CN109082109A - A kind of polyamide and graphene high heat conducting nano composite material and preparation method thereof - Google Patents
A kind of polyamide and graphene high heat conducting nano composite material and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of polyamide and graphene high heat conducting nano composite material, the raw material of the composite material forms and its weight percent are as follows: polyamide 48-60%, graphene agent 20-30%, crystalline flake graphite 15-28%, silane coupling agent 0.12 ~ 0.18%, dispersing agent 0.12 ~ 0.18%, antioxidant 0.22 ~ 0.27%, the graphene agent are selected from one of redox graphene or graphene oxide or a variety of.The present invention is by using redox graphene or graphene oxide, make polyamide that there is good heating conduction, effectively improve the thermal conductivity of composite material, and then ensure that composite material can effectively radiate to electronic components such as LED illumination component, IC, achieve the effect that extend electronic component service life.
Description
Technical field
The present invention relates to a kind of polyamide nano-composite, especially a kind of polyamide and graphene high heat conducting nano are multiple
Condensation material and preparation method thereof.
Background technique
In electronics and opto-electronics, the heating conduction of material is particularly important, is all concerned all the time and research
Subject under discussion, especially in consumer electrical product and LED illumination market, heat dissipation effect is directly related with the service life of product,
Thermal conductivity of material is poor easily to cause product in running order for a long time, and product service life is caused to decline.Macromolecule material
Material has many advantages, such as light weight, corrosion resistance, tough physical property and excellent processability, and it is light can to realize that electronic product obtains easily
The target of thinning, but common high molecular material thermal conductivity is poor, causes LED illumination component, IC thermal diffusivity poor, causes electric appliance
The service life of element is by biggish negative effect.
Polyamide, English name polyamide are the product that throughput requirements are maximum in engineering plastics, purposes is most wide
?.It is widely used in the fields such as machinery, auto-parts, electric equipment products, textile, chemical industry equipment and aviation.Its main feature
For excellent mechanical property, high mechanical strength, obdurability be good, tool electrical insulating property, heat-resistant deforming temperature height and abrasion performance are good etc.
Advantage.The heating conduction of polyamide itself is poor.In order to make the polyamide as heat insulator become good heat conductor, usually
It needs to add a large amount of heat-conducting filler or inorganic alloys conductor and can just polyamide be made to be stablized through complicated processing procedure
The production batch uniformity and excellent heating conduction.
Grapheme material is passed through researches show that the substance to possess highest coefficient of heat transfer in current application material in the world, is approximately
14 times of copper, 3.5 times of graphite, and there is very excellent mechanical property and chemical stability.Therefore graphene is considered most
It is suitble to solve current LED illumination and consumer electrical product heat dissipation problem.
Summary of the invention
The present invention provides a kind of polyamide and graphene high heat conducting nano composite material and preparation method thereof, at least to solve
The certainly lower problem of polyamide thermal conductivity in the prior art.
Mesh of the present invention it is the provision of a kind of polyamide and graphene high heat conducting nano composite material, the composite material
Raw material composition and its weight percent are as follows: polyamide 48-60%, graphene agent 20-30%, crystalline flake graphite 15-28%, silane are even
Mixture 0.12 ~ 0.18%, dispersing agent 0.12 ~ 0.18%, antioxidant 0.22 ~ 0.27%, the graphene agent are selected from redox graphite
One of alkene or graphene oxide are a variety of.
Further, composite material raw material composition and its weight percent are as follows: polyamide 54.5%, graphene agent 25%,
Crystalline flake graphite 20%, silane coupling agent 0.15%, dispersing agent 0.1%, antioxidant 0.25%.
Further, the polyamide is selected from polyamide 6, polyamide 66, polyamide 610, polyamide 46, polyamide
One of 612 or a variety of, and the flow index of the polyamide is 3g/10min -10g/10min.
Further, graphite partial size is 50nm -100nm in the graphene agent.
Further, the silane coupling agent is selected from γ-aminopropyl triethoxysilane or γ-(2,3- epoxies
Propoxyl group) one of propyl trimethoxy silicane or a variety of.
Further, the antioxidant is selected from one of Antioxidant 1098,168,1010,626 or 1076
Or it is a variety of.
Further, the polyamide includes polyamide 6, polyamide 610, perfluoroalkyl ethanol, in the polyamide
Polyamide 6, polyamide 610, perfluoroalkyl ethanol weight ratio be (5-10): (3-15): (0.1-1).
Another mesh of the invention it is the provision of the preparation of above-mentioned polyamide Yu graphene high heat conducting nano composite material
Method, comprising the following steps:
Step 1: polyamide is dry at 95-115 DEG C into drying equipment with hot-air circulation to remove water 4-6 hours；
Step 2: the height of step 1 gained polyamide, graphene agent merging nitrogen filled protection being mixed in mixer, at 245-260 DEG C
Melting mixing 8-13 minutes；
Step 3: to be added in the resulting polyamide of step 2 and graphene composite material semi-finished product crystalline flake graphite, silane coupling agent,
Dispersing agent and antioxidant, merging nitrogen filled protection height mix in mixer at 260 DEG C melting mixing 15 minutes to get polyamide with
Redox graphene or graphene oxide composite material.
Another mesh of the invention it is the provision of the use of above-mentioned polyamide Yu graphene high heat conducting nano composite material
Method includes the following steps
Step 1: polyamide is that (10:1-30) is mixed, and is added to weight ratio with the composite material of graphene with pure polyamide
Melt blending extruding pelletization is carried out in double-screw extruding pelletizing machine to get finished product.
Step 2: the finished product of obtaining step 1 is placed in the baking oven of 60 DEG C of nitrogen filled protections after maturation 8 hours, sealed package
Up to target product.
Further, in the step 1 double-screw extruding pelletizing machine melt blending condition are as follows: at 265 DEG C, with 680
The screw speed of rpm is granulated master batch.
The present invention compared with the existing technology, using redox graphene or graphene oxide, has polyamide good
Good heating conduction, effectively improves the thermal conductivity of composite material, and then ensure that composite material can be to LED illumination component, IC etc.
Electronic component is effectively radiated, and achievees the effect that extend electronic component service life.Meanwhile the present invention is using journey, height in short-term
Efficiency and step explicitly mix at a high speed mixing technology and the polyamide with high stable batch uniformity and excellent heat conducting performance are made
Composite material simplifies the production technology of composite material, stabilizing material quality, reduces cost；And product is made to possess physical property sustainment rate
Height, processing performance is excellent and has the high advantage of thermal conductivity.
Specific embodiment
It in order to enable those skilled in the art to better understand the solution of the present invention, below will be to the skill in the embodiment of the present invention
Art scheme is clearly and completely described, it is clear that and the described embodiment is only a part of the embodiment of the present invention, without
It is whole embodiments.
Embodiment 1
The raw material of 1 composite material of embodiment forms and its weight percent are as follows: polyamide 6 48%, the oxygen that partial size is 100nm
Graphite alkene 30%, crystalline flake graphite 21.37%, γ-aminopropyl triethoxysilane 0.18%, lauryl sodium sulfate 0.18%,
Antioxidant 1098 0.27%。
1 composite material of embodiment the preparation method is as follows:
Step 1: polyamide 6 is dry at 100 DEG C into drying equipment with hot-air circulation to remove water 4 hours；
Step 2: the height of step 1 gained polyamide 6, graphene oxide merging nitrogen filled protection being mixed in mixer, is melted at 260 DEG C
Melt mixing 12 minutes；
Step 3: crystalline flake graphite, γ-ammonia being added into the resulting polyamide 6 of step 2 and graphene oxide composite material semi-finished product
Propyl-triethoxysilicane, lauryl sodium sulfate and Antioxidant 1098 are placed in the mixed mixer of nitrogen filled protection height
The melting mixing 15 minutes composite materials to get the present embodiment 1 polyamide and graphene at 260 DEG C.
Embodiment 2
The raw material of 2 composite material of embodiment forms and its weight percent are as follows: polyamide 66 54.5%, partial size 100nm
Redox graphene 25%, crystalline flake graphite 20%, γ-(2,3- glycidoxy) propyl trimethoxy silicane 0.15%,
Lauryl sodium sulfate 0.1%, Antioxidant168 0.25%.
2 composite material of embodiment the preparation method is as follows:
Step 1: polyamide 66 is dry at 100 DEG C into drying equipment with hot-air circulation to remove water 4 hours；
Step 2: the height of step 1 gained polyamide 66, redox graphene merging nitrogen filled protection being mixed in mixer, 260
Melting mixing 12 minutes at DEG C；
Step 3: to be added in the resulting polyamide 66 of step 2 and redox graphene composite material semi-finished product crystalline flake graphite,
γ-(2,3- glycidoxy) propyl trimethoxy silicane, lauryl sodium sulfate and Antioxidant168, merging are filled
In the high mixed mixer of nitrogen protection at 260 DEG C melting mixing 15 minutes to get the compound of 2 polyamide of the present embodiment and graphene
Material.
Embodiment 3
The raw material of 3 composite material of embodiment forms and its weight percent are as follows: polyamide 6 0%, graphene agent 20%, scale
Graphite 19.54%, γ-(2,3- glycidoxy) propyl trimethoxy silicane 0.12%, lauryl sodium sulfate 0.12%,
Antioxidant1010 0.22%.Wherein, the polyamide includes polyamide 6, polyamide 610, perfluoroalkyl ethanol, and institute
State polyamide 6, polyamide 610, perfluoroalkyl ethanol weight ratio be 10:5:0.5；The graphene agent includes partial size 100nm
Redox graphene and partial size 100nm graphene oxide, and the weight ratio of redox graphene and graphene oxide
For 1:1.
3 composite material of embodiment the preparation method is as follows:
Step 1: polyamide is dry at 100 DEG C into drying equipment with hot-air circulation to remove water 4 hours；
Step 2: the height of step 1 gained polyamide, graphene agent merging nitrogen filled protection being mixed in mixer, is melted at 260 DEG C
It is kneaded 12 minutes；
Step 3: crystalline flake graphite, γ-(2,3- being added into the resulting polyamide of step 2 and graphene composite material semi-finished product
Glycidoxy) propyl trimethoxy silicane, lauryl sodium sulfate and Antioxidant1010, it is mixed to be placed in nitrogen filled protection height
In mixer at 260 DEG C the melting mixing 15 minutes composite materials to get the present embodiment 3 polyamide and graphene.
Reference examples 1
The raw material of 1 composite material of reference examples forms and its weight fraction ratio are as follows: 54.5 parts of polyamide 66, partial size 100nm
25 parts of redox graphene, 0.15 part of γ-(2,3- glycidoxy) propyl trimethoxy silicane, dodecyl sulphur
0.1 part of sour sodium, 0.25 part of Antioxidant168.
1 composite material of reference examples the preparation method is as follows:
Step 1: polyamide 66 is dry at 100 DEG C into drying equipment with hot-air circulation to remove water 4 hours；
Step 2: the height of step 1 gained polyamide 66, redox graphene merging nitrogen filled protection being mixed in mixer, 260
Melting mixing 12 minutes at DEG C；
Step 3: to be added in the resulting polyamide 66 of step 2 and redox graphene composite material semi-finished product γ-(2,
3- glycidoxy) propyl trimethoxy silicane, lauryl sodium sulfate and Antioxidant168, it is mixed to be placed in nitrogen filled protection height
In mixer at 260 DEG C the melting mixing 15 minutes composite materials to get this reference examples 1 polyamide and graphene.
Reference examples 2
The raw material of 2 composite material of reference examples forms and its weight fraction ratio are as follows: 54.5 parts of polyamide 66, γ-(2,3-
Glycidoxy) 0.15 part of propyl trimethoxy silicane, 0.1 part of lauryl sodium sulfate, 0.25 part of Antioxidant168.
2 composite material of reference examples the preparation method is as follows:
Step 1: polyamide 66 is dry at 100 DEG C into drying equipment with hot-air circulation to remove water 4 hours；
Step 2: the height of step 1 gained polyamide 66 merging nitrogen filled protection being mixed in mixer, melting mixing 12 divides at 260 DEG C
Clock；
Step 3: γ-(2,3- glycidoxy) propyl trimethoxy silicane, ten is added to the resulting polyamide 66 of step 2
Sodium dialkyl sulfate and Antioxidant168, merging nitrogen filled protection height mix mixer at 260 DEG C melting mixing 15 divide
Clock to get this reference examples 2 polyamide and graphene composite material.
Embodiment 4
Using the composite material of the polyamide of embodiment 2 and graphene as master batch, carry out as follows using the method for production:
Step 1: 2 polyamide of embodiment being mixed with the composite material of graphene with polyamide 6 with weight ratio 1:1, is placed into double
In screw extruder pelletizer, with 205 DEG C of first area's processing temperature, 220 DEG C of two area's processing temperature, three area's processing temperatures 235
DEG C, 255 DEG C of four area's processing temperature, 265 DEG C of granulating head area processing temperature, 680 rpm of screw speed melt altogether
Mixed extruding pelletization；
Step 2: the finished product of obtaining step 1 is placed in 60 DEG C of nitrogen filled protection baking ovens after maturation 4 hours up to target product.
Properties inspection is carried out to embodiment 1-3 and reference examples 1-2 using ASTM examination criteria, as a result such as following table institute
Show,
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Reference examples 1 | Reference examples 2 | |
| Tensile strength (MPa) | 61.2 | 68.8 | 70.2 | 79.3 | 80.5 | 89.3 |
| Bending modulus (MPa) | 17880 .7 | 17740 .3 | 17650 .9 | 10467.3 | 10005.2 | 9452.8 |
| Impact strength (J/ M) | 24.1 | 31.2 | 33.5 | 42.6 | 41.3 | 53.2 |
| Thermal conductivity (W/m. K) | 56.72 | 54.68 | 51.68 | 34.15 | 28.42 | 0.32 |
| Salt fog resistance (2500h) | There is aging on surface Slight crack | There is aging on surface Slight crack | Without obvious aging Slight crack | There is aging on surface Slight crack | There is aging on surface Slight crack | Surface has aging to split Trace |
1-4 of the embodiment of the present invention uses redox graphene or graphene oxide, and polyamide is made to have good thermal conductivity
Can, effectively improve the thermal conductivity of composite material, and then ensure composite material can to the electronic components such as LED illumination component, IC into
Row effectively heat dissipation, achievees the effect that extend electronic component service life.Meanwhile the embodiment of the present invention 2, by using scale stone
Ink makes 2 composite material of embodiment have preferable heating conduction, compared to the reference examples 1 only with graphene, 2 heat of embodiment
It leads performance and is substantially better than reference examples 1, even with embodiment 4 similar in 1 carbon element content of reference examples, using graphene and scale
The heating conduction of the embodiment 4 of graphite mixing is also significantly better than the heating conduction of reference examples 1.
In addition, as shown above, by using the polyamide containing perfluoroalkyl ethanol in embodiment 3, effectively improving compound
The corrosion resistance of material, it is ensured that composite material can be applied to a variety of harsh environments, and then expand the usable model of composite material
It encloses.
Finally it should be noted that the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
Invention is explained in detail referring to above-described embodiment for pipe, it should be understood by a person of ordinary skill in the art that technology
Personnel read present specification after still can with modifications or equivalent substitutions are made to specific embodiments of the invention, but this
A little modifications are changed within all without departing from the present patent application accompanying claims protection scope.
Claims (10)
1. a kind of polyamide and graphene high heat conducting nano composite material, which is characterized in that the raw material of the composite material forms
And its weight percent are as follows: polyamide 48-60%, graphene agent 20-30%, crystalline flake graphite 15-28%, silane coupling agent 0.12 ~
0.18%, dispersing agent 0.12 ~ 0.18%, antioxidant 0.22 ~ 0.27%, the graphene agent are selected from redox graphene or oxidation
One of graphene is a variety of.
2. polyamide according to claim 1 and graphene high heat conducting nano composite material, which is characterized in that composite material
Raw material composition and its weight percent are as follows: polyamide 54.5%, graphene agent 25%, crystalline flake graphite 20%, silane coupling agent
0.15%, dispersing agent 0.1%, antioxidant 0.25%.
3. polyamide according to claim 1 or 2 and graphene high heat conducting nano composite material, which is characterized in that described
Polyamide is selected from one of polyamide 6, polyamide 66, polyamide 610, polyamide 46, polyamide 612 or a variety of and described
The flow index of polyamide is 3g/10min -10g/10min.
4. polyamide according to claim 1 or 2 and graphene high heat conducting nano composite material, which is characterized in that described
Graphite partial size is 50nm -100nm in graphene agent.
5. polyamide according to claim 1 or 2 and graphene high heat conducting nano composite material, which is characterized in that described
Silane coupling agent is selected from γ-aminopropyl triethoxysilane or γ-(2,3- glycidoxy) propyl trimethoxy silicane
It is one or more.
6. polyamide according to claim 1 or 2 and graphene high heat conducting nano composite material, which is characterized in that described
Antioxidant is selected from one of Antioxidant 1098,168,1010,626 or 1076 or a variety of.
7. polyamide according to claim 1 or 2 and graphene high heat conducting nano composite material, which is characterized in that described
Polyamide includes polyamide 6, polyamide 610, perfluoroalkyl ethanol, polyamide 6, polyamide 610, perfluor alkane in the polyamide
The weight ratio of base ethyl alcohol is (5-10): (3-15): (0.1-1).
8. a kind of preparation method of polyamide as claimed in claim 1 or 2 and graphene high heat conducting nano composite material, feature
It is, comprising the following steps:
Step 1: polyamide is dry at 95-115 DEG C into drying equipment with hot-air circulation to remove water 4-6 hours；
Step 2: the height of step 1 gained polyamide, graphene agent merging nitrogen filled protection being mixed in mixer, at 245-260 DEG C
Melting mixing 8-13 minutes；
Step 3: to be added in the resulting polyamide of step 2 and graphene composite material semi-finished product crystalline flake graphite, silane coupling agent,
Dispersing agent and antioxidant, merging nitrogen filled protection height mix in mixer at 260 DEG C melting mixing 15 minutes to get polyamide with
Graphene composite material.
9. a kind of application method of polyamide and graphene high heat conducting nano composite material as described in claim 1-2, feature
It is, steps are as follows:
Step 1: polyamide is that (10:1-30) is mixed, and is added to weight ratio with the composite material of graphene with pure polyamide
Melt blending extruding pelletization is carried out in double-screw extruding pelletizing machine to get finished product；
Step 2: the finished product of obtaining step 1 is placed in the baking oven of 60 DEG C of nitrogen filled protections after maturation 8 hours, and sealed package to obtain the final product
Target product.
10. the application method of polyamide according to claim 9 and graphene high heat conducting nano composite material, feature
It is, the melt blending condition of double-screw extruding pelletizing machine in the step 1 are as follows: at 265 DEG C, turned with the screw rod of 680 rpm
Speed is granulated master batch.
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| CN113861817A (en) * | 2021-11-09 | 2021-12-31 | 烟台恒诺新材料有限公司 | Oily ultraviolet-resistant corrosion-resistant anti-drop coating material and preparation method thereof |
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| CN104559149A (en) * | 2014-12-16 | 2015-04-29 | 惠州力王佐信科技有限公司 | Carbon composite high-thermal-conductivity plastic material 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 |
| CN107324973A (en) * | 2017-07-05 | 2017-11-07 | 巨化集团技术中心 | A kind of preparation method of perfluoroalkyl ethanol |
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