CN106751581A - A kind of LED copper powder compounded fire-retardant plastics of high heat conduction of the bortz powder that carbon fiber and graphite alkene is filled and preparation method thereof - Google Patents
A kind of LED copper powder compounded fire-retardant plastics of high heat conduction of the bortz powder that carbon fiber and graphite alkene is filled and preparation method thereof Download PDFInfo
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- CN106751581A CN106751581A CN201611224822.3A CN201611224822A CN106751581A CN 106751581 A CN106751581 A CN 106751581A CN 201611224822 A CN201611224822 A CN 201611224822A CN 106751581 A CN106751581 A CN 106751581A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of LED copper powder compounded fire-retardant plastics of high heat conduction of the bortz powder that carbon fiber and graphite alkene is filled, and its preparation technology, characterized in that, with magnesia, boron nitride, PBT, EVA, glass fibre, 107 glue, dibutyl tin laurate, tetraethyl orthosilicate, melamine cyanurate, Firebrake ZB, hypo-aluminum orthophosphate, bamboo charcoal, Nano-meter SiO_22, dihydroxy dibutyl tin oxide, graphene oxide, carbon fiber, bortz powder, copper powder, crome metal etc. be raw material.The present invention is prepared for the heat-conducting silicon rubber of KH550 surface treatments；With dihydroxy dibutyl tin oxide as catalyst, Nano-meter SiO_2 is used2To polybutylene terephthalate (PBT)（PBT）Carry out activeness and quietness treatment；Composite flame-retardant agent is prepared for using hypo-aluminum orthophosphate, melamine cyanurate；Obtain a kind of copper powder compounded fire-retardant plastic of high heat conduction of the bortz powder of LED carbon fiber and graphites alkene filling.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of bortz powder of LED carbon fibers-Graphene filling-
The fire-retardant plastic of copper powder compounded high heat conduction, and its preparation technology.
Background technology
LED has the advantages that small volume, long lifespan, low-carbon environment-friendly, energy-conservation stabilization as a kind of excellent photoelectric device,
Being expected in following several years will be as preferably general illumination light source of new generation.As LED develops to light intensity high, 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 magnesia and boron nitride as heat filling, adds ethylene-vinyl acetate copolymer (EVA) and glass fibre to enter it
The treatment of row activeness and quietness, heat-conductive composite material is prepared for using double screw extruder, improves the thermal 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 magnesia, 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 silicon rubber；With dihydroxy butyl chloride
Change tin is catalyst, uses Nano-meter SiO_22To polybutylene terephthalate (PBT)（PBT）Carry out activeness and quietness treatment；Hypo-aluminum orthophosphate
(AHP) phosphorus content is high, 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；Using the ductility of copper product, copper is filled in the space of diamond particles
In, the heat conductivity being made is high, the rough surface of composite, increases the contact area with air, strengthens convection current
Heat radiation, is conducive to being used as the heat abstractor of LED illumination；Obtain a kind of bortz powder of LED carbon fibers-Graphene filling-
The fire-retardant plastic of copper powder compounded high heat conduction.
The content of the invention
The present invention solves the technical problem of the bortz powder-copper for providing a kind of LED carbon fibers-Graphene filling
The compound fire-retardant plastic of high heat conduction of powder and its preparation technology, the thermal conductivity of composite materials made according to the technique are high, fire-retardant
Performance is good, can preferably improve the radiating of LED.
The technical problems to be solved by the invention are realized using following technical scheme：
Magnesia 7-10, boron nitride 8-13, PBT 10-23, EVA 5-9, glass fibre 4-7,107 glue 2-3, the fourth of tin dilaurate two
Base tin 1-3, tetraethyl orthosilicate 2-3, melamine cyanurate 3-5, Firebrake ZB 2-5, hypo-aluminum orthophosphate 2-3, bamboo charcoal 1-3, nanometer
SiO2 2-5, dihydroxy dibutyl tin oxide 1-2, graphene oxide 2-6, carbon fiber 4-9, KH550 1-2, bortz powder 2-4, copper
Powder 1-3, crome metal 1-2, ethanol, acetone, NaOH solution, distillation appropriate amount of water.
A kind of preparation of the fire-retardant plastic of high heat conduction of the bortz powder of LED carbon fibers-Graphene filling-copper powder compounded
Method, it is characterised in that carry out according to the following steps：
A. KH550 is mixed with ethanol, heating water bath adds magnesia and boron nitride to 70-90 DEG C, stirs 10-30min, takes
Go out to stand 1-2h, upper solution is sucked with suction pipe, after drying 1-2h in 75-95 DEG C, mix with 107 glue, add tin dilaurate
Dibutyl tin, tetraethyl orthosilicate, stir 1-2h；
B. to NaOH solution is added in melamine cyanurate, stir, add Firebrake ZB, 65-95 DEG C of reaction 1- of intensification
3h, obtains thick white product, and suction filtration, washing 3-5 times dry 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, ultra-fine grinding obtains composite flame-retardant agent；
C. PBT is heated to 150-170 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, is well mixed, and adds two
Hydroxybutyl stannic chloride, after polymerisation 1-2h, move into ice-water bath in and crush, gained sample is done in 105-130 DEG C of vacuum
Dry 2-4h；
D. resulting material in c is added graphene oxide into, ultrasonic vibration 2-3h adds carbon fiber and acetone, is well mixed, surpasses
Sound oscillation 1-2h；
E. bortz powder and copper powder are mixed, with the method for magnetron sputtering in its surface metallization chromium, is then placed in mould
In, be placed in plasma vacuum high pressure combustion freezing of a furnace, 10-30min be warmed up to 1000-1100 DEG C, pressure 20-40MPa, sintering
20-40min；Do hip treatment after sintering in 150-200MPa, 1000-1050 DEG C under argon atmosphere, be incubated 2-4h, obtain
Bortz powder-copper powder compounded material；
F. resulting material in a, d, e and other surplus stocks are put into homogenizer and stir 1-2h, be placed in twin-screw extrusion
In machine, in 200-250 DEG C of melting extrusion, cooled down through air, granulator granulation, place into 75-95 DEG C of drying 4-8h in baking oven, taken
Go out, through injection machine in 235-255 DEG C of injection moulding, obtain a kind of bortz powder-copper powder of LED carbon fibers-Graphene filling
The fire-retardant plastic of compound high heat conduction.
Reaction mechanism of the invention is as follows：
（1）With magnesia, 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 silicon rubber is improve.
（2）Hypo-aluminum orthophosphate (AHP) has the advantages that phosphorus content is high, good flame retardation effect, and the addition of synergist bamboo charcoal can promote
AHP is degraded and 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 the anti-flammability for inside polymeric matrix, being conducive to improving 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 smaller
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 radius-thickness ratio high, 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）Using the ductility of copper product, copper is filled in the space of diamond particles, the composite thermal conductivity being made
Rate is high, the rough surface of composite, increases the contact area with air, strengthens convection current heat radiation, is conducive to being used as LED photographs
Bright heat abstractor.
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 high heat conduction of the bortz powder of a kind of LED carbon fibers-Graphene filling-copper powder compounded, under
The raw material for stating weight portion (g) is obtained：
Magnesia 10, boron nitride 13, PBT 123, EVA 9, the glue 2 of glass fibre 7,107, dibutyl tin laurate 1, positive silicic acid
Ethyl ester 2, melamine cyanurate 3, Firebrake ZB 2, hypo-aluminum orthophosphate 3, bamboo charcoal 1, Nano-meter SiO_22 5, dihydroxy dibutyl tin oxide 1,
Graphene oxide 6, carbon fiber 9, KH550 1, bortz powder 4, copper powder 3, crome metal 2, ethanol, acetone, NaOH solution, distilled water
In right amount.
A kind of preparation of the fire-retardant plastic of high heat conduction of the bortz powder of LED carbon fibers-Graphene filling-copper powder compounded
Method, it is characterised in that carry out according to the following steps：
A. KH550 is mixed with ethanol, heating water bath adds magnesia and boron nitride to 80-90 DEG C, stirs 30min, takes out
1h is stood, upper solution is sucked with suction pipe, after drying 1h in 85-95 DEG C, mixed with 107 glue, add di lauric dibutyl
Tin, tetraethyl orthosilicate, stir 1h；
B. to NaOH solution is added in melamine cyanurate, stir, add Firebrake ZB, 1h is reacted in 85-95 DEG C of intensification,
Thick white product is obtained, suction filtration, washing 3 times dry 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, ultra-fine grinding obtains composite flame-retardant agent；
C. PBT is heated to 150-160 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, is well mixed, and adds two
Hydroxybutyl stannic chloride, after polymerisation 2h, move into ice-water bath in and crush, by gained sample in 120-130 DEG C vacuum drying
2h；
D. resulting material in c is added graphene oxide into, ultrasonic vibration 2h adds carbon fiber and acetone, is well mixed, ultrasound
Vibration 1h；
E. bortz powder and copper powder are mixed, with the method for magnetron sputtering in its surface metallization chromium, is then placed in mould
In, be placed in plasma vacuum high pressure combustion freezing of a furnace, 120min be warmed up to 1000-1100 DEG C, pressure 30-40MPa, sintering
30-40min；Do hip treatment after sintering in 150-200MPa, 1000-1050 DEG C under argon atmosphere, be incubated 2h, obtain golden
Emery-copper powder compounded material；
F. resulting material in a, d, e and other surplus stocks are put into homogenizer and stir 1h, be placed in double screw extruder
In, in 230-250 DEG C of melting extrusion, cooled down through air, granulator granulation, 85-95 DEG C of drying 4h in baking oven is placed into, take out,
Through injection machine in 245-255 DEG C of injection moulding, the bortz powder of a kind of LED carbon fibers-Graphene filling-copper powder compounded is obtained
The fire-retardant plastic of high heat conduction.
A kind of high heat conduction of the bortz powder of LED carbon fibers-Graphene filling prepared by above-described embodiment-copper powder compounded is fire-retardant
The performance test results of plastic are as follows：
Thermal conductivity factor is 315.63W/m K, and thermal coefficient of expansion is 14.21 × 10-6·K-1(50-150 DEG C), tensile strength is
60.72MPa, bending strength is 45.94MPa, and impact strength is 3.39KJ/m2, elongation at break is up to 13.95%.
Claims (2)
1. a kind of fire-retardant plastic of high heat conduction of the bortz powder of LED carbon fibers-Graphene filling-copper powder compounded, its feature
It is to be obtained by the raw material of following weight parts：
Magnesia 7-10, boron nitride 8-13, PBT 10-23, EVA 5-9, glass fibre 4-7,107 glue 2-3, the fourth of tin dilaurate two
Base tin 1-3, tetraethyl orthosilicate 2-3, melamine cyanurate 3-5, Firebrake ZB 2-5, hypo-aluminum orthophosphate 2-3, bamboo charcoal 1-3, nanometer
SiO2 2-5, dihydroxy dibutyl tin oxide 1-2, graphene oxide 2-6, carbon fiber 4-9, KH550 1-2, bortz powder 2-4, copper
Powder 1-3, crome metal 1-2, ethanol, acetone, NaOH solution, distillation appropriate amount of water.
2. a kind of bortz powder-copper powder compounded height of LED carbon fibers according to claim 1-Graphene filling is led
Thermal resistance fires the preparation method of plastic, it is characterised in that carry out according to the following steps：
A. KH550 is mixed with ethanol, heating water bath adds magnesia and boron nitride to 70-90 DEG C, stirs 10-30min, takes
Go out to stand 1-2h, upper solution is sucked with suction pipe, after drying 1-2h in 75-95 DEG C, mix with 107 glue, add tin dilaurate
Dibutyl tin, tetraethyl orthosilicate, stir 1-2h；
B. to NaOH solution is added in melamine cyanurate, stir, add Firebrake ZB, 65-95 DEG C of reaction 1- of intensification
3h, obtains thick white product, and suction filtration, washing 3-5 times dry 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, ultra-fine grinding obtains composite flame-retardant agent；
C. PBT is heated to 150-170 DEG C, Nano-meter SiO_22, resulting material is added thereto in b, is well mixed, and adds dihydroxy
Base dibutyl tin oxide, after polymerisation 1-2h, move into ice-water bath in and crush, by gained sample in 105-130 DEG C vacuum drying
2-4h；
D. resulting material in c is added graphene oxide into, ultrasonic vibration 2-3h adds carbon fiber and acetone, is well mixed, surpasses
Sound oscillation 1-2h；
E. bortz powder and copper powder are mixed, with the method for magnetron sputtering in its surface metallization chromium, is then placed in mould
In, be placed in plasma vacuum high pressure combustion freezing of a furnace, 10-30min be warmed up to 1000-1100 DEG C, pressure 20-40MPa, sintering
20-40min；Do hip treatment after sintering in 150-200MPa, 1000-1050 DEG C under argon atmosphere, be incubated 2-4h, obtain
Bortz powder-copper powder compounded material；
F. resulting material in a, d, e and other surplus stocks are put into homogenizer and stir 1-2h, be placed in twin-screw extrusion
In machine, in 200-250 DEG C of melting extrusion, cooled down through air, granulator granulation, place into 75-95 DEG C of drying 4-8h in baking oven, taken
Go out, through injection machine in 235-255 DEG C of injection moulding, obtain a kind of bortz powder-copper powder of LED carbon fibers-Graphene filling
The fire-retardant plastic of compound high heat conduction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611224822.3A CN106751581A (en) | 2016-12-27 | 2016-12-27 | A kind of LED copper powder compounded fire-retardant plastics of high heat conduction of the bortz powder that carbon fiber and graphite alkene is filled and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611224822.3A CN106751581A (en) | 2016-12-27 | 2016-12-27 | A kind of LED copper powder compounded fire-retardant plastics of high heat conduction of the bortz powder that carbon fiber and graphite alkene is filled and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111057379A (en) * | 2019-12-26 | 2020-04-24 | 华南理工大学 | High-thermal-conductivity insulating silicone rubber composite material containing carbon fibers and preparation method thereof |
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Application publication date: 20170531 |