CN110551391A - Method for preparing nylon 6-based heat dissipation composite material through reactive extrusion - Google Patents
Method for preparing nylon 6-based heat dissipation composite material through reactive extrusion Download PDFInfo
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- CN110551391A CN110551391A CN201911019171.8A CN201911019171A CN110551391A CN 110551391 A CN110551391 A CN 110551391A CN 201911019171 A CN201911019171 A CN 201911019171A CN 110551391 A CN110551391 A CN 110551391A
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- 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
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
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Abstract
a method for preparing a nylon 6-based heat dissipation composite material through reactive extrusion comprises the steps of adding a caprolactam monomer, a ring-opening catalyst caprolactam sodium salt, a cocatalyst HDI hexamethylene isocyanate and oligo-layer graphene with a thickness of 2-10 carbon layers into a reaction kettle, pre-dispersing under the action of ultrasonic waves, adding the materials into the reaction kettle according to the preferable mass ratio of 1200: 100: 5: 80, vacuumizing the reaction kettle at 150 ℃ for 15 minutes when the vacuum degree in the kettle is reduced to-0.1 Mpa, removing trace moisture in the reaction kettle, stirring for 10 minutes, adding the materials into an extruder, extruding and granulating at 210 ~ 230 ℃ to obtain an in-situ polymerized nylon 6-based graphene composite material, and performing injection molding on the material to obtain a heat dissipation substrate for preparing heat dissipation devices such as a computer heat dissipation base and a heat dissipation shell of a set top box.
Description
Technical Field
The invention relates to the technical field of reactive extrusion, in particular to the technical field of a method for preparing a nylon 6-based heat dissipation composite material by reactive extrusion.
Background
The reactive extrusion is a method that an extruder is used as a continuous reactor, monomers of polymers, fillers and auxiliaries react in the extruder to generate chemical reaction, namely, the continuous synthesis reaction of monomer raw materials and the melt processing of the polymers are integrated through a reactive extrusion technology, and required materials or products are formed in one step through a screw extruder. Compared with the common extrusion granulation technology, the reactive extrusion granulation technology can improve the interface bonding property of the filler and the polymer matrix, improve the dispersibility of the filler and the strength of the composite material, and achieve the purpose of polymer modification or incompatible system compatibilization; in addition, the reaction extrusion process has less overall procedures, low energy consumption and high production efficiency, and is suitable for being used as a composite material with small dosage and high performance requirement. Therefore, this technology has recently been applied in more and more fields. Such as conductive plastics, gas barrier materials, reinforced and toughened plastics, and the like.
with the increasing development of electronic products, people have been unable to keep electronic products in all aspects of life. However, the heat generation problem of electronic products is always a cause of affecting the product life and sensitivity. In order to prolong the service life of electronic products, the heat dissipation performance of materials such as electronic device chips, PCB mainboards, heat dissipation plates and the like directly determines the service life of the whole product. Traditionally, the products are generally made of metal materials, so that the strength is high, and the heat transfer performance is very strong; however, the heat transfer is high, so that the heat can be quickly transferred to the whole plate, and all the small parts mounted on the small parts are affected by the heat at the same time. This is very disadvantageous for some heat sensitive components. The heat radiation mode of the heat conduction plastic is heat conduction and also heat radiation; in the component that generates heat big transmits heat to thermal conductive plastic, because thermal conductive plastic heat-conduction is more full than sheet metal, radiate a large amount of heats to the surrounding environment in the time of the transmission, and avoid making local temperature sensing element on the mainboard receive the damage. Although the heat conductive plastic is an ideal material for heat dissipation devices of electronic components, the heat conductive plastic used in electronic and electric appliances generally has the following requirements: (1) the mechanical strength is high, and the high impact requirement can be met, especially thin-walled products; (2) the heat conducting performance is excellent, heat can be dissipated timely, and heat accumulation is avoided; (3) high fluidity and meets the molding requirements of products with complex shapes and thin-wall products. Therefore, as a heat conductive plastic for electronic devices, it is difficult for ordinary filled heat conductive plastics to meet the requirements of high performance heat dissipation devices.
Therefore, the graphene-filled nylon 6-based heat dissipation composite material is prepared by adopting a reaction extrusion molding method aiming at the problems that the common filled type heat conduction plastic is low in mechanical strength and difficult in flowability to meet the molding requirement of a thin-wall product, and is used for preparing a heat dissipation main board, a heat dissipation shell and the like of an electronic appliance. The method not only solves the heat dissipation problem of the nylon 6-based heat dissipation material, but also solves the problem of uneven dispersion of graphene in common plastic melt extrusion.
disclosure of Invention
The invention aims to make up for the defects of the existing heat dissipation plate material, provides a novel heat dissipation plate material, and solves the problems that the heat is gathered due to the quick heat conduction of a metal heat dissipation material, and the mechanical strength and the molding processability of the traditional heat conduction plastic are reduced under the high filling.
The technical scheme of the invention is as follows:
A method for preparing a nylon 6-based heat dissipation composite material by reactive extrusion comprises the following steps:
Dispersing expanded graphite with a certain mass in a proper amount of ethanol solution by adopting a liquid-phase ultrasonic stripping method, wherein the mass ratio of ethanol to graphite is 100: 5, adding a silane coupling agent with the graphite mass fraction of 3%, ultrasonically dispersing for 20 minutes at the wave frequency of 150 ~ 200KHz, and vacuumizing and drying at 60 ℃ to obtain the few-layer graphene;
Step two, adding caprolactam monomer, caprolactam salt, a cocatalyst HDI hexamethylene isocyanate and the processed few-layer graphene into a reaction kettle according to the mass ratio of 1000 ~ 1500: 90 ~ 120: 5 ~ 10: 50 ~ 100, pre-dispersing under the action of ultrasonic waves, vacuumizing the kettle to-0.1 Mpa, vacuumizing the reaction kettle at 150 ℃ for 15 minutes to remove trace moisture in the reaction kettle, continuously stirring for 10 minutes, adding the mixture into an extruder, and extruding and granulating to obtain the nylon 6-based graphene composite material, wherein the temperature of the extruder is set to 210 ~ 230-230 ℃;
And step three, adding the nylon 6-based graphene composite material particles obtained in the step two into an injection molding machine for injection molding to obtain the required heat dissipation device, wherein the temperature of the injection molding machine is set to be 220 ~ 240 ℃.
further, the preferable mass ratio of the caprolactam monomer, the ring-opening catalyst caprolactam salt, the cocatalyst HDI hexamethylene isocyanate and the few-layer graphene is 1200: 100: 5: 80; the ring-opening agent is caprolactam salt which is caprolactam sodium salt;
And further, dispersing expanded graphite in an ethanol solution by using a liquid-phase ultrasonic stripping method, adding a silane coupling agent with the graphite mass fraction of 3%, wherein the ultrasonic frequency is 150 ~ 200KHz, and performing vacuum drying at 60 ℃ to obtain the few-layer graphene, wherein the few-layer graphene is a graphite sheet material with the carbon layer thickness of 2-10.
compared with the prior art, the preparation of the nylon 6-based heat dissipation material has the following benefits:
The first and the second extrusion technologies integrate the continuous synthesis reaction of caprolactam monomer and the melt processing of polymer, and the required material is formed in one step by a screw extruder, and the process can improve the interface bonding property of the filler and the polymer matrix, improve the dispersibility of the filler and the strength of the composite material, and achieve the purpose of polymer modification or incompatible system compatibilization.
Secondly, the process for preparing the nylon 6-based composite material has the advantages that the graphene is dispersed in the caprolactam monomer in advance, so that the caprolactam monomer is fully dispersed, and the heat conductivity of the nylon 6 can be effectively improved.
Thirdly, the nylon 6-based heat dissipation composite material prepared by the process has high mechanical strength and excellent molding fluidity, and is suitable for preparing thin-wall devices with complex shapes.
examples of the embodiments
The present invention will be described in more detail with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
example 1, a method for preparing a nylon 6-based heat dissipation composite by reactive extrusion:
dispersing 50 g of expanded graphite in 1000 g of ethanol solution by adopting a liquid-phase ultrasonic stripping method, adding a silane coupling agent with the graphite mass fraction of 3%, ultrasonically dispersing for 20 minutes at the wave frequency of 150 ~ 200KHz, and vacuumizing and drying at 60 ℃ to obtain the few-layer graphene;
Step two, adding caprolactam monomer, caprolactam sodium salt, HDI and the processed few-layer graphene into a reaction kettle according to the mass ratio of 1000: 90: 5: 50, pre-dispersing under the action of ultrasonic waves, vacuumizing the reaction kettle to-0.1 Mpa, vacuumizing the reaction kettle for 15 minutes at 150 ℃, removing trace moisture in the reaction kettle, continuously stirring for 10 minutes, adding the mixture into an extruder, and extruding and granulating to obtain the nylon 6-based graphene composite material, wherein the temperature of the extruder is set to 210 ~ 230 ℃.
And step three, adding the nylon 6-based graphene composite material particles obtained in the step two into an injection molding machine for injection molding to obtain the required heat dissipation device, setting the temperature of the injection molding machine to be 220 ~ 240 ℃ and carrying out performance test according to related national standards.
According to the relevant national standard, the test result of the first embodiment is as follows: the tensile strength was 83MPa, the bending strength was 90MPa, the melt index was 35g/10min, and the in-plane thermal conductivity was 12W/m.K.
example 2, a method for preparing a nylon 6-based heat dissipation composite by reactive extrusion:
Dispersing 100 g of expanded graphite in 2000 g of ethanol solution by adopting a liquid-phase ultrasonic stripping method, adding a silane coupling agent with the graphite mass fraction of 3%, ultrasonically dispersing for 20 minutes at the wave frequency of 150 ~ 200KHz, and vacuumizing and drying at 60 ℃ to obtain the few-layer graphene;
Step two, adding caprolactam monomer, caprolactam sodium salt, HDI and the processed few-layer graphene into a reaction kettle according to the mass ratio of 1200: 100: 5: 80, pre-dispersing under the action of ultrasonic waves, vacuumizing the reaction kettle to-0.1 Mpa, vacuumizing the reaction kettle for 15 minutes at 150 ℃, removing trace moisture in the reaction kettle, continuously stirring for 10 minutes, adding the mixture into an extruder, and extruding and granulating to obtain the nylon 6-based graphene composite material, wherein the temperature of the extruder is set to 210 ~ 230 ℃.
And step three, adding the nylon 6-based graphene composite material particles obtained in the step two into an injection molding machine for injection molding to obtain the required heat dissipation device, setting the temperature of the injection molding machine to be 220 ~ 240 ℃ and carrying out performance test according to related national standards.
According to the relevant national standard, the test result of the second embodiment is as follows: the tensile strength was 95MPa, the bending strength was 100MPa, the melt index was 40g/10min, and the in-plane thermal conductivity was 18W/m.K.
Example 3, a method of preparing a nylon 6-based heat dissipating composite by reactive extrusion:
dispersing 100 g of expanded graphite in 2000 g of ethanol solution by adopting a liquid-phase ultrasonic stripping method, adding a silane coupling agent with the graphite mass fraction of 3%, ultrasonically dispersing for 20 minutes at the wave frequency of 150 ~ 200KHz, and vacuumizing and drying at 60 ℃ to obtain the few-layer graphene;
Step two, adding caprolactam monomer, caprolactam sodium salt, HDI and the processed few-layer graphene into a reaction kettle according to the mass ratio of 1200: 80: 10: 100, pre-dispersing under the action of ultrasonic waves, vacuumizing the reaction kettle to-0.1 Mpa, vacuumizing the reaction kettle for 15 minutes at 150 ℃, removing trace moisture in the reaction kettle, continuously stirring for 10 minutes, adding the mixture into an extruder, and extruding and granulating to obtain the nylon 6-based graphene composite material, wherein the temperature of the extruder is set to 210 ~ 230 ℃.
And step three, adding the nylon 6-based graphene composite material particles obtained in the step two into an injection molding machine for injection molding to obtain the required heat dissipation device, setting the temperature of the injection molding machine to be 220 ~ 240 ℃ and carrying out performance test according to related national standards.
The test results of example three, according to the relevant national standards, are: tensile strength 73MPa, bending strength 85MPa, melt index 25g/10min, in-plane thermal conductivity is 16W/m.K.
Claims (4)
1. A method for preparing a nylon 6-based heat dissipation composite material by reactive extrusion comprises the following steps:
dispersing expanded graphite with a certain mass in a proper amount of ethanol solution by adopting a liquid-phase ultrasonic stripping method, wherein the mass ratio of ethanol to graphite is 100: 5, adding a silane coupling agent with the graphite mass fraction of 3%, ultrasonically dispersing for 20 minutes at the wave frequency of 150 ~ 200KHz, and vacuumizing and drying at 60 ℃ to obtain the few-layer graphene;
step two, adding caprolactam monomer, caprolactam salt, a cocatalyst HDI hexamethylene isocyanate and the processed few-layer graphene into a reaction kettle according to the mass ratio of 1000 ~ 1500: 90 ~ 120: 5 ~ 10: 50 ~ 100, pre-dispersing under the action of ultrasonic waves, vacuumizing the kettle to-0.1 Mpa, vacuumizing the reaction kettle at 150 ℃ for 15 minutes to remove trace moisture in the reaction kettle, continuously stirring for 10 minutes, adding the mixture into an extruder, and extruding and granulating to obtain the nylon 6-based graphene composite material, wherein the temperature of the extruder is set to 210 ~ 230-230 ℃;
and step three, adding the nylon 6-based graphene composite material particles obtained in the step two into an injection molding machine for injection molding to obtain the required heat dissipation device, wherein the temperature of the injection molding machine is set to be 220 ~ 240 ℃.
2. the reactive extrusion method for preparing a nylon 6-based heat dissipation composite material according to claim 1, wherein the preferred mass ratio of the caprolactam monomer, the ring-opening catalyst caprolactam salt, the cocatalyst HDI hexamethylene isocyanate and the few-layer graphene is 1200: 100: 5: 80.
3. The reactive extrusion method for preparing a nylon 6-based heat dissipation composite material according to claim 1, wherein the few-layer graphene is a graphite flake material with a thickness of 2-10 carbon layers.
4. The ring opener of claim 1 wherein the salt of caprolactam is caprolactam sodium.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2622753A (en) * | 2023-01-04 | 2024-03-27 | Univ Qilu Technology | Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2622753A (en) * | 2023-01-04 | 2024-03-27 | Univ Qilu Technology | Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof |
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Application publication date: 20191210 |