CN106009648A - Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material - Google Patents

Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material Download PDF

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Publication number
CN106009648A
CN106009648A CN201610545438.7A CN201610545438A CN106009648A CN 106009648 A CN106009648 A CN 106009648A CN 201610545438 A CN201610545438 A CN 201610545438A CN 106009648 A CN106009648 A CN 106009648A
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China
Prior art keywords
parts
titanium dioxide
composite material
conductive composite
carbon fiber
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CN201610545438.7A
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Chinese (zh)
Inventor
肖宪书
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Bengbu Gaohua Resolution Technology Co Ltd
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Bengbu Gaohua Resolution Technology Co Ltd
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Priority to CN201610545438.7A priority Critical patent/CN106009648A/en
Publication of CN106009648A publication Critical patent/CN106009648A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a titanium dioxide-polyamide thermal conductive composite material for LED lamps. The composite material is prepared from, by weight, 6-200 parts of polyamide, 40-50 parts of polyamide 66, 20-30 parts of rutile type titanium dioxide, 20-30 parts of carbon fibers, 50-60 parts of acetone, 80-100 parts of 60%-70% nitric acid, 3-4 parts of nonylphenol polyoxyethylene ether, 3-4 parts of lauric acid, 15-20 parts of methylbenzene-2,4-diisocyanate, 20-25 parts of 2-hydroxypropyl methacrylate, 0.4-1 part of catalyst, 0.4-2 parts of polymerization inhibitor, 3-5 parts of ethoxyquin, 3-4 parts of disodium stannous citrate, 150-170 parts of tetrahydrofuran, 80-100 parts of methylbenzene and an appropriate amount of deionized water. The polyamide thermal conductive composite material is compact in structure, rapid in heat transfer and heat dissipation, good in mechanical property, durable in use and capable of effectively protecting high-strength LED lamps and greatly prolonging the service life of the lamps.

Description

A kind of LED titanium dioxide-nylon heat-conductive composite material and preparation method thereof
Technical field
The present invention relates to a kind of nylon guide hot material and preparation method thereof, be specifically related to a kind of LED titanium dioxide-nylon Heat-conductive composite material.
Background technology
In general, the heat conductivity of pure plastic material is far away not as good as metal, ceramic material, but its insulating properties Good.Heat-conducting plastic not only has metal and the heat transfer performance of pottery, also retains common plastics simultaneously and in design, performance and becomes The advantage of present aspect, has the selection of base resin uniform, lightweight, multiple of dispelling the heat, processing and forming convenience, thermal coefficient of expansion Low, molding shrinkage is low, operating temperature is low and improve design freedom feature, be widely used in all trades and professions.
At present, the most typical application of heat-conducting plastic is at lighting field, is mainly used in making the LED joint needing to dispel the heat good The Lamp cup etc. of energy lamp, although the heat that LED electricity-saving lamp is consumed is more much smaller than ordinary light source, but because LED energy-saving lamp structure Compact, powerful, the most effectively dispel the heat and remain an important problem.
Chinese patent application CN102408710A discloses a kind of high heat conduction nylon 66 composite material, and its base material all uses Nylon66 fiber, hardness is high, and after adding heat filling, material tensile property, bending property are deteriorated, and only add coupling agent in its formula And antioxidant so that the poor processability of whole system, breakage phenomena can be produced in producing extrusion, it is impossible to be applicable to work Industry continuous prodution.
Summary of the invention
It is an object of the invention to provide a kind of LED titanium dioxide-nylon heat-conductive composite material and preparation method thereof.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described heat-conductive composite material is by following heavy The raw material of amount part is made: nylon 6 200 parts, nylon66 fiber 40-50 part, Rutile type titanium dioxide 20-30 part, carbon fiber 20-30 Part, acetone 50-60 part, 60-70% nitric acid 80-100 part, NPE 3-4 part, lauric acid 3-4 part, Toluene-2,4-diisocyanate, 4- Diisocyanate 15-20 part, (methyl) Hydroxypropyl acrylate 20-25 part, catalyst 0.4-1 part, polymerization inhibitor 0.4-2 part, ethoxy Base quinoline 3-5 part, distannous citrate 3-4 part, oxolane 150-170 part, toluene 80-100 part, deionized water are appropriate.
A kind of LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described heat-conductive composite material is by such as Lower step prepares:
(1) surface modification of carbon fiber
Carbon fiber is placed in acetone soln immersion 10-12h, filters, deionized water wash 2-3 time, 100-120 DEG C of forced air drying Machine is dried 3-4h;With 60-70% nitric acid reflux oxidation carbon fiber 5-7h, filtering, deionized water wash to PH is 6-7, in 100- 120 DEG C of blast driers are dried to constant weight;The carbon fiber of nitric acid oxidation is placed in NPE, lauric acid and phase When, in the solution in the deionized water configuration of 10-12 times of its total weight parts, ultrasonic 40-50min, 50-60 DEG C is dried, obtains table The carbon fiber that face is modified;
(2) preparation of high polymer cladding titanium dioxide
Rutile type titanium dioxide is ground screening, and ultrasonic disperse, in oxolane and toluene, adds Toluene-2,4-diisocyanate, 4-bis-isocyanide Acid esters, catalyst, polymerization inhibitor mix homogeneously;At 30-40 DEG C, it is slowly added dropwise (methyl) Hydroxypropyl acrylate;Rise high-temperature extremely 50-60 DEG C, react 5-8h, obtain high polymer cladding titanium dioxide;
(3) preparation of titanium dioxide-nylon heat-conductive composite material
Nylon 6 is placed in the blast drier of 80-85 DEG C together with nylon66 fiber and is dried 8-10h, with the carbon fiber of surface modification, High polymer cladding titanium dioxide, ethoxy quinoline, distannous citrate add high mixer high speed stirring 40-50min together, treat It is added into after mix homogeneously double screw extruder melt extrudes, tie rod cooling granulation.
A kind of LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described catalyst can be selected from February One or more in dilaurylate, dibutyitin maleate, butyl maleate dibutyl tin, stannous octoate compound.
A kind of LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described polymerization inhibitor can be selected to hydroxyl Base methyl phenyl ethers anisole, hydroquinone, one or more in 2,6 ditertiary butyl p cresol compound.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention uses high nylon 6 heat-resist, elastic to compound as base with endurance, hardness nylon66 fiber high, anti abrasive Body material;Use and there is the coefficient of friction titanium dioxide that very low and high temperature stability is fine, intensity is high, heat conductivity is high, and utilize titanium White lead and the synergism of carbon fiber, improve the heat conductivility of nylon heat-conductive composite material;Carbon fiber is carried out surface modification, It is coated with titanium dioxide so that carbon fiber and titanium dioxide are uniformly dispersed in matrix material, carbon fiber and titanium dioxide and Buddhist nun with high polymer Interfacial interaction power between dragon matrix is strong, is conducive to the heat conduction in interface, reduces interface resistance, and the most also utilizing should Power is in the transmission of interface, and stronger interface interaction significantly improves the mechanical property of nylon heat-conductive composite material with thermally-stabilised Property.
Detailed description of the invention
The LED of the present embodiment titanium dioxide-nylon heat-conductive composite material, described heat-conductive composite material is by following weight Part raw material make: nylon 6 200 parts, nylon66 fiber 40 parts, Rutile type titanium dioxide 20 parts, 20 parts of carbon fiber, 60 parts of acetone, 60% 100 parts of nitric acid, NPE 4 parts, lauric acid 3 parts, Toluene-2,4-diisocyanate, 4-diisocyanate 15 parts, (methyl) propylene Acid hydroxypropyl acrylate 20 parts, catalyst 0.5 part, polymerization inhibitor 2 parts, ethoxy quinoline 5 parts, distannous citrate 4 parts, oxolane 170 parts, toluene 100 parts, deionized water appropriate.
The LED of the present embodiment titanium dioxide-nylon heat-conductive composite material, described heat-conductive composite material is by following steps Prepare:
(1) surface modification of carbon fiber
Carbon fiber is placed in acetone soln immersion 12h, filters, deionized water wash 3 times, 120 DEG C of blast driers are dried 4h;With 60% nitric acid reflux oxidation carbon fiber 7h, filtering, deionized water wash to PH is 6, is dried in 120 DEG C of blast driers To constant weight;The carbon fiber of nitric acid oxidation is placed in NPE, lauric acid and is equivalent to 10 times of its total weight parts Deionized water configuration solution in, ultrasonic 50min, 60 DEG C be dried, obtain the carbon fiber of surface modification;
(2) preparation of high polymer cladding titanium dioxide
Rutile type titanium dioxide is ground screening, and ultrasonic disperse, in oxolane and toluene, adds Toluene-2,4-diisocyanate, 4-bis-isocyanide Acid esters, catalyst, polymerization inhibitor mix homogeneously;At 30 DEG C, it is slowly added dropwise (methyl) Hydroxypropyl acrylate;Rise high-temperature to 50 DEG C, react 8h, obtain high polymer cladding titanium dioxide;
(3) preparation of titanium dioxide-nylon heat-conductive composite material
Nylon 6 is placed in the blast drier of 85 DEG C together with nylon66 fiber and is dried 10h, with carbon fiber, the Gao Ju of surface modification Thing cladding titanium dioxide, ethoxy quinoline, distannous citrate add together high mixer high speed stirring 50min, to be mixed all It is added into after even double screw extruder melt extrudes, tie rod cooling granulation.
After tested, the LED of present invention titanium dioxide-nylon heat conduction thermal conductivity of composite materials is more than 3W/(m*K), inhale Water rate (23 DEG C, 24h) is less than 0.10%, and hot strength is more than 40MPa, and bending strength is more than 60MPa.

Claims (4)

1. LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described heat-conductive composite material is by following The raw material of weight portion is made: nylon 6 200 parts, nylon66 fiber 40-50 part, Rutile type titanium dioxide 20-30 part, carbon fiber 20-30 Part, acetone 50-60 part, 60-70% nitric acid 80-100 part, NPE 3-4 part, lauric acid 3-4 part, Toluene-2,4-diisocyanate, 4- Diisocyanate 15-20 part, (methyl) Hydroxypropyl acrylate 20-25 part, catalyst 0.4-1 part, polymerization inhibitor 0.4-2 part, ethoxy Base quinoline 3-5 part, distannous citrate 3-4 part, oxolane 150-170 part, toluene 80-100 part, deionized water are appropriate.
2. LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described heat-conductive composite material is by as follows Step prepares:
(1) surface modification of carbon fiber
Carbon fiber is placed in acetone soln immersion 10-12h, filters, deionized water wash 2-3 time, 100-120 DEG C of forced air drying Machine is dried 3-4h;With 60-70% nitric acid reflux oxidation carbon fiber 5-7h, filtering, deionized water wash to PH is 6-7, in 100- 120 DEG C of blast driers are dried to constant weight;The carbon fiber of nitric acid oxidation is placed in NPE, lauric acid and phase When, in the solution in the deionized water configuration of 10-12 times of its total weight parts, ultrasonic 40-50min, 50-60 DEG C is dried, obtains table The carbon fiber that face is modified;
(2) preparation of high polymer cladding titanium dioxide
Rutile type titanium dioxide is ground screening, and ultrasonic disperse, in oxolane and toluene, adds Toluene-2,4-diisocyanate, 4-bis-isocyanide Acid esters, catalyst, polymerization inhibitor mix homogeneously;At 30-40 DEG C, it is slowly added dropwise (methyl) Hydroxypropyl acrylate;Rise high-temperature extremely 50-60 DEG C, react 5-8h, obtain high polymer cladding titanium dioxide;
(3) preparation of titanium dioxide-nylon heat-conductive composite material
Nylon 6 is placed in the blast drier of 80-85 DEG C together with nylon66 fiber and is dried 8-10h, with the carbon fiber of surface modification, High polymer cladding titanium dioxide, ethoxy quinoline, distannous citrate add high mixer high speed stirring 40-50min together, treat It is added into after mix homogeneously double screw extruder melt extrudes, tie rod cooling granulation.
3. LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described catalyst can be selected from two Laurels One or more in acid dibutyl tin, dibutyitin maleate, butyl maleate dibutyl tin, stannous octoate compound.
4. LED titanium dioxide-nylon heat-conductive composite material, it is characterised in that described polymerization inhibitor can be selected to hydroxyl Methyl phenyl ethers anisole, hydroquinone, one or more in 2,6 ditertiary butyl p cresol compound.
CN201610545438.7A 2016-07-12 2016-07-12 Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material Pending CN106009648A (en)

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CN201610545438.7A CN106009648A (en) 2016-07-12 2016-07-12 Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610545438.7A CN106009648A (en) 2016-07-12 2016-07-12 Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104559145A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 High-toughness and high-thermal-conductivity polymer material and preparation method thereof
CN105348867A (en) * 2015-12-16 2016-02-24 江南大学 Modification method of nano aluminium oxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104559145A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 High-toughness and high-thermal-conductivity polymer material and preparation method thereof
CN105348867A (en) * 2015-12-16 2016-02-24 江南大学 Modification method of nano aluminium oxide

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Application publication date: 20161012