CN105542450A - Preparation method of electrically and thermally conductive nanocomposite material - Google Patents
Preparation method of electrically and thermally conductive nanocomposite material Download PDFInfo
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- CN105542450A CN105542450A CN201610080774.9A CN201610080774A CN105542450A CN 105542450 A CN105542450 A CN 105542450A CN 201610080774 A CN201610080774 A CN 201610080774A CN 105542450 A CN105542450 A CN 105542450A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K2201/001—Conductive additives
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- 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
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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
- C08L2205/02—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
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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
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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)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses an electrically and thermally conductive nanocomposite material and a preparation method thereof. The preparation method comprises the following steps: (1) mixing nylon 6, a nylon 6 masterbatch, a toughening agent, an antioxidant and lubricating agents uniformly in a stirrer and putting the mixture in a main feeding hole; (2) carrying out extrusion moulding by twin screws, thus obtaining the electrically and thermally conductive nanocomposite material. The composite material is environmentally friendly and accords with the ROHs (restriction of hazardous substances) of the EU (European union).
Description
Technical field
The present invention relates to a kind of conductive nano heat-conductive composite material and preparation method thereof.
Background technology
Plastics industry has been a Chaoyang industry since 20th century, is mainly applied range, easily repeatedly uses and accepted by the people.
Nylon is the general designation of polymeric amide, is the extrusion resin that in five large general engineering plastic, output is maximum, kind is maximum, most widely used, over-all properties is the most excellent.In polyamide resin, output and the consumption of nylon 6 and nylon66 fiber are maximum, account for about 90% of total polymeric amide, and nylon mainly has outstanding feature in mechanics, chemistry, thermal property etc.
In recent years, heat-conductivity conducting matrix material is developed gradually, but price is high, processing is more difficult, so adopt new material extremely urgent, along with the performance of Graphene manifests gradually, its heat-resisting conductivity is also by most material use, but due to the easy reunion of nano material, extrusion molding is difficult to demonstrate nano-meter characteristic in the material.
Summary of the invention
For solving the problem, the invention provides a kind of conductive nano heat-conductive composite material, comprising the raw material of following mass fraction:
Preferably, nylon 6 master batch is Graphene master batch.
Preferably, Graphene master batch is composed of the following components: nylon 69 5-98 part, Graphene 2-3 part.
Preferably, Graphene master batch is prepared by following methods: (1), joined by graphite in the solution of Strong oxdiative silane, heating, and be stirred to and evenly become liquid, stirring velocity can be 400-600RPM; (2), by solution by accelerating to 50-100m/s, wherein can be accelerated by high pressure; (3) high-speed liquid, obtained by step (2) enters high-speed ultrasonic vaporific pelletizing head-on collision equipment; (4) emulsion, by step 3 penetrated enters into the emulsion of hexanolactam, stirs, adds catalyzer, pressure synthesis and get final product.
Preferably, the present invention also can comprise coupling agent, specifically can be Aluminate and/or titanic acid ester.
Preferably, described oxidation inhibitor is hindered phenol antioxygen or phosphite antioxidant.
Preferably, described oxidation inhibitor is one or more the mixture in B215, B225 and B900.
In the present invention, Graphene manufacture in the following ways: 1, joined by graphite in the solution of Strong oxdiative silane, heating, high-speed stirring, to evenly becoming liquid; 2, solution is accelerated to 50-100m/s by high pressure; 3, the high-speed liquid obtained by step 2 enters high-speed ultrasonic vaporific pelletizing head-on collision equipment, produces gluey nano-solution.
In the present invention, Graphene master batch can be prepared by such as under type: in autoclave, 1, add caprolactam, catalyzer, above-mentioned gluey nano-solution; 2, heat, pressurize, stir, long chain polymer to be formed, extrudes formation particle.
Preferably, described toughner is one or more the mixture in ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene methyl methacrylate multipolymer and ethylene-methyl acrylate copolymer.
Described hindered phenol antioxygen can be in 1076,168,264 and 1010 one or more.
Described lubricant is one or more in EBS, Magnesium Stearate, calcium stearate, PE wax and silicone powder.
A preparation method for conductive nano heat-conductive composite material, comprises the steps: (1), mixing: by nylon 6, nylon 6 master batch, toughner, oxidation inhibitor, lubricant in stirrer for mixing evenly, put into main spout; (2), shaping by twin-screw extrusion.
Preferably, described twin screw is parallel double-screw.
Preferably, described twin screw length-to-diameter ratio is 48:1.
Preferably, described twin screw processing temperature is 215-245 DEG C.
Preferably, nylon 6 master batch is Graphene master batch.
The present invention also provides a kind of preparation method of Graphene master batch, comprises the following steps: (1), joined by graphite in the solution of Strong oxdiative silane, and heating, is stirred to and evenly becomes liquid; (2), solution is accelerated to 50-100m/s by high pressure; (3) high-speed liquid, obtained by step (2) enters high-speed ultrasonic vaporific pelletizing head-on collision equipment; (4) emulsion, by step 3 penetrated enters into the emulsion of hexanolactam, stirs, adds catalyzer, pressure synthesis and get final product.
Preferably, described catalyzer is basic catalyst.
Preferably, described basic catalyst is sodium hydroxide or sodium caprolactam(ate).
The invention has the beneficial effects as follows: matrix material prepared by the present invention has excellent performance.Solve the reunion of Graphene, give a kind of industrial production process of nano-graphene simultaneously.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1:
A kind of conductive nano heat-conductive composite material and preparation thereof, its table composed as follows of filling a prescription:
Table 1: the formula composition of a kind of conductive nano heat-conductive composite material and preparation thereof
Embodiment 2:
Table 2: the formula composition of a kind of conductive nano heat-conductive composite material and preparation thereof
Raw material | Mass parts |
PA6 | 85 |
Graphene master batch | 10 |
Ethylene-methyl acrylate copolymer | 5 |
Antioxidant 1010 | 0.1 |
Antioxidant 1076 | 0.1 |
Calcium stearate | 0.3 |
Comparative example 1:
Table 3: a kind of conductive nano heat-conductive composite material and preparation formula composition thereof
Raw material | Mass parts |
PA6 | 94 |
Graphene | 1 |
Ethylene-methyl acrylate copolymer | 5 |
Antioxidant 1010 | 0.1 |
Antioxidant 1076 | 0.1 |
Calcium stearate | 0.3 |
Comparative example 2:
Table 4: a kind of conductive nano heat-conductive composite material and preparation formula composition thereof
Shaping such as to utilize twin screw extruder to melt extrude shaping by routine techniques for the formula of embodiments of the invention, and the temperature melt extruded is 210-245 DEG C, screw speed: 380 ~ 420 turns/min, and screw slenderness ratio is 48:1.
The matrix material prepared by routine 1-4 carries out performance test, and the test result of gained sees the following form:
Table 5: the performance of embodiment gained matrix material
Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 | |
Tensile strength (Mpa) | 45 | 47 | 43 | 44 |
Notched Izod impact strength (kJ/ ㎡) | 6.5 | 6 | 4.8 | 4.3 |
Flexural strength (Mpa) | 90 | 96 | 86 | 89 |
Specific conductivity (S.CM -1) | 56 | 73 | 4 | 11 |
Thermal conductivity (W..M -1.K -1) | 4.1 | 5.6 | 1.2 | 1.6 |
Claims (8)
1. a preparation method for conductive nano heat-conductive composite material, is characterized in that: comprise the steps: (1), mixing: by nylon 6, nylon 6 master batch, toughner, oxidation inhibitor, lubricant in stirrer for mixing evenly, put into main spout; (2), shaping by twin-screw extrusion.
2. method according to claim 1, described twin screw is parallel double-screw.
3. method according to claim 1, is characterized in that: described twin screw length-to-diameter ratio is 48:1.
4. method according to claim 1, is characterized in that: described twin screw processing temperature is 215-245 DEG C.
5. the method according to any one of claim 1-4, is characterized in that, nylon 6 master batch is Graphene master batch.
6. a preparation method for Graphene master batch, comprises the following steps: (1), joined by graphite in the solution of Strong oxdiative silane, and heating, is stirred to and evenly becomes liquid; (2), solution is accelerated to 50-100m/s by high pressure; (3) high-speed liquid, obtained by step (2) enters high-speed ultrasonic vaporific pelletizing head-on collision equipment; (4) emulsion, by step 3 penetrated enters into the emulsion of hexanolactam, stirs, adds catalyzer, pressure synthesis and get final product.
7. method according to claim 6, is characterized in that: described catalyzer is basic catalyst.
8. method according to claim 7, described basic catalyst is sodium hydroxide or sodium caprolactam(ate).
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060293427A1 (en) * | 2005-06-10 | 2006-12-28 | Martens Marvin M | Thermally conductive polyamide-based components used in light emitting diode reflector applications |
CN101928457A (en) * | 2010-05-18 | 2010-12-29 | 赵明久 | Carbon-based nano cast nylon composite material and in-situ polymerization preparation method thereof |
CN102424705A (en) * | 2011-09-21 | 2012-04-25 | 中国科学技术大学 | Preparation method of polymer/graphene nano composite material |
CN103450674A (en) * | 2013-09-11 | 2013-12-18 | 上海大学 | Nylon 6/graphene nanometer composite material with high thermal conductivity and preparation method thereof |
CN105273399A (en) * | 2015-11-13 | 2016-01-27 | 厦门泰启力飞电子科技有限公司 | Polyamide/graphene high-thermal-conductivity nanocomposite material and preparing method thereof |
-
2016
- 2016-02-04 CN CN201610080774.9A patent/CN105542450A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060293427A1 (en) * | 2005-06-10 | 2006-12-28 | Martens Marvin M | Thermally conductive polyamide-based components used in light emitting diode reflector applications |
CN101928457A (en) * | 2010-05-18 | 2010-12-29 | 赵明久 | Carbon-based nano cast nylon composite material and in-situ polymerization preparation method thereof |
CN102424705A (en) * | 2011-09-21 | 2012-04-25 | 中国科学技术大学 | Preparation method of polymer/graphene nano composite material |
CN103450674A (en) * | 2013-09-11 | 2013-12-18 | 上海大学 | Nylon 6/graphene nanometer composite material with high thermal conductivity and preparation method thereof |
CN105273399A (en) * | 2015-11-13 | 2016-01-27 | 厦门泰启力飞电子科技有限公司 | Polyamide/graphene high-thermal-conductivity nanocomposite material and preparing method thereof |
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