilicon encapsulating material can improve the optical output power of illuminating device, increase the service life, reduce electrisity consumption, have that transparency is high, UV resistant, the advantage such as ageing-resistant, color inhibition, high-low temperature resistant.
Polysiloxane containing ladder-like polysiloxane structure is the organosilicon polymer containing regular duplex structure block, this special composition and molecular structure make it compared with general polysiloxane, there is better resistant of high or low temperature, lower surface energy, and good electric insulation, hydrophobic, difficult combustion, nontoxic corrosion-free and physiological inertia.This polysiloxane can be used for manufacturing the embedding of LED organic silicon packaging glue, photoelectricity, electronics and microelectronic industry, sealing, bonding and coating, high printing opacity, high rigidity eyeglass etc.
Hydroxy-end capped ladder-like polysiloxane segment is incorporated in silicone resin by Chinese patent literature CN104327272A (application number 201410467689.9) and CN104327289A (application number 201410467654.5), improve physical strength and the snappiness of silicone resin, good with base material cohesiveness, ability thermal shock, ultraviolet light resistant, and there is high transmission rate, can be used for LED be representative electronic devices and components encapsulation.But, not containing functional group in the side base of this ladder polysiloxane block, as vinyl, hydrogen base etc., Concentrative crosslinking can not be formed further, mechanical property can be caused weaker.
The vinyl silicone oil that Chinese patent literature CN102344684A (application number 201110233591.3) introduces vulcabond modification, end is hydroxyl has prepared LED module packaging organo-silicone rubber, improve the tear resistance of silicon rubber, but not obvious to the raising of its tensile strength and tensile yield.
Chinese patent literature CN103146202A (application number 201310087259.X) introduces end-vinyl ultra-branching polysiloxane, be applied in LED package liquid silastic, mechanical property is improved, but still the LED of requirements at the higher level can not be met.
POSS is applied in LED encapsulation material by Chinese patent literature CN102181159A (application number 201110061714.X), but POSS complicated process of preparation, cost is higher, is unsuitable for industrial application.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of LED liquid silastic containing polysilsesquioxane, there is good tensile strength, tear strength, elongation and light transmission; The present invention provides its preparation method simultaneously.
LED liquid silastic containing polysilsesquioxane of the present invention, be made up of the raw material of following parts by weight:
Wherein:
The described polysiloxane containing function base vinyl polysilsesquioxane structure is the polysiloxane of the ladder-like polysiloxane structure containing more than 2 alkenyls in the base of side, comprises a structure and a ' structure;
Described a structure is:
In formula, R
1and R
2for methyl, phenyl and/or vinyl; Link number n=1-10000;
Described a ' structure is:
In formula, link number m=1-1000;
The described polysiloxane containing function base hydrogen base polysilsesquioxane structure is the polysiloxane for the ladder-like polysiloxane structure containing more than 2 hydrogen bases in the base of side, comprises b structure and b ' structure;
Described b structure is:
In formula, R
11and R
22for methyl, phenyl and/or hydrogen base, link number X=1-1000,
Described b ' structure is:
In formula, link number Y=1-100;
The described dendritic organopolysiloxane containing unsaturated link(age) is the organopolysiloxane containing more than 2 alkenyl resin structures in molecule.
The described LED liquid silastic containing polysilsesquioxane is preferably made up of the raw material of following parts by weight:
Wherein:
The described polysiloxane containing function base vinyl polysilsesquioxane structure is the linear silicones containing more than 2 vinyl ladder-like polysiloxane structures in the base of side, and average viscosity is 4000-20000mPas.
The described polysiloxane containing function base hydrogen base polysilsesquioxane structure is the straight chain hydrogen containing siloxane containing more than 2 hydrogen base ladder-like polysiloxane structures in the base of side, and average viscosity is 30-1000mPas.
The described dendritic organopolysiloxane containing unsaturated link(age) is the one in vinyl polysiloxane or phenyl vinyl polysiloxane, and average viscosity is 4000-30000mPas.
Described platinum complex catalyst is platinum water or Ka Shi platinum catalyst; Inhibitor is alkynol class inhibitor, is preferably the one in propiolic alcohol, 1-ethynyl-1-hexalin, 2-phenyl-3-butyne-2-alcohol or methylbutynol; Tackifier are silicon rubber tackifier, are preferably KH560 or KH570.
The described polysiloxane containing function base vinyl polysilsesquioxane structure is adopted and is prepared with the following method:
(1) first, at 0-60 DEG C, reactant is joined in water and solvent and reacts 1-72h, after filtration, wash, dry in the base of side containing the polysilsesquioxane of function base vinyl;
Wherein, described reactant is one or more in vinyl trichloro silane, vinyltrimethoxy silane or vinyltriethoxysilane; Described solvent is one or more in acetone, toluene or acetonitrile, and solvent load is 0.1-10 times of reactant total mass; The consumption of water is 0.1-5 times of reactant total mass;
(2) polysilsesquioxane containing function base vinyl in side base step (1) prepared joins in DMC, phenyl ring body or vinyl ring body, add vinyl double-seal head, add Tetramethylammonium hydroxide silicon alkoxide again and react 4-6h at 100-140 DEG C, after destroying catalyzer, again at 150-170 DEG C of de-low 4h-6h, must containing the polysiloxane of function base vinyl polysilsesquioxane structure.
The described polysiloxane containing function base hydrogen base polysilsesquioxane structure is adopted and is prepared with the following method:
(1) first, at 60-80 DEG C, reactant is joined in water and solvent and reacts 1-24h, after filtration, wash, dry in the base of side containing the polysilsesquioxane of function base hydrogen base;
Wherein, described reactant is one or more in trichlorosilane, Trimethoxy silane or triethoxyl silane; Described solvent is toluene, and solvent load is 0.1-10 times of reactant total mass; The consumption of water is 0.1-5 times of reactant total mass;
(2) polysilsesquioxane containing function base hydrogen base in side base step (1) prepared joins in DMC, phenyl ring body or hydrogeneous ring body, add hydrogeneous double-seal head, the sulfuric acid adding 2% again reacts 4-6h at 25 DEG C, after catalyst neutralisation, again at 150-170 DEG C of de-low 4h-6h, must containing the polysiloxane of function base hydrogen base polysilsesquioxane structure.
The preparation method of the described LED liquid silastic containing polysilsesquioxane, comprises the steps:
(1) at room temperature mix containing polysiloxane 0-30 part of function base vinyl polysilsesquioxane structure, the dendritic organopolysiloxane 30-100 part containing unsaturated link(age), platinum complex catalyst 0.3-0.5 part, obtain A glue;
(2) at room temperature mix containing polysiloxane 30-100 part of function base vinyl polysilsesquioxane structure, the polysiloxane 1-30 part containing function base hydrogen base polysilsesquioxane structure, inhibitor 0.012-0.03 part, tackifier 0.5-2 part, obtain B glue;
(3) get A glue weight part same with B glue to mix, vacuum defoamation 5-30min, is placed in Teflon mould; Sulfuration 0.5-1.5h at 50-80 DEG C, then sulfuration 0.5-4h at 100-200 DEG C, obtain the described LED liquid silastic containing polysilsesquioxane.
Described sulfuration 0.5-4h at 100-200 DEG C, is preferably sulfuration 2-4h at 100-200 DEG C.
The mol ratio of the LED liquid silastic Si-Vi:Si-H containing polysilsesquioxane that step (3) prepares is 1:(0.5-1.8), be preferably 1:(1.0-1.5); Wherein, Si-Vi represents silico ethylene base, and Si-H represents silicon hydrogen base.
In sum, beneficial effect of the present invention is as follows:
(1) containing function base polysilsesquioxane structure polysiloxane because of in the base of side containing function base, as vinyl, hydrogen base, make the LED silicon rubber after solidifying can form Concentrative crosslinking point, so, substantially increase the mechanical mechanics properties such as the tensile strength of product, tear strength, tensile yield.
(2) containing in the polysiloxane of function base polysilsesquioxane structure because having the regular ladder structure of polysilsesquioxane, thus improve the thermotolerance of product.
(3) preparation method described in, comprises the preparation of A glue and B glue, and the A glue prepared and B glue can separately be preserved, and the storage for LED liquid silastic provides conveniently.
(4) the LED liquid silastic water white transparency prepared, transmittance >=99%, is very suitable for the embedding of LED, paster type encapsulation, can also be applied to the fields such as optical lens, solar cell substrate, touch-screen.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The all raw materials used in embodiment, except specified otherwise, are commercial.
Embodiment 1
Preparation containing the polysiloxane of function base vinyl polysilsesquioxane structure:
200mL solvent toluene is added in the there-necked flask that 500mL is clean, 100mL deionized water, then at 0 DEG C, 100g vinyl trichloro silane is added in about 15min under mechanical stirring, reaction 72h, after filtration, 18.7g vinyl ladder-like polysiloxane is obtained after washing, the vinyl ladder-like polysiloxane prepared is added in the 1000mL flask that 500g dehydration DMC is housed, add 10g vinyl double-seal head again, 20ppm tetramethyl-aqua ammonia silicon alkoxide, at 100 DEG C of copolymerization 4h, catalyzer 2h is destroyed at 165 DEG C, then at 150 DEG C of de-low 4h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base vinyl polysilsesquioxane structure in the base of side.
Preparation containing the polysiloxane of function base hydrogen base polysilsesquioxane structure:
200mL solvent toluene is added in the there-necked flask that 500mL is clean, 100mL deionized water, then at 60 DEG C, 100g trichlorosilane is added in about 30min under mechanical stirring, reaction 24h, after filtration, washing, obtain the hydrogeneous ladder-like polysiloxane of 10g, the hydrogeneous ladder-like polysiloxane prepared is added in the 500mL flask of the DMC 100g that dehydration is housed, add again the hydrogeneous double-seal head of 20g and 2% sulfuric acid at 25 DEG C of copolymerization 4h, then, to add in excess of sodium carbonate and after, filter, de-low 4h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base hydrogen base polysilsesquioxane structure in the base of side.
Preparation containing the LED liquid silastic of polysilsesquioxane:
To 60.0g vinyl polysiloxane, add the Ka Shi platinum catalyst of 0.50g 3000ppm, entirety mixes rear discharging, is prepared into LED A glue; To 55.0g containing in the polysiloxane of function base vinyl polysilsesquioxane structure, add the polysiloxane of 4.50g containing function base hydrogen base polysilsesquioxane structure, 0.017g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH560 of 0.95g, mix, be prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 10min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 2h, obtains the product test sample of smooth cleaning.
Embodiment 2
Preparation containing the polysiloxane of function base vinyl polysilsesquioxane structure:
250mL solvent acetone is added in the there-necked flask that 500mL is clean, 5mL deionized water, then at 50 DEG C, 50g vinyltrimethoxy silane is added in about 30min under mechanical stirring, reaction 13h, after filtration, the trapezoidal vinyl polysilsesquioxane of 13g is obtained after washing, the vinyl polysilsesquioxane prepared is added in the 1000mL flask that vinyl ring body 400g is housed, add 10g vinyl double-seal head and 10ppm tetramethyl-aqua ammonia silicon alkoxide again, at 140 DEG C of copolymerization 6h, catalyzer 2h is destroyed at 165 DEG C, then at 170 DEG C of de-low 6h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base vinyl polysilsesquioxane structure.
Preparation containing the polysiloxane of function base hydrogen base polysilsesquioxane structure:
200mL solvent toluene is added in the there-necked flask that 500mL is clean, 100mL deionized water, then at 70 DEG C, 90.0g Trimethoxy silane is added in about 30min under mechanical stirring, reaction 24h, after filtration, washing, obtain the hydrogeneous trapezoidal silsesquioxane of 10g, the hydrogeneous ladder-like polysiloxane prepared is added in the 500mL flask that hydrogeneous ring body 100g is housed, add again the hydrogeneous double-seal head of 20g and 2% sulfuric acid in 25 DEG C of copolymerization 4h, then, to add in excess bicarbonate and after, filter, de-low 4h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base hydrogen base polysilsesquioxane structure in the base of side.
Preparation containing the LED liquid silastic of polysilsesquioxane:
To 10.0g containing in the polysiloxane of function base vinyl polysilsesquioxane structure, add the Ka Shi platinum catalyst of 33.5g vinyl polysiloxane and 0.36g 3000ppm, after entirety mixes, be prepared into LED A glue; To 40g containing in the polysiloxane of function base vinyl polysilsesquioxane structure, add the polysiloxane of 3.50g containing function base hydrogen base polysilsesquioxane structure, 0.012g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH570 of 0.90g, is prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 20min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 2h, obtains the product test sample of smooth cleaning.
Embodiment 3
Preparation containing the polysiloxane of function base vinyl polysilsesquioxane structure:
250mL acetonitrile is added in the there-necked flask that 500mL is clean, 50mL deionized water, then at 60 DEG C, 25.7g vinyltriethoxysilane and 107.0g phenyltrimethoxysila,e is added in about 30min under mechanical stirring, reaction 72h, after filtration, 28g vinyl polysilsesquioxane is obtained after carrying out washing treatment, the vinyl polysilsesquioxane of preparation is added in the 1000mL flask that 800g dehydration phenyl ring body is housed, add 10g vinyl double-seal head again, add 20ppm tetramethyl-aqua ammonia silicon alkoxide, at 120 DEG C of copolymerization 5h, catalyzer 2h is destroyed at 170 DEG C, then at 170 DEG C of de-low 4h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base vinyl polysilsesquioxane structure.
Preparation containing the polysiloxane of function base hydrogen base polysilsesquioxane structure:
250mL solvent toluene is added in the there-necked flask that 500mL is clean, 50mL deionized water, then at 80 DEG C, 27.84g triethoxyl silane and 35g phenyl front three chlorosilane is added in about 30min under mechanical stirring, reaction 13h, after filtration after washing, obtain the hydrogeneous polysilsesquioxane of 17g, by the hydrogeneous ladder-like polysiloxane of preparation, add in the 500mL flask that hydrogeneous ring body 100g is housed, add again the hydrogeneous double-seal head of 15g and 4% sulfuric acid at 25 DEG C of copolymerization 4h, then, to add in excess of sodium carbonate and after, filter, de-low 4h, volatile matter is reduced to less than 1%, obtain the polysiloxane containing function base hydrogen base polysilsesquioxane structure.
Preparation containing the LED liquid silastic of polysilsesquioxane:
To 80.0g phenyl vinyl polysiloxane, add the Ka Shi platinum catalyst of 0.36g 3000ppm, be prepared into LED A glue; To the above-mentioned preparation of 50.0g containing function base vinyl polysilsesquioxane structure polysiloxane in, add the polysiloxane containing function base hydrogen base polysilsesquioxane structure of the above-mentioned preparation of 30g, 0.015g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH560 of 0.81g, mix, be prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 10min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 3h, obtains the product test sample of smooth cleaning.
Comparative example 1
To 60.0g vinyl polysiloxane, add the Ka Shi platinum catalyst of 0.50g 3000ppm, entirety mixes rear discharging, is prepared into LED A glue; To in 55.0g vinyl silicone oil, add 4.50g containing hydrogen silicone oil, 0.017g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH560 of 0.95g, mixes, is prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 10min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 2h, obtains the product test sample of smooth cleaning.
Comparative example 2
To in 10.0g vinyl silicone oil, add the Ka Shi platinum catalyst of 33.5g vinyl polysiloxane and 0.36g 3000ppm, after entirety mixes, be prepared into LED A glue; To in 40g vinyl silicone oil, add 3.50g hydrogen base star polysiloxane, 0.012g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH570 of 0.90g, is prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 20min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 2h, obtains the product test sample of smooth cleaning.
Comparative example 3
To 80.0g phenyl vinyl polysiloxane, add the Ka Shi platinum catalyst of 0.36g 3000ppm, be prepared into LED A glue; To in 50.0g phenyl-vinyl silicon oil, add 30g phenyl Silicon Containing Hydrogen resin, 0.015g 1-ethynyl-1-hexalin, the silicon rubber tackifier KH560 of 0.81g, mixes, is prepared into LED B glue; Finally, after obtained LED A glue and B glue being mixed at ambient temperature, vacuum defoamation 10min, is placed in Teflon mould, levelling; Sulfuration 1h at 80 DEG C, then at 150 DEG C of sulfuration 3h, obtains the product test sample of smooth cleaning.
Tensile strength and the tensile yield of the product test sample above embodiment and comparative example obtained respectively are tested according to GB/T528-1998, tear strength is tested according to GB/T529-1999, hardness is according to GB/T531-1999, specific refractory power adopts Abbe refractometer to test at 25 DEG C, and transmittance adopts the testing plate that ultraviolet-visible spectrophotometer test 1mm is thick.Test result is as shown in table 1.
The performance test results of table 1 embodiment 1-3 and comparative example 1-3 sample
Contrasted from the detected result of table 1 embodiment 1-2 and comparative example 1-2, embodiment 1-2 is polymkeric substance based on the polysiloxane containing function base vinyl polysilsesquioxane structure, be linking agent containing function base hydrogen base polysilsesquioxane, make the tensile strength of LED liquid silastic, tear strength, the mechanical mechanics properties such as tensile yield have had than the silicon rubber (comparative example 1-2) of common preparation and have significantly improved, wherein, tensile strength improves more than 25%, tear strength improves more than 30%, tensile yield improves more than 30%, hardness there has also been and significantly improves.
Contrasted from the detected result of table 1 embodiment 1-3 and comparative example 1-3, at 200 DEG C, toast 72h, embodiment 1-3, with because of containing ladder-like polysiloxane structure, makes LED liquid silastic degradation not obvious, elasticity is better, illustrates that its thermotolerance is good.
Claims (10)
1., containing a LED liquid silastic for polysilsesquioxane, it is characterized in that: be made up of the raw material of following parts by weight:
Wherein:
The described polysiloxane containing function base vinyl polysilsesquioxane structure is the polysiloxane of the ladder-like polysiloxane structure containing more than 2 alkenyls in the base of side, comprises a structure and a ' structure;
Described a structure is:
In formula, R
1and R
2for methyl, phenyl and/or vinyl; Link number n=1-10000;
Described a ' structure is:
In formula, link number m=1-1000;
The described polysiloxane containing function base hydrogen base polysilsesquioxane structure is the polysiloxane for the ladder-like polysiloxane structure containing more than 2 hydrogen bases in the base of side, comprises b structure and b ' structure;
Described b structure is:
In formula, R
11and R
22for methyl, phenyl and/or hydrogen base, link number X=1-1000,
Described b ' structure is:
In formula, link number Y=1-100;
The described dendritic organopolysiloxane containing unsaturated link(age) is the organopolysiloxane containing more than 2 alkenyl resin structures in molecule.
2. the LED liquid silastic containing polysilsesquioxane according to claim 1, is characterized in that: be made up of the raw material of following parts by weight:
3. the LED liquid silastic containing polysilsesquioxane according to claim 1, it is characterized in that: the described polysiloxane containing function base vinyl polysilsesquioxane structure is the linear silicones containing more than 2 vinyl ladder-like polysiloxane structures in the base of side, and average viscosity is 4000-20000mPas.
4. the LED liquid silastic containing polysilsesquioxane according to claim 1, it is characterized in that: the described polysiloxane containing function base hydrogen base polysilsesquioxane structure is the straight chain hydrogen containing siloxane containing more than 2 hydrogen base ladder-like polysiloxane structures in the base of side, and average viscosity is 30-1000mPas.
5. the LED liquid silastic containing polysilsesquioxane according to claim 1, it is characterized in that: the described dendritic organopolysiloxane containing unsaturated link(age) is the one in vinyl polysiloxane or phenyl vinyl polysiloxane, and average viscosity is 4000-30000mPas.
6. the LED liquid silastic containing polysilsesquioxane according to claim 1, is characterized in that: described platinum complex catalyst is platinum water or Ka Shi platinum catalyst; Inhibitor is alkynol class inhibitor; Tackifier are silicon rubber tackifier.
7. the LED liquid silastic containing polysilsesquioxane according to claim 1, is characterized in that: the described polysiloxane containing function base vinyl polysilsesquioxane structure is adopted and prepared with the following method:
(1) first, at 0-60 DEG C, reactant is joined in water and solvent and reacts 1-72h, after filtration, wash, dry in the base of side containing the polysilsesquioxane of function base vinyl;
Wherein, described reactant is one or more in vinyl trichloro silane, vinyltrimethoxy silane or vinyltriethoxysilane; Described solvent is one or more in acetone, toluene or acetonitrile, and solvent load is 0.1-10 times of reactant total mass; The consumption of water is 0.1-5 times of reactant total mass;
(2) polysilsesquioxane containing function base vinyl in side base step (1) prepared joins in DMC, phenyl ring body or vinyl ring body, add vinyl double-seal head, add Tetramethylammonium hydroxide silicon alkoxide again and react 4-6h at 100-140 DEG C, after destroying catalyzer, again at 150-170 DEG C of de-low 4h-6h, must containing the polysiloxane of function base vinyl polysilsesquioxane structure.
8. the LED liquid silastic containing polysilsesquioxane according to claim 1, is characterized in that: the described polysiloxane containing function base hydrogen base polysilsesquioxane structure is adopted and prepared with the following method:
(1) first, at 60-80 DEG C, reactant is joined in water and solvent and reacts 1-24h, after filtration, wash, dry in the base of side containing the polysilsesquioxane of function base hydrogen base;
Wherein, described reactant is one or more in trichlorosilane, Trimethoxy silane or triethoxyl silane; Described solvent is toluene, and solvent load is 0.1-10 times of reactant total mass; The consumption of water is 0.1-5 times of reactant total mass;
(2) polysilsesquioxane containing function base hydrogen base in side base step (1) prepared joins in DMC, phenyl ring body or hydrogeneous ring body, add hydrogeneous double-seal head, the sulfuric acid adding 2% again reacts 4-6h at 25 DEG C, after catalyst neutralisation, again at 150-170 DEG C of de-low 4h-6h, must containing the polysiloxane of function base hydrogen base polysilsesquioxane structure.
9. a preparation method for the arbitrary described LED liquid silastic containing polysilsesquioxane of claim 1-8, is characterized in that: comprise the steps:
(1) at room temperature mix containing polysiloxane 0-30 part of function base vinyl polysilsesquioxane structure, the dendritic organopolysiloxane 30-100 part containing unsaturated link(age), platinum complex catalyst 0.3-0.5 part, obtain A glue;
(2) at room temperature mix containing polysiloxane 30-100 part of function base vinyl polysilsesquioxane structure, the polysiloxane 1-30 part containing function base hydrogen base polysilsesquioxane structure, inhibitor 0.012-0.03 part, tackifier 0.5-2 part, obtain B glue;
(3) get A glue weight part same with B glue to mix, vacuum defoamation 5-30min, is placed in Teflon mould; Sulfuration 0.5-1.5h at 50-80 DEG C, then sulfuration 0.5-4h at 100-200 DEG C, obtain the described LED liquid silastic containing polysilsesquioxane.
10. the preparation method of the LED liquid silastic containing polysilsesquioxane according to claim 9, is characterized in that: the mol ratio of the LED liquid silastic Si-Vi:Si-H containing polysilsesquioxane that step (3) prepares is 1:(0.5-1.8); Wherein, Si-Vi represents silico ethylene base, and Si-H represents silicon hydrogen base.
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| CN110607163A (en) * | 2019-10-31 | 2019-12-24 | 东莞市贝特利新材料有限公司 | EMC packaging silica gel and application |
| CN111718446A (en) * | 2019-03-18 | 2020-09-29 | 陆筱棣 | Method for preparing polymer microspheres, obtained polymer microspheres and application |
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| CN106543440B (en) * | 2016-10-31 | 2019-08-20 | 上海大学 | Annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof |
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| CN111718446A (en) * | 2019-03-18 | 2020-09-29 | 陆筱棣 | Method for preparing polymer microspheres, obtained polymer microspheres and application |
| CN110607163A (en) * | 2019-10-31 | 2019-12-24 | 东莞市贝特利新材料有限公司 | EMC packaging silica gel and application |
| CN110607163B (en) * | 2019-10-31 | 2021-11-12 | 东莞市贝特利新材料有限公司 | EMC packaging silica gel and application |
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| CN111793366A (en) * | 2020-08-07 | 2020-10-20 | 东莞市固泰有机硅有限公司 | White carbon black-free solid silicon rubber for high-hardness rubber roller and preparation method thereof |
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