CN112708270B - High-thermal-conductivity nylon-based composite material and preparation method thereof - Google Patents
High-thermal-conductivity nylon-based 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
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Abstract
The invention discloses a high-thermal-conductivity nylon-based composite material, which comprises the following components in parts by weight: 25-60 parts of nylon resin, 30-65 parts of graphite powder, 0.3-2 parts of coupling agent containing mercaptopropyl and 5-15 parts of glass fiber. The high-thermal-conductivity nylon-based composite material prepared by the invention can still be normally extruded and produced by using a conventional extruder when the filling amount of the graphite thermal-conductivity filler is more than 60wt%, and the composite material has good processing fluidity, so that the problem of glue shortage can not occur in the process of injection molding of a molded product, and the molding processing quality of the molded product is ensured; the prepared molded product has excellent heat conducting performance and good mechanical property, can directly replace metal aluminum materials to be used as heat radiating parts of lamps with high heat radiating performance requirements, such as high-power industrial and mining lamps, outdoor projection lamps, commercial PAR lamps, car lamps and the like, and expands the application range of the nylon-based composite material.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-thermal-conductivity nylon-based composite material and a preparation method thereof.
Background
With the development of science and technology and production, many products have higher requirements on heat conduction materials, and hope that the products have more excellent comprehensive performance, light weight, strong chemical corrosion resistance, impact resistance, simple and convenient processing and forming and the like. Conventional heat conductive materials such as metal and ceramic materials have been difficult to satisfy the above performance requirements, and therefore, the development of new heat conductive materials is urgently needed.
Nylon is a common engineering plastic, has the advantages of light weight, good fluidity, good processability, low cost and the like, and is widely applied to the fields of electronics and electrical products, household electrical appliances, electromechanical industry, automobile electrical products and the like. However, the nylon has low bulk thermal conductivity (lambda), generally 0.25W/m.K, which greatly limits the application of the nylon in the fields of heat dissipation and heat conduction. In order to improve the heat-conducting property of nylon, the conventional technical means is to fill heat-conducting filler in nylon, and the nylon has low preparation cost, is easy to form and process, and is very suitable for industrial production. However, to achieve useful thermal conductivity, the nylon system must be filled with a large amount of thermally conductive filler (typically more than 30wt% thermally conductive filler). However, the mechanical properties and processing flow properties of the polymer material are affected by the filling of a large amount of heat-conducting filler. Particularly, in order to obtain high heat conductivity, more than 50wt% of heat conductive filler is usually required to be filled, so that the mechanical property and the processing fluidity of the nylon-based heat conductive composite material are suddenly reduced, the problems of strand breaking and difficult granulation frequently occur in the extrusion processing process of the composite material, the production efficiency is seriously influenced, meanwhile, the problem of glue shortage of products frequently occurs in the process of processing the products by injection molding, the quality of the products is influenced, and further, the actual application value is lost due to the fact that the processing fluidity is too low, and the injection molding cannot be performed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a high-thermal-conductivity nylon-based composite material and a preparation method thereof, so that the nylon-based composite material has excellent thermal conductivity, mechanical property and processing fluidity, and can be applied to the fields of heat dissipation and heat conduction with high heat dissipation requirements instead of metal aluminum materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-thermal-conductivity nylon-based composite material comprises the following components in parts by weight:
25-60 parts of nylon resin,
30-65 parts of graphite powder,
0.3 to 2 parts of coupling agent containing mercaptopropyl,
5-15 parts of glass fiber.
The nylon resin is at least one of PA6, PA66 and PA 6/66.
The graphite powder is flake graphite, spherical graphite or a compound of the flake graphite and the spherical graphite.
Preferably, the mesh size of the flake graphite is 100-1000 meshes, and the mesh size of the spherical graphite is 100-1000 meshes.
The mercaptopropyl-containing coupling agent is one or more of gamma-mercaptopropyl trimethoxysilane, 3-mercaptopropyl-triethoxysilane, 3-mercaptopropyl methyldiethoxysilane, gamma-mercaptopropyl trialkoxysilane, 3-mercaptopropyl dimethylethoxysilane, gamma-mercaptopropyl dimethoxymethylsilane, gamma-mercaptopropyl methyldimethoxysilane, gamma-mercaptopropyl-ethoxybis (propyl hexapropoxy) silane, 2-mercaptopropyl trimethoxysilane, 2-mercaptopropyl triethoxysilane and gamma-mercaptopropyl methoxysilane.
Preferably, the high-thermal-conductivity nylon-based composite material comprises the following components in parts by weight:
30-40 parts of nylon resin,
50-65 parts of graphite powder,
0.5-2 parts of coupling agent containing mercaptopropyl,
5-15 parts of glass fiber,
0.5-1 part of a flow improver;
the graphite powder is a compound of crystalline flake graphite and spherical graphite, and the weight ratio of the crystalline flake graphite to the spherical graphite in the compound is 1: 3-3: 1.
Preferably, the nylon resin has a relative viscosity of 1.8 to 2.4, and preferably a PA6 resin having a relative viscosity of 1.8 to 2.4.
Further preferably, the graphite powder is a compound of 100-mesh crystalline flake graphite and 1000-mesh spherical graphite in a weight ratio of 1: 1-3: 1.
The flow improver selects one or more of lubricant TR063A, dendritic polymer and hyperbranched resin.
The high-thermal-conductivity nylon-based composite material is prepared by adopting the following process: proportionally adding the raw materials into a mixer for mixing, adding the mixed materials into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion and granulation by the same-direction double-screw extruder to obtain granules, wherein the granulation process adopts an air cooling hot cutting granulation process.
Another object of the present invention is to provide a molded article made of the above highly thermal conductive nylon-based composite material, which can be directly used as a heat-dissipating member of high-power industrial and mining lamps, outdoor projection lamps, commercial PAR lamps, car lamps, and the like, which require high heat-dissipating performance, instead of aluminum materials.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the mercaptopropyl-containing coupling agent is introduced, so that on one hand, the binding force between inorganic fillers such as graphite powder and glass fiber and a nylon resin matrix is effectively increased, the graphite powder, the glass fiber and the nylon resin are firmly bound together, and the mechanical property of the composite material is improved; on the other hand, the dispersibility of the graphite powder heat-conducting filler in the nylon resin matrix is improved, so that more heat-conducting paths are constructed, and the heat-conducting nylon-based composite material has excellent heat-conducting property.
(2) The high-thermal-conductivity nylon-based composite material can still be normally extruded and produced by using a conventional extruder when the filling amount of the graphite thermal-conductivity filler is more than 60wt%, and the composite material has good processing fluidity, so that the problem of glue shortage cannot occur in the process of injection molding of a molded product, and the molding processing quality of the molded product is ensured; the prepared molded product has excellent heat conducting performance and good mechanical property, can directly replace metal aluminum materials to be used as heat radiating parts of lamps with high heat radiating performance requirements, such as high-power industrial and mining lamps, outdoor projection lamps, commercial PAR lamps, car lamps and the like, and expands the application range of the nylon-based composite material.
Drawings
FIG. 1 is a photograph showing the heat dissipation of the heat-conducting nylon-based material and the aluminum heat sink of the present invention to the heat-generating sheet.
Fig. 2 is a heat dissipation temperature rise curve of the heat-conducting nylon-based material and the aluminum heat sink of the present invention to the heating plate.
Detailed Description
To further clarify the objects, technical solutions and advantages of the present invention, the following detailed description of the present invention is provided with reference to specific examples, which should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention will be further described with reference to examples 1 to 8 and comparative examples 1 to 4.
Example 1
(1) Weighing the following components in parts by weight: 60 parts of nylon resin (30 parts of PA6 with the relative viscosity of 2.0 and 30 parts of PA66 with the relative viscosity of 2.0), 30 parts of flake graphite (1000 meshes), 10 parts of glass fiber and 0.5 part of 3-mercaptopropyltriethoxysilane;
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
The air-cooling hot-cutting granulation process is adopted to replace the conventional water-cooling brace granulation process, so that the problem of frequent material breakage of water-cooling brace granulation in the extrusion processing granulation process caused by high filling amount of the inorganic filler is well avoided, the production efficiency of the composite material can be obviously improved, and the prepared granules are more uniform in size.
Example 2
(1) Weighing the following components in parts by weight: 40 parts of nylon resin (PA 6 with the relative viscosity of 1.8), 50 parts of spherical graphite (500 meshes), 10 parts of glass fiber, 1 part of gamma-mercaptopropyl-methyldimethoxysilane and 0.5 part of dendritic polymer (CYD-816A, Withachen molecular new material Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 3
(1) Weighing the following components in parts by weight: 30 parts of nylon resin (PA 6 with the relative viscosity of 2.0), 35 parts of flake graphite (100 meshes), 30 parts of spherical graphite (1000 meshes), 5 parts of glass fiber, 2 parts of 3-mercaptopropyltriethoxysilane and 1.5 parts of hyperbranched resin (HyPer HPN202, Wuhan hyperbranched resin science and technology Limited);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 4
(1) Weighing the following components in parts by weight: 45 parts of nylon resin (PA 66 with the relative viscosity of 2.4), 10 parts of flake graphite (100 meshes), 30 parts of spherical graphite (1000 meshes), 15 parts of glass fiber, 1 part of gamma-mercaptopropyl-methyldimethoxysilane and 0.5 part of dendritic polymer (CYD-816A, Wihamen molecular new materials Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 5
(1) Weighing the following components in parts by weight: 35 parts of nylon resin (PA 6 with the relative viscosity of 2.0), 45 parts of flake graphite (100 meshes), 15 parts of spherical graphite (1000 meshes), 5 parts of glass fiber, 0.6 part of 3-mercaptopropyl dimethyl ethoxy silane and 1 part of dendritic polymer (CYD-816A, Wihamen molecular new material Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 6
(1) Weighing the following components in parts by weight: 35 parts of nylon resin (PA 6 with the relative viscosity of 2.0), 30 parts of flake graphite (100 meshes), 30 parts of spherical graphite (1000 meshes), 5 parts of glass fiber, 0.6 part of 3-mercaptopropyl dimethyl ethoxy silane and 1 part of dendritic polymer (CYD-816A, Wihamen molecular new material Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 7
(1) Weighing the following components in parts by weight: 35 parts of nylon resin (PA 6 with the relative viscosity of 2.0), 40 parts of flake graphite (100 meshes), 20 parts of spherical graphite (1000 meshes), 5 parts of glass fiber, 0.6 part of 3-mercaptopropyl dimethyl ethoxy silane and 1 part of dendritic polymer (CYD-816A, Wihamen molecular new material Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Example 8
(1) Weighing the following components in parts by weight: 55 parts of nylon resin (PA 6 with the relative viscosity of 2.4), 30 parts of flake graphite (500 meshes), 15 parts of glass fiber, 0.45 part of 3-mercaptopropyltriethoxysilane, and 0.5 part of hyperbranched resin (HyPer HPN202, Wuhan hyperbranched resin science and technology Co., Ltd.);
(2) and uniformly mixing the weighed components by a high-speed mixer to obtain a premix, putting the premix into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion, air cooling and hot cutting granulation by the aid of the co-rotating double-screw extruder to obtain the composite material.
Comparative example 1
Comparative example 1 provides a nylon composite, differing from example 2 in that: the gamma-mercaptopropylmethyldimethoxysilane was replaced with KH-550 silane coupling agent, and the rest was the same as in example 2.
Comparative example 2
Comparative example 2 provides a nylon composite, differing from example 3 in that: the procedure of example 3 was repeated except that 3-mercaptopropyltriethoxysilane was replaced with KH-550 silane coupling agent.
Comparative example 3
Comparative example 3 provides a nylon composite, differing from example 3 in that: the procedure of example 3 was repeated except that 3-mercaptopropyltriethoxysilane was replaced with a KH-560 silane coupling agent.
Comparative example 4
Comparative example 4 provides a nylon composite, differing from example 3 in that: the procedure of example 3 was repeated except that no coupling agent was added.
And (3) performance testing: the nylon-based composite materials prepared in the examples 1-8 and the comparative examples 1-4 are respectively put into a constant temperature drying oven to be dried for 3 hours at 110 ℃, then are subjected to sample preparation on a 90T injection molding machine, are cooled and placed for 24 hours, and then are tested, and the performance detection results are shown in Table 1.
With the following test criteria:
(1) thermal conductivity (λ): testing according to ASTM E-1461 standard method under 80 deg.C and sample thickness of 2 mm;
(2) tensile strength: tested according to ISO 527-1/-2 standard method, at 23 ℃ and 2 mm/min;
(3) bending strength: testing according to ISO 178 standard method under 23 deg.C and 2 mm/min;
(4) impact strength of the simply supported beam: the test was carried out according to ISO 179/1eU standard method.
TABLE 1 Performance test results of thermally conductive nylon-based composites
It is apparent from the performance test results in table 1 that the high graphite filled heat conductive nylon-based composite material without coupling agent (comparative example 4) has excellent heat conductivity, and due to the addition of a large amount of flow improver, the melt flow rate performance is relatively high, but the mechanical properties are low, and the application requirements of large heat dissipation elements cannot be met. And adding a coupling agent KH550 and KH560 system without mercaptopropyl groups to prepare the high-graphite filled heat-conducting nylon-based composite material (comparative examples 2-3), compared with a system without coupling agent (comparative example 4), the mechanical property of the composite material is improved, but the heat conducting property and the melt flow rate of the composite material are reduced, and the composite material is characterized in that the melt flow rate of the composite material is greatly reduced from 26.5g/10min to 13.5g/10min, so that the problem of rubber shortage of a product in the injection molding process of a molded product is obvious, and the subsequent assembly quality and the service life of the molded product are directly influenced.
By adopting the technical scheme of the invention, the high-graphite filled heat-conducting nylon-based composite material containing the mercaptopropyl coupling agent (example 3) is added, and the heat-conducting performance and the mechanical performance of the composite material are improved, particularly the mechanical performance is greatly improved, compared with a system without the coupling agent, the melt flow rate is basically not influenced, and the problem of glue shortage of products is avoided when the heat-radiating molded products are processed by injection molding. Compared with other coupling agents, the thiopropyl-containing coupling agent has the advantages that on one hand, the interface layer formed between the nylon matrix and the inorganic filler (graphite powder and glass fiber) has low thermal resistance, and on the other hand, the thiopropyl-containing coupling agent plays a good role of a bridge between the nylon matrix and the inorganic filler, so that the inorganic filler can be better dispersed and combined between the nylon matrix, a firmer and more compact heat-conducting network passage is formed, the heat-conducting property of the composite material is improved, and the mechanical property of the composite material is also ensured; furthermore, the mercaptopropyl-containing coupling agent and the flow improver have good compatibility and are mutually synergistic, so that the comprehensive performance of the high-graphite filled heat-conducting nylon-based composite material is ensured.
In order to better verify the heat dissipation effect of the high-thermal-conductivity nylon-based composite material, the high-thermal-conductivity nylon-based composite material of embodiment 3 is injection-molded to form a small fin radiator, and the heat dissipation effect is compared with that of a 6063 aluminum radiator with the same structure. The verification method comprises the following steps: the heat dissipation effect of the radiators made of the two materials on the alumina ceramic heating sheet is monitored by using an infrared thermal imager and a temperature measuring instrument, and a heat dissipation imaging photo (figure 1) and a heat rise curve (figure 2) of the radiators on the heating sheet are obtained.
As seen from the thermal imaging photograph in fig. 1, the thermal imaging area (i.e., imaging area in fig. 1) when the heat dissipation of the heat sink formed by the nylon-based composite material with high thermal conductivity is balanced is equivalent to the thermal imaging area (i.e., imaging area in fig. 1) when the heat dissipation of the heat sink is balanced by the 6063 aluminum heat sink. As seen from the temperature rise curve of fig. 2, when the heat dissipation temperature of the heating plate is balanced by using the 6063 aluminum heat sink, the temperature of the heating plate is 41.5 ℃, while when the heat dissipation temperature of the heating plate is balanced by using the heat sink formed by using the high thermal conductivity nylon-based composite material of the present invention, the temperature of the heating plate is 44.9 ℃, which is only 3.3 ℃ higher than the former, and the heat sink can be directly used as an aluminum heat sink.
The above embodiments are provided only for illustrating the present invention and not for limiting the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and therefore all equivalent technical solutions should also fall within the scope of the present invention, and should be defined by the claims.
Claims (10)
1. The high-thermal-conductivity nylon-based composite material is characterized by comprising the following components in parts by weight:
25-60 parts of nylon resin,
30-65 parts of graphite powder,
0.3 to 2 parts of coupling agent containing mercaptopropyl,
5-15 parts of glass fiber;
the mercaptopropyl-containing coupling agent is one or more of gamma-mercaptopropyl-trimethoxysilane, 3-mercaptopropyl-triethoxysilane, 3-mercaptopropyl-methyldiethoxysilane, 3-mercaptopropyl-dimethylethoxysilane, gamma-mercaptopropyl-dimethoxymethylsilane, 2-mercaptopropyl-trimethoxysilane, 2-mercaptopropyl-triethoxysilane and gamma-mercaptopropyl-methoxysilane.
2. The nylon-based composite material of claim 1, wherein the nylon resin is at least one of PA6, PA66, PA 6/66.
3. The nylon-based composite material with high thermal conductivity of claim 1, wherein the graphite powder is flake graphite, spherical graphite or a mixture of the flake graphite and the spherical graphite.
4. The nylon-based composite material with high thermal conductivity according to claim 3, wherein the flake graphite has a mesh size of 100 to 1000 mesh, and the spherical graphite has a mesh size of 100 to 1000 mesh.
5. The high thermal conductivity nylon-based composite material according to claim 1, comprising the following components in parts by weight:
30-40 parts of nylon resin,
50-65 parts of graphite powder,
0.5-2 parts of coupling agent containing mercaptopropyl,
5-15 parts of glass fiber,
0.5-1 part of a flow improver;
the graphite powder is a compound of crystalline flake graphite and spherical graphite, and the weight ratio of the crystalline flake graphite to the spherical graphite in the compound is 1: 3-3: 1.
6. The nylon-based composite material with high thermal conductivity according to claim 5, wherein the graphite powder is a compound of 100-mesh crystalline flake graphite and 1000-mesh spherical graphite in a weight ratio of 1: 1-3: 1.
7. The high thermal conductivity nylon-based composite material according to claim 5, wherein the nylon resin has a relative viscosity of 1.8 to 2.4.
8. The nylon-based composite material of claim 6, wherein the flow improver is one or more selected from the group consisting of TR063A, dendritic polymer, and hyperbranched resin.
9. A method for preparing the high thermal conductive nylon-based composite material according to any one of claims 1 to 8, comprising the steps of: proportionally adding the raw materials into a mixer for mixing, adding the mixed materials into a feed hopper of a double-screw extruder, and carrying out melt blending, extrusion and granulation by the same-direction double-screw extruder to obtain granules, wherein the granulation adopts an air cooling hot cutting granulation process.
10. A molded article, characterized in that it is made of the highly thermally conductive nylon-based composite material according to any one of claims 1 to 8.
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