CN106751512A - A kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP and preparation method thereof - Google Patents

A kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP and preparation method thereof Download PDF

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Publication number
CN106751512A
CN106751512A CN201611166161.3A CN201611166161A CN106751512A CN 106751512 A CN106751512 A CN 106751512A CN 201611166161 A CN201611166161 A CN 201611166161A CN 106751512 A CN106751512 A CN 106751512A
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epoxy resin
type epoxy
app
heat conduction
high heat
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CN201611166161.3A
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Inventor
李华生
刘勇
陈燕
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Priority to CN201611166161.3A priority Critical patent/CN106751512A/en
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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
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • 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
    • 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
    • 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
    • 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
    • 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 invention discloses a kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP, and its preparation technology, 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, ethylenediamine, PTS, multi-walled carbon nano-tubes, urea, APP, 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

A kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite wood of APP Material and preparation method thereof
Technical field
The present invention relates to field of compound material, and in particular to a kind of LED tack coats fire-retardant high heat conduction type of APP 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；The present invention makes with urea as raw material For the APP of urea-formaldehyde resin microcapsule, the compatibility and water resistance with epoxy resin are improved, have epoxy resin There are good heat endurance, excellent fire resistance；Obtain a kind of fire-retardant high heat conduction type epoxy of LED tack coats APP Resin composite materials.
The content of the invention
The present invention solves the technical problem of a kind of LED tack coats fire-retardant high heat conduction type ring of APP of offer Epoxy resin composite material and its preparation technology, the thermal conductivity of composite materials made according to the technique are high, can preferably improve LED Radiating, fire resistance is good, heat endurance is good
The technical problems to be solved by the invention are realized using following technical scheme：
Bisphenol A type epoxy resin E-51 22-28, B4C powder 4-9, Al2O33-8,107 glue 2-4, February
Dilaurylate 3-5, tetraethyl orthosilicate 4-7, graphene oxide 7-10, ethylenediamine 3-5, PTS 4-8, multi-wall carbon nano-tube Pipe 4-8, urea 4-8, APP 3-5, hexadecyltrimethylammonium chloride 0.5-1, methyl hexahydrophthalic anhydride 3-8, silicone emulsion 3-5, KH550, ethanol, distilled water, DMF, appropriate formalin.
A kind of LED tack coats preparation method of the fire-retardant high heat conduction type epoxy resin composite material of APP, it is special Levy and be, 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. 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 multi-walled carbon nano-tubes, sonic oscillation stirring 1-2h；
D. by urea and formalin with 1:2-4 mixes, and tune pH is 7-8, is warming up to 70-80 DEG C of reaction 2-3h, obtains A liquid；Will be poly- Ammonium phosphate 1:3-5 is added in ethanol, agitated under sonication 1-2h, adds A liquid, hexadecyltrimethylammonium chloride, is well mixed, and is adjusted PH is 4-5, is warming up to 80-90 DEG C of reaction 2-4h, and filtering, drying are stand-by；
E. by a, c, d resulting material mix, add methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1-2h, add silicone emulsion in 60-80 DEG C of vacuum defoamation 1-2h, is poured into mould, and 2-5h is solidified in 80-150 DEG C of drying box, and natural cooling obtains one Plant the LED tack coats enhanced high heat conduction type epoxy resin composite material of multi-walled carbon nano-tubes.
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）The present invention is prepared for the APP of urea-formaldehyde resin microcapsule with urea as raw material, improves and asphalt mixtures modified by epoxy resin The compatibility and water resistance of fat, make epoxy resin have good heat endurance, excellent fire resistance.
（5）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 fire-retardant high heat conduction type epoxy resin composite material of APP, by following weight parts (g) Raw material be obtained：
Bisphenol A type epoxy resin E-51 28, B4C powder 9, Al2O38,107 glue 4, the fourth of tin dilaurate two
Base tin 3, tetraethyl orthosilicate 7, graphene oxide 10, ethylenediamine 5, PTS 8, multi-walled carbon nano-tubes 8, urea 6, APP 5, hexadecyltrimethylammonium chloride 0.5, methyl hexahydrophthalic anhydride 8, silicone emulsion 5, KH550, ethanol, distilled water, DMF, Fu Er Appropriate Malin.
A kind of LED tack coats preparation method of the fire-retardant high heat conduction type epoxy resin composite material of APP, it is special Levy and be, carry out according to the following steps：
A. by Al2O3、B4C powder dries 2h in being put into drying box at 100-110 DEG C, is down to room temperature, adds KH550, ethanol, Ultrasonic disperse 1h, filtering, 80-90 DEG C of vacuum drying is ground, 200 mesh sieves is crossed, by gained powder and 107 glue, 1-2 part of two bays Sour dibutyl tin, tetraethyl orthosilicate mixing, stir 1h；
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 80-90 DEG C of drying adds bisphenol A type epoxy resin E-51 to stir, in 150-160 DEG C of vacuum 3h, cooling, sealing preserve are heated in case；
C. resulting material in b is mixed with PTS, is warming up to 85-95 DEG C and stirs, 1:4 are added dropwise the remaining fourth of part tin dilaurate two Ji Xi and distilled water, isothermal reaction 3h add multi-walled carbon nano-tubes, sonic oscillation stirring 1h；
D. by urea and formalin with 1:2 mixing, tune pH is 7-8, is warming up to 70-80 DEG C of reaction 2h, obtains A liquid；By polyphosphoric acid Ammonium 1:In 3 addition ethanol, agitated under sonication 1h adds A liquid, hexadecyltrimethylammonium chloride, is well mixed, and tune pH is 4-5, 80-90 DEG C of reaction 2h is warming up to, filtering, drying are stand-by；
E. a, c, d resulting material are mixed, adds methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1h to add silicone emulsion in 70- 80 DEG C of vacuum defoamation 2h, are poured into mould, and 2h is solidified in 130-150 DEG C of drying box, and natural cooling obtains a kind of LED The tack coat enhanced high heat conduction type epoxy resin composite material of multi-walled carbon nano-tubes.
A kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP prepared by above-described embodiment Performance test results it is 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%, UL94 has reached V-1.

Claims (2)

1. a kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP, it is characterised in that by following The raw material of weight portion is obtained：
Bisphenol A type epoxy resin E-51 22-28, B4C powder 4-9, Al2O33-8,107 glue 2-4, February
Dilaurylate 3-5, tetraethyl orthosilicate 4-7, graphene oxide 7-10, ethylenediamine 3-5, PTS 4-8, multi-wall carbon nano-tube Pipe 4-8, urea 4-8, APP 3-5, hexadecyltrimethylammonium chloride 0.5-1, methyl hexahydrophthalic anhydride 3-8, silicone emulsion 3-5, KH550, ethanol, distilled water, DMF, appropriate formalin.
2. a kind of LED tack coats according to claim 1 fire-retardant high heat conduction type epoxy resin composite wood of APP The preparation method of material, 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. 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 multi-walled carbon nano-tubes, sonic oscillation stirring 1-2h；
D. by urea and formalin with 1:2-4 mixes, and tune pH is 7-8, is warming up to 70-80 DEG C of reaction 2-3h, obtains A liquid；Will be poly- Ammonium phosphate 1:3-5 is added in ethanol, agitated under sonication 1-2h, adds A liquid, hexadecyltrimethylammonium chloride, is well mixed, and is adjusted PH is 4-5, is warming up to 80-90 DEG C of reaction 2-4h, and filtering, drying are stand-by；
E. by a, c, d resulting material mix, add methyl hexahydrophthalic anhydride, ultrasonic disperse treatment 1-2h, add silicone emulsion in 60-80 DEG C of vacuum defoamation 1-2h, is poured into mould, and 2-5h is solidified in 80-150 DEG C of drying box, and natural cooling obtains one Plant the LED tack coats enhanced high heat conduction type epoxy resin composite material of multi-walled carbon nano-tubes.
CN201611166161.3A 2016-12-16 2016-12-16 A kind of LED tack coats fire-retardant high heat conduction type epoxy resin composite material of APP and preparation method thereof Pending CN106751512A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108485593A (en) * 2018-01-22 2018-09-04 广州市白云化工实业有限公司 Organosilicon condensed type double-component casting glue and its application
CN111763406A (en) * 2020-08-05 2020-10-13 兰州交通大学 Preparation process of graphene nanocomposite

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Publication number Priority date Publication date Assignee Title
CN1148402A (en) * 1995-03-10 1997-04-23 东芝化学株式会社 Halogen-free flame-retardant epoxy resin composition
CN103694644A (en) * 2013-12-30 2014-04-02 景旺电子科技(龙川)有限公司 Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1148402A (en) * 1995-03-10 1997-04-23 东芝化学株式会社 Halogen-free flame-retardant epoxy resin composition
CN103694644A (en) * 2013-12-30 2014-04-02 景旺电子科技(龙川)有限公司 Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108485593A (en) * 2018-01-22 2018-09-04 广州市白云化工实业有限公司 Organosilicon condensed type double-component casting glue and its application
CN111763406A (en) * 2020-08-05 2020-10-13 兰州交通大学 Preparation process of graphene nanocomposite

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