CN106753129A - A kind of LED tack coats are modified enhanced high heat conduction type epoxy resin composite material and preparation method thereof with hyperbranched surface - Google Patents
A kind of LED tack coats are modified enhanced high heat conduction type epoxy resin composite material and preparation method thereof with hyperbranched surface Download PDFInfo
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- CN106753129A CN106753129A CN201611167318.4A CN201611167318A CN106753129A CN 106753129 A CN106753129 A CN 106753129A CN 201611167318 A CN201611167318 A CN 201611167318A CN 106753129 A CN106753129 A CN 106753129A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
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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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4223—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aromatic
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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
- C09J11/04—Non-macromolecular additives inorganic
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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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- 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
- C09J11/08—Macromolecular additives
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
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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
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Abstract
It is modified enhanced high heat conduction type epoxy resin composite material, and its preparation technology with hyperbranched surface the invention discloses a kind of LED tack coats, it is characterised in that with bisphenol A type epoxy resin E 51, B4C powder, Al2O3, 107 glue, dibutyl tin laurate, tetraethyl orthosilicate, graphene oxide, N methyl pyrrolidones, 3,5 diaminobenzoic acids, pyridine, triphenylphosphine, PTS, multi-walled carbon nano-tubes, methyl hexahydrophthalic anhydride, silicone emulsion etc. be raw material.The present invention is with B4C powder, Al2O3It is filler, is prepared for the heat-conducting silicon rubber of KH550 surface treatments；Graphene oxide is carried out with ethylenediamine amino modified；The method for passing through chemical modification with PTS, is prepared for modifying epoxy resin by organosilicon；It is prepared for CNT reinforced epoxy based composites, excellent in mechanical performance.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of LED tack coats are modified enhanced height with hyperbranched surface
Heat-conducting type epoxy resin composite material, and its preparation technology.
Background technology
The use of solid-state illumination white light LEDs is more and more extensive, but, because the environment temperature and node residing for LED are arrived
The thermal resistance of environment has material impact, therefore great power LED to its luminous efficiency, service life
Efficient stable heat dissipation problem turn into influence its popularization and application significant obstacle.
Huge Hong Zong is in master thesis《Influence of the epoxy composite material tack coat to LED junction temperature》In one text, using mixing
The method of miscellaneous micrometer alumina and boron carbide is improved to the heat conductivility and adhesive property of epoxy resin, is prepared for high heat conduction
Epoxy resin composite material.In order to improve particle dispersiveness in the epoxy, the number of bubbles after solidification is reduced, to filler
It is dried treatment：By B4C、Al2O3Powder is dried in being put into drying box at 100 DEG C, adds KH-550, absolute ethyl alcohol, ultrasound
Then dispersion, magnetic agitation dries in 80 DEG C of baking oven.The preparation of epoxy resin composite material：To bisphenol A type epoxy resin
The particulate after dried process is added in E-51, is put into 80 DEG C of baking ovens, add amine curing agent, stirring adds defoamer vacuum
Deaeration, is then placed in mould and solidifies in 80 DEG C of drying box.But it is not enough to there is heat conductivility.
The a certain adhesive linkage that epoxy resin composite material prepared by the present invention is used in great power LED.With B4C powder,
Al2O3It is filler, with tetraethyl orthosilicate as vulcanizing agent, with dibutyl tin laurate as catalyst, is prepared at KH550 surfaces
The heat-conducting silicon rubber of reason, improves the heat conductivility of silicon rubber；Graphene oxide is carried out with ethylenediamine amino modified, successfully connect
Enter amino, the calorifics and mechanical property of epoxy resin can be significantly improved；With poly- MTES (PTS) by chemistry
Modified method, is prepared for modifying epoxy resin by organosilicon, and the hydrolysate of PTS is mainly with the hydroxyl generation in epoxy resin instead
Should, organosilicon is successfully introduced into epoxy resin；With methyl hexahydrophthalic anhydride as curing agent, with silicone emulsion as defoamer, by super
Sound dispersion is prepared for CNT reinforced epoxy based composites, excellent in mechanical performance.Obtain a kind of LED tack coats and use super
Branched surface is modified enhanced high heat conduction type epoxy resin composite material.
The content of the invention
Led with the hyperbranched surface enhanced height that is modified the present invention solves the technical problem of a kind of LED tack coats are provided
Heat type epoxy resin composite material and its preparation technology, the thermal conductivity of composite materials made according to the technique are high, can be preferably
Improve the radiating of LED, mechanical property is good.
The technical problems to be solved by the invention are realized using following technical scheme：
Bisphenol A type epoxy resin E-51 23-32, B4C powder 6-10, Al2O33-8,107 glue 2-4, two
Dibutyl tin laurate 3-5, tetraethyl orthosilicate 4-7, graphene oxide 6-10, ethylenediamine 3-5,1-METHYLPYRROLIDONE 2-
4,3,5- diaminobenzoic acid 2-3, pyridine 1-2, triphenylphosphine 1-3, PTS 2-4, multi-walled carbon nano-tubes 7-12, methyl hexahydrobenzene
Acid anhydride 4-8, silicone emulsion 3-5, KH550, ethanol, distilled water, DMF, appropriate concentrated nitric acid.
A kind of LED tack coats are modified the preparation side of enhanced high heat conduction type epoxy resin composite material with hyperbranched surface
Method, it is characterised in that carry out according to the following steps：
A. by Al2O3、B4C powder dries 2-3h in being put into drying box at 90-110 DEG C, is down to room temperature, adds KH550, second
Alcohol, ultrasonic disperse 1-2h, filtering, 70-90 DEG C of vacuum drying is ground, 100-200 mesh sieves is crossed, by gained powder and 107 glue, 1-2
Part dibutyl tin laurate, tetraethyl orthosilicate mixing, stir 1-2h；
B. in graphene oxide 1:2-4 adds DMF, then mixes with ethylenediamine, ultrasonically treated 1-2h, in 110-130 DEG C of reaction
4-8h, filtering, alcohol wash water are washed 3-5 times, 70-90 DEG C of drying, add bisphenol A type epoxy resin E-51 to stir, in 140-160
2-3h, cooling, sealing preserve are heated in DEG C vacuum tank；
C. in multi-walled carbon nano-tubes 1:20-30 adds concentrated nitric acid, is heated to boiling, and condensing reflux 3-5h is filtered, is washed to
Neutrality, is distributed in 1-METHYLPYRROLIDONE, 3,5- diaminobenzoic acids, pyridine and triphenylphosphine is added, in 100-110 DEG C of nitrogen
3-6h is reacted under gas atmosphere, room temperature is cooled to, it is stand-by；
D. resulting material in b is mixed with PTS, is warming up to 75-95 DEG C and stirs, 1:2-5 is added dropwise remaining part tin dilaurate two
Butyl tin and distilled water, isothermal reaction 3-5h add resulting material in c, sonic oscillation stirring 1-2h；
E. a, d resulting material are mixed, adds methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1-2h to add silicone emulsion in 60-
80 DEG C of vacuum defoamation 1-2h, are poured into mould, and 2-5h is solidified in 80-150 DEG C of drying box, and natural cooling obtains one kind
LED tack coats are modified enhanced high heat conduction type epoxy resin composite material with hyperbranched surface.
Reaction mechanism of the invention is as follows：
（1）With Al2O3、B4C powder is filler, with tetraethyl orthosilicate as vulcanizing agent, with dibutyl tin laurate as catalyst,
The heat-conducting silicon rubber of KH550 surface treatments is prepared for, the heat conductivility of silicon rubber is improve.
（2）Graphene oxide has radius-thickness ratio high, heat conduction master batch is formed after thermal reduction and forms heat conduction in the composite
Path, is carried out amino modified with ethylenediamine to graphene oxide, is successfully accessed amino, can significantly improve the calorifics of epoxy resin
And mechanical property.
（3）The method for passing through chemical modification with poly- MTES (PTS), is prepared for modifying epoxy resin by organosilicon,
The hydrolysate of PTS is mainly and is reacted with the hydroxyl in epoxy resin, and organosilicon is successfully introduced into epoxy resin, chemical modification
Epoxy resin product has excellent tensile strength and elongation at break, heat endurance.
（4）With methyl hexahydrophthalic anhydride as curing agent, with silicone emulsion as defoamer, carbon nanometer is prepared for by ultrasonic disperse
Pipe reinforced epoxy based composites, mechanical property, excellent thermal conductivity.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of LED tack coats are modified enhanced high heat conduction type epoxy resin composite material with hyperbranched surface, by following heavy
The raw material of amount part (g) is obtained：
Bisphenol A type epoxy resin E-51 32, B4C powder 10, Al2O38,107 glue 4, tin dilaurate two
Butyl tin 5, tetraethyl orthosilicate 7, graphene oxide 10, ethylenediamine 5,1-METHYLPYRROLIDONE 4,3,5- diaminobenzoic acids
3, pyridine 2, triphenylphosphine 3, PTS 4, multi-walled carbon nano-tubes 12, methyl hexahydrophthalic anhydride 8, silicone emulsion 5, KH550, ethanol, steaming
Distilled water, DMF, appropriate concentrated nitric acid.
A kind of LED tack coats are modified the preparation side of enhanced high heat conduction type epoxy resin composite material with hyperbranched surface
Method, it is characterised in that carry out according to the following steps：
A. by Al2O3、B4C powder dries 2h in being put into drying box at 90-100 DEG C, is down to room temperature, adds KH550, ethanol,
Ultrasonic disperse 1h, filtering, 70-80 DEG C of vacuum drying is ground, 100 mesh sieves is crossed, by gained powder and 107 glue, 1-2 part of two bays
Sour dibutyl tin, tetraethyl orthosilicate mixing, stir 2h；
B. in graphene oxide 1:4 add DMF, then mix with ethylenediamine, ultrasonically treated 1h, and 4h is reacted at 120-130 DEG C,
Filtering, alcohol wash water are washed 3 times, and 70-80 DEG C of drying adds bisphenol A type epoxy resin E-51 to stir, in 150-160 DEG C of vacuum
2h, cooling, sealing preserve are heated in case；
C. in multi-walled carbon nano-tubes 1:20 add concentrated nitric acid, are heated to boiling, and condensing reflux 3h is filtered, is washed to neutrality,
It is distributed in 1-METHYLPYRROLIDONE, 3,5- diaminobenzoic acids, pyridine and triphenylphosphine is added, in 100-110 DEG C of nitrogen gas
3h is reacted under atmosphere, room temperature is cooled to, it is stand-by；
D. resulting material in b is mixed with PTS, is warming up to 85-95 DEG C and stirs, 1:5 are added dropwise the remaining fourth of part tin dilaurate two
Ji Xi and distilled water, isothermal reaction 3h add resulting material in c, sonic oscillation stirring 1-2h；
E. a, d resulting material are mixed, adds methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1h to add silicone emulsion in 70-80
DEG C vacuum defoamation 2h, is poured into mould, and 3h is solidified in 100-120 DEG C of drying box, and natural cooling obtains a kind of LED and glues
Knot layer is modified enhanced high heat conduction type epoxy resin composite material with hyperbranched surface.
A kind of LED tack coats prepared by above-described embodiment are modified enhanced high heat conduction type epoxy resin composite wood with hyperbranched surface
The performance test results of material are as follows：
Thermal conductivity >=5.4 W/mK, tensile strength >=75.9MPa, bending strength >=139.8MPa, bending modulus >=4.5GPa,
Elongation at break >=21.9%.
Claims (2)
1. a kind of LED tack coats are modified enhanced high heat conduction type epoxy resin composite material with hyperbranched surface, it is characterised in that
It is obtained by the raw material of following weight parts：
Bisphenol A type epoxy resin E-51 23-32, B4C powder 6-10, Al2O33-8,107 glue 2-4, two
Dibutyl tin laurate 3-5, tetraethyl orthosilicate 4-7, graphene oxide 6-10, ethylenediamine 3-5,1-METHYLPYRROLIDONE 2-
4,3,5- diaminobenzoic acid 2-3, pyridine 1-2, triphenylphosphine 1-3, PTS 2-4, multi-walled carbon nano-tubes 7-12, methyl hexahydrobenzene
Acid anhydride 4-8, silicone emulsion 3-5, KH550, ethanol, distilled water, DMF, appropriate concentrated nitric acid.
2. a kind of LED tack coats according to claim 1 are modified enhanced high heat conduction type epoxy resin with hyperbranched surface
The preparation method of composite, it is characterised in that carry out according to the following steps：
A. by Al2O3、B4C powder dries 2-3h in being put into drying box at 90-110 DEG C, is down to room temperature, adds KH550, second
Alcohol, ultrasonic disperse 1-2h, filtering, 70-90 DEG C of vacuum drying is ground, 100-200 mesh sieves is crossed, by gained powder and 107 glue, 1-2
Part dibutyl tin laurate, tetraethyl orthosilicate mixing, stir 1-2h；
B. in graphene oxide 1:2-4 adds DMF, then mixes with ethylenediamine, ultrasonically treated 1-2h, in 110-130 DEG C of reaction
4-8h, filtering, alcohol wash water are washed 3-5 times, 70-90 DEG C of drying, add bisphenol A type epoxy resin E-51 to stir, in 140-160
2-3h, cooling, sealing preserve are heated in DEG C vacuum tank；
C. in multi-walled carbon nano-tubes 1:20-30 adds concentrated nitric acid, is heated to boiling, and condensing reflux 3-5h is filtered, is washed to
Neutrality, is distributed in 1-METHYLPYRROLIDONE, 3,5- diaminobenzoic acids, pyridine and triphenylphosphine is added, in 100-110 DEG C of nitrogen
3-6h is reacted under gas atmosphere, room temperature is cooled to, it is stand-by；
D. resulting material in b is mixed with PTS, is warming up to 75-95 DEG C and stirs, 1:2-5 is added dropwise remaining part tin dilaurate two
Butyl tin and distilled water, isothermal reaction 3-5h add resulting material in c, sonic oscillation stirring 1-2h；
E. a, d resulting material are mixed, adds methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1-2h to add silicone emulsion in 60-
80 DEG C of vacuum defoamation 1-2h, are poured into mould, and 2-5h is solidified in 80-150 DEG C of drying box, and natural cooling obtains one kind
LED tack coats are modified enhanced high heat conduction type epoxy resin composite material with hyperbranched surface.
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| CN201611167318.4A CN106753129A (en) | 2016-12-16 | 2016-12-16 | A kind of LED tack coats are modified enhanced high heat conduction type epoxy resin composite material and preparation method thereof with hyperbranched surface |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418490A (en) * | 2017-09-26 | 2017-12-01 | 安徽大松树脂有限公司 | A kind of epoxy resin adhesive containing graphene oxide |
| CN109935663A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of preparation method of composite material film and QLED device |
| CN112980292A (en) * | 2021-03-01 | 2021-06-18 | 杜磊 | Super-wear-resistant toughened modified waterborne epoxy resin floor paint and preparation method thereof |
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| CN103467917A (en) * | 2013-08-22 | 2013-12-25 | 上海交通大学 | Preparation method of modified compound filler filled breakdown-resisting epoxy composite |
| CN103525005A (en) * | 2013-08-22 | 2014-01-22 | 上海交通大学 | Preparation method of epoxy composite material with low packing content, high thermal conductivity and ternary nano/micro structure |
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2016
- 2016-12-16 CN CN201611167318.4A patent/CN106753129A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467917A (en) * | 2013-08-22 | 2013-12-25 | 上海交通大学 | Preparation method of modified compound filler filled breakdown-resisting epoxy composite |
| CN103525005A (en) * | 2013-08-22 | 2014-01-22 | 上海交通大学 | Preparation method of epoxy composite material with low packing content, high thermal conductivity and ternary nano/micro structure |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418490A (en) * | 2017-09-26 | 2017-12-01 | 安徽大松树脂有限公司 | A kind of epoxy resin adhesive containing graphene oxide |
| CN109935663A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of preparation method of composite material film and QLED device |
| CN112980292A (en) * | 2021-03-01 | 2021-06-18 | 杜磊 | Super-wear-resistant toughened modified waterborne epoxy resin floor paint and preparation method thereof |
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Application publication date: 20170531 |