CN106751583A - A kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe and preparation method thereof - Google Patents
A kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe and preparation method thereof Download PDFInfo
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- CN106751583A CN106751583A CN201611225923.2A CN201611225923A CN106751583A CN 106751583 A CN106751583 A CN 106751583A CN 201611225923 A CN201611225923 A CN 201611225923A CN 106751583 A CN106751583 A CN 106751583A
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- cdte
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- iridescent
- adjustable
- heat conduction
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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
- 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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- 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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- 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
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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
- 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
- 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
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Abstract
The invention discloses a kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe, 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, LiOH, urea, CdTe, mercaptopropionic acid, cellulose 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 fire-retardant plastic of high heat conduction of LED celluloses adjustable iridescent of CdTe.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of LED high heat conductions of the adjustable iridescent of cellulose-CdTe
Fire-retardant plastic, 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；In the presence of LiOH/ urea, during low temperature, by cellulose dissolution in partly leading
In the mercaptopropionic acid of body nano-particle CdTe, compound is formed, at room temperature after short time placement, formd fluorescence volume high
Sub- efficiency, adjustable fluorescence color, the composite of high stability, in can be applicable to the encapsulating material of LED；A kind of LED is obtained to use
The fire-retardant plastic of high heat conduction of iridescent that cellulose-CdTe is adjustable.
The content of the invention
The present invention solves the technical problem of providing a kind of LED high heat conduction of the adjustable iridescent of cellulose-CdTe
Fire-retardant plastic and its preparation technology, according to the technique make thermal conductivity of composite materials is high, fire resistance is good, can be preferably
Improve the radiating of LED.
The technical problems to be solved by the invention are realized using following technical scheme：
Magnesia 6-10, boron nitride 8-14, PBT 15-25, EVA 5-10, glass fibre 4-10,107 glue 2-3, tin dilaurate two
Butyl tin 1-2, tetraethyl orthosilicate 1-2, melamine cyanurate 3-5, Firebrake ZB 2-3, hypo-aluminum orthophosphate 2-4, bamboo charcoal 1-2, receive
Rice SiO2 2-3, dihydroxy dibutyl tin oxide 1-3, graphene oxide 2-4, carbon fiber 4-7, KH550 1-2, LiOH 2-3, urea
1-2, CdTe 3-5, mercaptopropionic acid 1-2, cellulose 2-4, ethanol, acetone, NaOH solution, distillation appropriate amount of water.
A kind of LED preparation methods of the fire-retardant plastic of high heat conduction of the adjustable iridescent of cellulose-CdTe, its feature exists
In carrying 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. LiOH and urea are dissolved in the mercaptopropionic acid of semi-conductor nano particles CdTe, in -20~-12 DEG C of additions
Cellulose, is sufficiently stirred for 1-3h, obtains semi-conductor nano particles complex solution；
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, the high heat conduction for obtaining a kind of LED celluloses adjustable iridescent of-CdTe is fire-retardant
Plastic.
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）In the presence of LiOH/ urea, during low temperature, by cellulose dissolution in the sulfydryl of semi-conductor nano particles CdTe
In propionic acid solution, formed compound, at room temperature the short time place after, formd fluorescence quantum efficiency high, adjustable fluorescence color,
The composite of high stability, in can be applicable to the encapsulating material of LED.
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 fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose-CdTe, by the original of following weight parts (g)
Material is obtained：
Magnesia 10, boron nitride 14, PBT 25, EVA 10, the glue 2 of glass fibre 10,107, dibutyl tin laurate 1, positive silicon
Acetoacetic ester 1, melamine cyanurate 3, Firebrake ZB 2, hypo-aluminum orthophosphate 4, bamboo charcoal 1, Nano-meter SiO_22 3, dihydroxy dibutyl tin oxide
1, graphene oxide 4, carbon fiber 7, KH550 1, LiOH 2, urea 2, CdTe 5, mercaptopropionic acid 1, cellulose 4, ethanol, third
Ketone, NaOH solution, distillation appropriate amount of water.
A kind of LED preparation methods of the fire-retardant plastic of high heat conduction of the adjustable iridescent of cellulose-CdTe, its feature exists
In carrying 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. LiOH and urea are dissolved in the mercaptopropionic acid of semi-conductor nano particles CdTe, in -15~-10 DEG C of additions
Cellulose, is sufficiently stirred for 2h, obtains semi-conductor nano particles complex solution；
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, a kind of high heat conduction flame retardant type of LED celluloses adjustable iridescent of-CdTe is obtained
Plastics.
A kind of LED prepared by above-described embodiment is examined with the performance of the fire-retardant plastic of high heat conduction of the adjustable iridescent of cellulose-CdTe
Survey result as follows：
Thermal conductivity factor is 319.62W/m K, and thermal coefficient of expansion is 12.84 × 10-6·K-1(50-150 DEG C), tensile strength is
59.79MPa, bending strength is 45.63MPa, and impact strength is 3.92KJ/m2, elongation at break is up to 13.75%.
Claims (2)
1. a kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose-CdTe, it is characterised in that by following weight
The raw material of part is obtained：
Magnesia 6-10, boron nitride 8-14, PBT 15-25, EVA 5-10, glass fibre 4-10,107 glue 2-3, tin dilaurate two
Butyl tin 1-2, tetraethyl orthosilicate 1-2, melamine cyanurate 3-5, Firebrake ZB 2-3, hypo-aluminum orthophosphate 2-4, bamboo charcoal 1-2, receive
Rice SiO2 2-3, dihydroxy dibutyl tin oxide 1-3, graphene oxide 2-4, carbon fiber 4-7, KH550 1-2, LiOH 2-3, urea
1-2, CdTe 3-5, mercaptopropionic acid 1-2, cellulose 2-4, ethanol, acetone, NaOH solution, distillation appropriate amount of water.
2. a kind of LED according to claim 1 systems of the fire-retardant plastic of high heat conduction of the adjustable iridescent of cellulose-CdTe
Preparation Method, it is characterised in that carry out according to the following steps：
KH550 is mixed with ethanol, heating water bath adds magnesia and boron nitride to 70-90 DEG C, stirs 10-30min, takes out
1-2h is stood, upper solution is sucked with suction pipe, after drying 1-2h in 75-95 DEG C, mixed with 107 glue, add tin dilaurate two
Butyl 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. LiOH and urea are dissolved in the mercaptopropionic acid of semi-conductor nano particles CdTe, in -20~-12 DEG C of additions
Cellulose, is sufficiently stirred for 1-3h, obtains semi-conductor nano particles complex solution；
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, the high heat conduction for obtaining a kind of LED celluloses adjustable iridescent of-CdTe is fire-retardant
Plastic.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611225923.2A CN106751583A (en) | 2016-12-27 | 2016-12-27 | A kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611225923.2A CN106751583A (en) | 2016-12-27 | 2016-12-27 | A kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe and preparation method thereof |
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| CN106751583A true CN106751583A (en) | 2017-05-31 |
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|---|---|---|---|
| CN201611225923.2A Pending CN106751583A (en) | 2016-12-27 | 2016-12-27 | A kind of LED fire-retardant plastics of high heat conduction of the adjustable iridescent of cellulose CdTe and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341985A (en) * | 2013-05-21 | 2013-10-09 | 哈尔滨工程大学 | Vacuum-assisted resin diffusion molding method for fiber-reinforced PBT composite material |
| CN104449738A (en) * | 2014-10-23 | 2015-03-25 | 吉林大学 | Cellulose and semiconductor nanoparticle compound, and preparation method and application in LED (Light-emitting Diode) package |
| CN105219040A (en) * | 2015-11-18 | 2016-01-06 | 南通开普乐工程塑料有限公司 | A kind of halogen free flame-retardant reinforced PBT composite material |
| CN105295317A (en) * | 2015-11-18 | 2016-02-03 | 东莞市万江明冠实业有限公司 | High-temperature resistance and low-temperature resistance PBT heat conduction and heat dissipating material, preparation method and applications 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 |
-
2016
- 2016-12-27 CN CN201611225923.2A patent/CN106751583A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341985A (en) * | 2013-05-21 | 2013-10-09 | 哈尔滨工程大学 | Vacuum-assisted resin diffusion molding method for fiber-reinforced PBT composite material |
| CN104449738A (en) * | 2014-10-23 | 2015-03-25 | 吉林大学 | Cellulose and semiconductor nanoparticle compound, and preparation method and application in LED (Light-emitting Diode) package |
| 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 |
| CN105219040A (en) * | 2015-11-18 | 2016-01-06 | 南通开普乐工程塑料有限公司 | A kind of halogen free flame-retardant reinforced PBT composite material |
| CN105295317A (en) * | 2015-11-18 | 2016-02-03 | 东莞市万江明冠实业有限公司 | High-temperature resistance and low-temperature resistance PBT heat conduction and heat dissipating material, preparation method and applications thereof |
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Application publication date: 20170531 |