CN106589856A - Carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for LED and preparation method of plastic - Google Patents
Carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for LED and preparation method of plastic Download PDFInfo
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- CN106589856A CN106589856A CN201611224826.1A CN201611224826A CN106589856A CN 106589856 A CN106589856 A CN 106589856A CN 201611224826 A CN201611224826 A CN 201611224826A CN 106589856 A CN106589856 A CN 106589856A
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for an LED and a preparation method of the plastic. The plastic is characterized by taking magnesium oxide, boron nitride, PBT, EVA, glass fiber, 107 glue, dibutyltin dilaurate, tetraethyl orthosilicate, melamine cyanurate, zinc borate, aluminum hypophosphite, bamboo charcoal, nano SiO2, butyltin chloride dihydroxide, graphene oxide, carbon fiber, aluminum oxide, 1-butyl-3-methylimidazolium hexafluorophosphate and the like as raw material. According to the plastic, H550 surface treated silicone rubber is prepared, butyltin chloride dihydroxide serves as a catalyst, and reinforcing and toughening treatment is conducted on polybutylene terephthalate (PBT) with nano SiO2; a composite flame retardant is prepared from aluminum hypophosphite and melamine cyanurate; the carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for the LED is obtained.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of flexible high heat conduction of LED carbon fibers-Graphene filling
Flame-resistant insulation plastic, and its preparation technology.
Background technology
LED has the advantages that small volume, life-span length, low-carbon environment-friendly, energy-conservation are stable as a kind of excellent photoelectric device,
It is expected that preferably general illumination light source of new generation will be become in following several years.As LED develops to high light intensity, high power,
Its heat dissipation problem is outstanding day by day, has had a strong impact on light output characteristic and the life-span of device of LED, it has also become high-power LED encapsulation must
The key issue that need to be solved., used as LED shell, with light weight, it is easy to machine-shaping, cost is low excellent for heat-conductive composite material
Point.
In order to improve the heat conductivility and mechanical property of heat-conductive composite material, to meet the use requirement of LED shell.
Ma Jieling is in its master thesis《The research of LED heat-conducting plastic》In, it is with polybutylene terephthalate (PBT) (PBT)
Matrix, with magnesium oxide and boron nitride as heat filling, adds ethylene-vinyl acetate copolymer (EVA) and glass fibre to enter it
The process of row activeness and quietness, using double screw extruder heat-conductive composite material is prepared for, and improves the heat conductivity of heat-conductive composite material
Energy and mechanical property, but there is heat conductivility deficiency, and do not possess fire resistance.
The present invention with magnesium oxide, boron nitride as filler, with tetraethyl orthosilicate as vulcanizing agent, be with dibutyl tin laurate
Catalyst, is prepared for the heat-conducting silicon rubber of KH550 surface treatments, improves the heat conductivility of silicone rubber；With dihydroxy butyl chloride
Change stannum is catalyst, uses Nano-meter SiO_22To polybutylene terephthalate (PBT)（PBT）Carry out activeness and quietness process；Hypo-aluminum orthophosphate
(AHP) phosphorus content height, good flame retardation effect, melamine cyanurate（MCA）It is a kind of typical nitrogen system bittern-free fire retardant, odorless
Tasteless, decomposition temperature is high, and low-smoke low-toxicity is prepared for composite flame-retardant agent；Carbon fiber is a kind of novel enhanced material of excellent performance,
There is low-density, height than strong and corrosion-resistant；The flexible high heat conduction for obtaining a kind of LED carbon fibers-Graphene filling is exhausted
The fire-retardant plastic of edge.
The content of the invention
The invention mainly solves the technical problem of providing a kind of flexible high heat conduction of LED carbon fibers-Graphene filling
Flame-resistant insulation plastic and its preparation technology, it is the thermal conductivity of composite materials height made according to the technique, good insulation preformance, fire-retardant
Performance is good, can preferably improve the radiating of LED.
The technical problem to be solved is realized using following technical scheme：
The glue 2-5 of magnesium oxide 5-8, boron nitride 8-13, PBT 10-25, EVA 5-10, glass fibre 4-10,107, tin dilaurate two
Butyl tin 1-2, tetraethyl orthosilicate 1-3, melamine cyanurate 3-7, Firebrake ZB 2-5, hypo-aluminum orthophosphate 2-6, bamboo charcoal 1-2, receives
Rice SiO2 2-3, dihydroxy dibutyl tin oxide 1-2, graphene oxide 2-5, carbon fiber 4-6, aluminium oxide 2-4,1- butyl -3- methyl
Limidazolium hexafluorophosphate 3-5, cumyl peroxide 0.1-0.5, KH550 1-2, ethanol, acetone, NaOH solution, distilled water are fitted
Amount.
A kind of preparation method of the fire-retardant plastic of flexible high heat conductive insulating of LED carbon fibers-Graphene filling, its feature
It is to carry out according to the following steps：
A. KH550 is mixed with ethanol, heating in water bath to 70-90 DEG C, adds magnesium oxide and boron nitride, stir 10-30min, taken
Go out to stand 1-2h, with suction pipe upper solution is sucked, dry after 1-2h in 75-95 DEG C, mix with 107 glue, add tin dilaurate
Dibutyl tin, tetraethyl orthosilicate, stir 1-2h；
B. add NaOH solution in melamine cyanurate, stir, add Firebrake ZB, 65-95 DEG C of reaction 1- of intensification
3h, obtains thick white product, and sucking filtration, washing 3-5 time are dried 1-3h in 115-165 DEG C；By hypo-aluminum orthophosphate, bamboo charcoal in 100-150
DEG C drying 1-2h after, mix with the former, superfine grinding obtains composite flame-retardant agent；
C. PBT is heated to into 150-170 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, mix homogeneously adds two
Hydroxybutyl stannic chloride, after polyreaction 1-2h, moves in ice-water bath and crushes, and gained sample is done in 105-130 DEG C of vacuum
Dry 2-4h；
D. resulting material in c is added graphene oxide into, supersonic vibration 2-3h adds carbon fiber and acetone, mix homogeneously to surpass
Sound oscillation 1-2h；
E. EVA, aluminium oxide and 1- butyl -3- Methylimidazole .s hexafluorophosphates are dried into 6- in 60-80 DEG C of vacuum drying oven
10h；Dried EVA and cumyl peroxide dynamic vulcanization 10-20min at 80 DEG C -150 DEG C is added after being dried
Aluminium oxide and 1- butyl -3- Methylimidazole. hexafluorophosphates, in 160-180 DEG C of melt blending 10-30min, discharging is stand-by；
F. resulting material in a, d, e and other surplus stocks are put in homogenizer and stir 1-2h, be placed in twin-screw extrusion
In machine, in 200-250 DEG C of melting extrusion, the cooling of Jing air, granulator granulation, 75-95 DEG C of drying 4-8h in baking oven is placed into, taken
Go out, Jing injection machines obtain a kind of flexible high heat conductive insulating of LED carbon fibers-Graphene filling in 235-255 DEG C of injection mo(u)lding
Fire-retardant plastic.
The reaction mechanism of the present invention is as follows：
（1）With magnesium oxide, boron nitride as 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 silicone rubber is improve.
（2）Hypo-aluminum orthophosphate (AHP) has the advantages that phosphorus content height, good flame retardation effect, and the addition of synergist bamboo charcoal can promote
AHP degradeds are made to generate phosphoric acid and pyrophosphoric acid, in solid phase, phosphoric acid and pyrophosphoric acid can promote composite degradation into charcoal, and drop
The fine and close layer of charcoal produced after solution can prevent oxygen and heat transfer to inside polymeric matrix, be conducive to improving the anti-flammability of material
Energy；Melamine cyanurate (MCA) is a kind of typical nitrogen system bittern-free fire retardant, and odorless, tasteless, decomposition temperature is high, and low cigarette is low
Poison, is controlled using Firebrake ZB to MCA, makes Firebrake ZB dispersed deposition on MCA surfaces, and MCA is coated, and is separated into less
Independent reaction system so that the viscosity of reaction system remains at a relatively low level.
（3）Nano-meter SiO_22With specific surface area is big, nontoxic, high temperature resistant the features such as, be a kind of excellent reinforcing material；With two
Hydroxybutyl stannic chloride is catalyst, using Nano-meter SiO_22To polybutylene terephthalate (PBT)（PBT）Carry out at activeness and quietness
Reason.
（4）Graphene oxide has high radius-thickness ratio, heat conduction master batch is formed after thermal reduction and forms heat conduction in the composite
Path, composite has good mechanical property, an excellent heat conductivility, and preparation process is simple, with low cost.Carbon is fine
Dimension is a kind of novel enhanced material of excellent performance, has the advantages that low-density, height than strong and corrosion-resistant.
（5）The flexible high heat conductive insulating type composite that the present invention is obtained has the spy such as high heat conduction, flexible, good insulating
Property, heat filling aluminium oxide profile is regular and density is big, is uniformly distributed in ethylene-vinyl acetate copolymer (EVA) matrix, rises
The effect of high filling is arrived；The addition of ionic liquid 1-butyl-3-methyl imidazolium hexafluorophosphate enhances filler and EVA matrixes
Interface compatibility, be conducive to dispersion of the filler in EVA matrixes.
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
The fire-retardant plastic of flexible high heat conductive insulating of a kind of LED carbon fibers-Graphene filling, by following weight parts (g)
Raw material be obtained：
Magnesium oxide 8, boron nitride 13, PBT 25, EVA 10, the glue 2 of glass fibre 10,107, dibutyl tin laurate 1, positive silicic acid
Ethyl ester 3, melamine cyanurate 7, Firebrake ZB 2, hypo-aluminum orthophosphate 6, bamboo charcoal 1, Nano-meter SiO_22 3, dihydroxy dibutyl tin oxide 2,
Graphene oxide 5, carbon fiber 4, aluminium oxide 2,1- butyl -3- Methylimidazole .s hexafluorophosphate 5, cumyl peroxide 0.5,
KH550 1, ethanol, acetone, NaOH solution, distillation appropriate amount of water.
A kind of preparation method of the fire-retardant plastic of flexible high heat conductive insulating of LED carbon fibers-Graphene filling, its feature
It is to carry out according to the following steps：
A. KH550 is mixed with ethanol, heating in water bath to 80-90 DEG C, adds magnesium oxide and boron nitride, stir 30min, taken out quiet
Put 1h, with suction pipe upper solution sucked, in 85-95 DEG C dry 1h after, mix with 107 glue, add dibutyl tin laurate,
Tetraethyl orthosilicate, stirs 1h；
B. add NaOH solution in melamine cyanurate, stir, add Firebrake ZB, 85-95 DEG C of intensification to react 1h,
Thick white product is obtained, sucking filtration, washing 3 times are dried 1h in 145-165 DEG C；By hypo-aluminum orthophosphate, bamboo charcoal in 140-150 DEG C of drying
After 1h, mix with the former, superfine grinding obtains composite flame-retardant agent；
C. PBT is heated to into 150-160 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, mix homogeneously adds two
Hydroxybutyl stannic chloride, after polyreaction 2h, moves in ice-water bath and crushes, by gained sample in 120-130 DEG C of vacuum drying
2h；
D. resulting material in c is added graphene oxide into, supersonic vibration 2h adds carbon fiber and acetone, mix homogeneously, ultrasound
Vibration 1h；
E. EVA, aluminium oxide and 1- butyl -3- Methylimidazole .s hexafluorophosphates are dried into 6- in 60-80 DEG C of vacuum drying oven
10h；Dried EVA and cumyl peroxide dynamic vulcanization 10-20min at 80 DEG C -150 DEG C is added after being dried
Aluminium oxide and 1- butyl -3- Methylimidazole. hexafluorophosphates, in 160-180 DEG C of melt blending 10-30min, discharging is stand-by；
F. resulting material in a, d, e and other surplus stocks are put in homogenizer and stir 1h, be placed in double screw extruder
In, in 230-250 DEG C of melting extrusion, the cooling of Jing air, granulator granulation, 85-95 DEG C of drying 4h in baking oven is placed into, take out,
Jing injection machines obtain a kind of high heat conductive insulating flame retardant type of LED carbon fibers-Graphene filling in 245-255 DEG C of injection mo(u)lding
Plastics.
A kind of property of the fire-retardant plastic of flexible high heat conductive insulating of LED carbon fibers prepared by above-described embodiment-Graphene filling
Energy testing result is as follows：
Heat conductivity is 320.64W/m K, and thermal coefficient of expansion is 13.75 × 10-6·K-1(50-150 DEG C), tensile strength is
59.73MPa, bending strength is 44.84MPa, and impact strength is 3.94KJ/m2, elongation at break is up to 13.55%.
Claims (2)
1. the fire-retardant plastic of flexible high heat conductive insulating that a kind of LED carbon fibers-Graphene is filled, it is characterised in that by following
The raw material of weight portion is obtained：
The glue 2-5 of magnesium oxide 5-8, boron nitride 8-13, PBT 10-25, EVA 5-10, glass fibre 4-10,107, tin dilaurate two
Butyl tin 1-2, tetraethyl orthosilicate 1-3, melamine cyanurate 3-7, Firebrake ZB 2-5, hypo-aluminum orthophosphate 2-6, bamboo charcoal 1-2, receives
Rice SiO2 2-3, dihydroxy dibutyl tin oxide 1-2, graphene oxide 2-5, carbon fiber 4-6, aluminium oxide 2-4,1- butyl -3- methyl
Limidazolium hexafluorophosphate 3-5, cumyl peroxide 0.1-0.5, KH550 1-2, ethanol, acetone, NaOH solution, distilled water are fitted
Amount.
2. the fire-retardant plastic of flexible high heat conductive insulating that a kind of LED carbon fibers according to claim 1-Graphene is filled
Preparation method, it is characterised in that carry out according to the following steps：
KH550 is mixed with ethanol, heating in water bath to 70-90 DEG C, add magnesium oxide and boron nitride, stir 10-30min, taken out
1-2h is stood, with suction pipe upper solution is sucked, dried after 1-2h in 75-95 DEG C, mixed with 107 glue, add tin dilaurate two
Butyl tin, tetraethyl orthosilicate, stir 1-2h；
B. add NaOH solution in melamine cyanurate, stir, add Firebrake ZB, 65-95 DEG C of reaction 1- of intensification
3h, obtains thick white product, and sucking filtration, washing 3-5 time are dried 1-3h in 115-165 DEG C；By hypo-aluminum orthophosphate, bamboo charcoal in 100-150
DEG C drying 1-2h after, mix with the former, superfine grinding obtains composite flame-retardant agent；
C. PBT is heated to into 150-170 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, mix homogeneously adds dihydroxy
Base dibutyl tin oxide, after polyreaction 1-2h, moves in ice-water bath and crushes, by gained sample in 105-130 DEG C of vacuum drying
2-4h；
D. resulting material in c is added graphene oxide into, supersonic vibration 2-3h adds carbon fiber and acetone, mix homogeneously to surpass
Sound oscillation 1-2h；
E. EVA, aluminium oxide and 1- butyl -3- Methylimidazole .s hexafluorophosphates are dried into 6- in 60-80 DEG C of vacuum drying oven
10h；Dried EVA and cumyl peroxide dynamic vulcanization 10-20min at 80 DEG C -150 DEG C is added after being dried
Aluminium oxide and 1- butyl -3- Methylimidazole. hexafluorophosphates, in 160-180 DEG C of melt blending 10-30min, discharging is stand-by；
F. resulting material in a, d, e and other surplus stocks are put in homogenizer and stir 1-2h, be placed in twin-screw extrusion
In machine, in 200-250 DEG C of melting extrusion, the cooling of Jing air, granulator granulation, 75-95 DEG C of drying 4-8h in baking oven is placed into, taken
Go out, Jing injection machines obtain a kind of flexible high heat conductive insulating of LED carbon fibers-Graphene filling in 235-255 DEG C of injection mo(u)lding
Fire-retardant plastic.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611224826.1A CN106589856A (en) | 2016-12-27 | 2016-12-27 | Carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for LED and preparation method of plastic |
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|---|---|---|---|
| CN201611224826.1A CN106589856A (en) | 2016-12-27 | 2016-12-27 | Carbon fiber-graphene filled flexible high thermal conductive insulating flame retardant plastic for LED and preparation method of plastic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110103891A (en) * | 2019-05-29 | 2019-08-09 | 河北科力汽车零部件有限公司 | A kind of windshield having from defrosting function |
| CN110655698A (en) * | 2019-11-05 | 2020-01-07 | 苏州鼎立工业胶辊有限公司 | High-thermal-conductivity composite rubber |
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| CN101555346A (en) * | 2009-05-25 | 2009-10-14 | 陈百良 | Nanometer polybutylene terephthalate (PBT) engineering plastic and fabrication method thereof |
| CN103618273A (en) * | 2013-10-10 | 2014-03-05 | 江苏江城电气有限公司 | Waterproof bus duct used in high temperature environment |
| CN105219036A (en) * | 2015-10-30 | 2016-01-06 | 安徽江淮汽车股份有限公司 | A kind of anti-flaming PBT composite and preparation method thereof |
| CN105985631A (en) * | 2015-02-02 | 2016-10-05 | 北京化工大学 | Heat-conducting composite material for LED (Light Emitting Diode) lamps and preparation method for heat-conducting composite material |
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2016
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| CN101555346A (en) * | 2009-05-25 | 2009-10-14 | 陈百良 | Nanometer polybutylene terephthalate (PBT) engineering plastic and fabrication method thereof |
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| CN105985631A (en) * | 2015-02-02 | 2016-10-05 | 北京化工大学 | Heat-conducting composite material for LED (Light Emitting Diode) lamps and preparation method for heat-conducting composite material |
| CN105219036A (en) * | 2015-10-30 | 2016-01-06 | 安徽江淮汽车股份有限公司 | A kind of anti-flaming PBT composite and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110103891A (en) * | 2019-05-29 | 2019-08-09 | 河北科力汽车零部件有限公司 | A kind of windshield having from defrosting function |
| CN110103891B (en) * | 2019-05-29 | 2022-07-22 | 河北科力汽车装备股份有限公司 | Front windshield with self-defogging function |
| CN110655698A (en) * | 2019-11-05 | 2020-01-07 | 苏州鼎立工业胶辊有限公司 | High-thermal-conductivity composite rubber |
| CN110655698B (en) * | 2019-11-05 | 2021-07-09 | 苏州鼎立工业胶辊有限公司 | High-thermal-conductivity composite rubber |
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Application publication date: 20170426 |