CN111393838A - High-strength electric-conductive heat-conductive nylon composite material and preparation method thereof - Google Patents
High-strength electric-conductive heat-conductive nylon composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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Abstract
The invention relates to the technical field of high polymer materials, and provides a high-strength electric and heat conductive nylon composite material and a preparation method thereof, aiming at solving the problem that the traditional electric and heat conductive nylon composite material is poor in processability, mechanical property and heat conductivity, wherein the high-strength electric and heat conductive nylon composite material is prepared from the following components in parts by weight: 50-100 parts of PA6 microspheres, 10-50 parts of PA6-12 microspheres, 1-6 parts of crystalline flake graphite and 2-5.0 parts of spherical graphite, wherein the mass ratio of the crystalline flake graphite to the spherical graphite is 3/2-2/1. The conductive nylon composite material with the isolation structure is prepared by adopting a mechanical blending and compression molding manner, so that the conductive performance of the material can be remarkably improved under the condition of lower conductive filler content; the electric and heat conductive fillers with different dimensions are adopted for compounding, and the nanoscale spherical graphite can fill gaps caused by the crystalline flake graphite, so that the mechanical property of the composite material is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-strength electric-conduction heat-conduction nylon composite material and a preparation method thereof.
Background
The conductive polymer composite materials (CPCs) are polymer composite material systems with conductive functions, which are prepared by taking polymer materials as matrixes and adding conductive fillers. The method can meet the application requirements of various fields by changing the types of the polymer matrix and the conductive filler and improving the processing conditions and the like while maintaining the excellent characteristics of the polymer material. Meanwhile, the conductive polymer composite material has attracted much attention due to its low cost, simple processing technology and suitability for large-scale production. The PA6 is an engineering plastic with excellent performance, has the advantages of good mechanical property, strong wear resistance, solvent resistance, corrosion resistance, self-lubrication, good processability and the like, and is applied to the fields of mechanical manufacture, packaging industry, electronic communication, automobile industry and the like. However, in many practical application occasions, certain requirements are also required for the conductivity of the nylon composite material, so that the construction of the conductive nylon composite material has important significance.
Among them, direct melt blending of nylon matrix and conductive filler is the simplest method for preparing CPCs, but it is often necessary to add more conductive filler to obtain satisfactory results. Too much conductive filler increases the melt viscosity of the composite material, so that the processability is reduced, and the application and industrial development of the CPCs are restricted. Research shows that the amount of the conductive filler can be remarkably reduced by building an isolation structure at a polymer interface through regulating and controlling the distribution of the conductive filler. However, the existence of the isolation structure makes the conductive filler dispersed at the polymer interface have a barrier effect on the diffusion of polymer molecular chains, so that the mechanical properties of the conductive polymer composite material are poor. Therefore, how to construct the isolated conductive structure and ensure that the composite material has good mechanical properties needs to be further researched. In addition, the conductive material often can produce certain heat in the use, and if the heat can not be eliminated in time, the use precision and the service life of the product can be obviously influenced, so that the development of the high-strength conductive nylon composite material with excellent heat conductivity has important significance.
Disclosure of Invention
The invention provides a high-strength electric and heat conductive nylon composite material with excellent mechanical property and heat conductive property, aiming at overcoming the problem of poor processability, mechanical property and heat conductive property of the traditional electric conductive nylon composite material.
The invention also provides a preparation method of the high-strength electric-conduction and heat-conduction nylon composite material, and the method adopts a mechanical blending and compression molding mode to prepare the electric-conduction nylon composite material with the isolation structure, so that the electric conductivity of the material can be obviously improved under the condition of low content of the electric-conduction filler.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-strength electric-conductive heat-conductive nylon composite material is prepared from the following components in parts by weight:
50-100 parts of PA6 microspheres,
10-50 parts of PA6-12 microspheres,
1 to 6 parts of flake graphite,
2 to 5.0 parts of spherical graphite,
the mass ratio of the crystalline flake graphite to the spherical graphite is 3/2-2/1.
Preferably, the PA6 microspheres are prepared from caprolactam (C L) and Polystyrene (PS) in a volume ratio of 70:30 by in-situ anionic polymerization.
Preferably, the PA6-12 microspheres are prepared from caprolactam (C L), laurolactam (LL) and Polystyrene (PS) in a volume ratio of 56:24:20 by in-situ anionic polymerization.
Preferably, the scale graphite has a size of 5 to 10 μm.
Preferably, the spherical graphite has a size of 400 to 600 nm.
According to the invention, the electric and heat conductive fillers with different dimensions are compounded, and the nanoscale spherical graphite can fill gaps caused by micron-level crystalline flake graphite, so that the mechanical property of the composite material is improved.
A preparation method of a high-strength electric-conduction heat-conduction nylon composite material comprises the following steps:
(1) according to the proportion, mechanically mixing PA6 microspheres, PA6-12 microspheres, crystalline flake graphite and spherical graphite at a high speed to obtain PA6/PA 6-12/graphite composite particles; in the step, the graphite is uniformly coated on the surfaces of the PA6 microspheres and the PA6-12 microspheres under the action of mechanical force;
(2) and (2) carrying out compression molding on the PA6/PA 6-12/graphite composite particles prepared in the step (1), and cooling to room temperature to obtain the high-strength electric-conduction heat-conduction nylon composite material.
In the invention, the PA6-12 microspheres with lower melting point are used as the binder, and at the mould pressing temperature, the PA6 microspheres are still solid particles, while the PA6-12 microspheres are in a molten state, which is beneficial to improving the interface bonding force among the components in the material, thereby improving the mechanical property of the material.
Preferably, in the step (1), the PA6 microspheres and the PA6-12 microspheres are dried in vacuum at 50-80 ℃ for 12-24 hours before high-speed mechanical mixing.
Preferably, in the step (1), a high-speed stirrer is adopted for high-speed mechanical mixing, the stirring speed of the high-speed stirrer is 800-1000 r/min, and the stirring time is 5-10 min.
Preferably, in the step (2), the compression molding temperature is 180-230 ℃, and the compression molding pressure is 5-15 MPa. The molding temperature is too low, so that the PA6-12 microspheres are still in a solid state, and the bonding force between the PA6 microspheres and graphite cannot be improved; too high a molding temperature can cause the PA6 microspheres to be in a molten state, so that the isolation structure is collapsed, and the conductive network is difficult to form; too low molding pressure can cause too many pores in the nylon composite material, increase interfaces, decrease the conductivity and mechanical properties of the material, and too high can cause graphite to permeate into a nylon matrix to damage a conductive network.
Preferably, in the step (2), the time for the compression molding is 5 to 10 min.
Therefore, the invention has the following beneficial effects:
(1) the conductive nylon composite material with the isolation structure is prepared by adopting a mechanical blending and compression molding manner, so that the conductive performance of the material can be remarkably improved under the condition of lower conductive filler content;
(2) according to the invention, the electric and heat conductive fillers with different dimensions are compounded, and the nanoscale spherical graphite can fill gaps caused by crystalline flake graphite, so that the mechanical property of the composite material is improved;
(3) in the invention, PA6-12 with a lower melting point is used as a binder, PA6 is still solid particles at the mould pressing temperature, and PA6-12 is in a molten state, so that the interface bonding force among the components in the material is favorably improved, and the mechanical property of the material is improved.
Drawings
FIG. 1 shows DSC temperature rise curves of PA6 microspheres (a) and PA6-12 microspheres (b).
FIG. 2 is a scanning electron microscope image of a sample of the high strength, electrical and thermal conductive nylon composite material prepared in example 1.
FIG. 3 is a scanning electron micrograph of a nylon composite sample prepared in comparative example 7.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
In the following examples of the invention, the PA6 microspheres are prepared from caprolactam and polystyrene by an in-situ anion polymerization method according to a volume ratio of 70: 30; the PA6-12 microsphere is prepared from caprolactam, laurolactam and polystyrene according to the volume ratio of 56:24:20 by an in-situ anion polymerization method.
Example 1
(1) Carrying out vacuum drying on PA6 microspheres and PA6-12 microspheres at 80 ℃ for 12h, and mechanically mixing 50.0g of PA6 microspheres, 50.0g of PA6-12 microspheres, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at the speed of 1000r/min for 5min to prepare PA6/PA 6-12/graphite composite particles;
(2) and (2) hot-pressing the composite particles prepared in the step (1) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the high-strength, electric-conduction and heat-conduction nylon composite material, wherein a scanning electron microscope image of the composite material is shown in figure 2.
Example 2
(1) Carrying out vacuum drying on PA6 microspheres and PA6-12 microspheres at 70 ℃ for 18h, and mechanically mixing 60.0g of PA6 microspheres, 40.0g of 40.0gPA6-12 microspheres, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at the speed of 800r/min for 10min to prepare PA6/PA 6-12/graphite composite particles;
(2) and (2) carrying out hot pressing on the composite particles prepared in the step (1) at 180 ℃ and 15MPa for 10min, and cooling to room temperature to obtain the composite material.
Example 3
(1) Carrying out vacuum drying on PA6 microspheres and PA6-12 microspheres for 24h at 60 ℃, and mechanically mixing 70.0gPA6 microspheres, 30.0gPA6-12 microspheres, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at the speed of 900r/min for 8min to prepare PA6/PA 6-12/graphite composite particles;
(2) and (2) carrying out hot pressing on the composite particles prepared in the step (1) at 230 ℃ and 5MPa for 5min, and cooling to room temperature to obtain the composite material.
Example 4
(1) Carrying out vacuum drying on PA6 microspheres and PA6-12 microspheres at 80 ℃ for 12h, and mechanically mixing 80.0g of PA6 microspheres, 20.0g of PA6-12 microspheres, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at the speed of 800r/min for 8min to prepare PA6/PA 6-12/graphite composite particles;
(2) and (2) carrying out hot pressing on the composite particles prepared in the step (1) at 210 ℃ and 12MPa for 8min, and cooling to room temperature to obtain the composite material.
Example 5
(1) Carrying out vacuum drying on PA6 microspheres and PA6-12 microspheres at 80 ℃ for 12h, and mechanically mixing 90.0g of PA6 microspheres, 10.0g of PA6-12 microspheres, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at the speed of 900r/min for 6min to prepare PA6/PA 6-12/graphite composite particles;
(2) and (2) carrying out hot pressing on the composite particles prepared in the step (1) at 220 ℃ and under 10MPa for 10min, and cooling to room temperature to obtain the composite material.
Comparative example 1
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the microspheres in vacuum at 80 ℃ for 12 hours;
(2) compression molding: and (2) carrying out hot pressing on the PA6 microspheres prepared in the step (1) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the PA6 plate.
Comparative example 2 (flake graphite to spherical graphite mass ratio 1/1)
(1) PA6 and PA6-12 microspheres are prepared by weighing quantitative C L and PS, preparing PA6 microspheres by in-situ anion polymerization, weighing quantitative C L, LL and PS, preparing PA6-12 microspheres by in-situ anion polymerization, and drying PA6 and PA6-12 microspheres for 12 hours in vacuum at 80 ℃;
(2) preparation of conductive composite particles: mechanically mixing 50.0gPA6, 50.0gPA6-12, 2.5g of crystalline flake graphite and 2.5g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA6/PA 6-12/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
COMPARATIVE EXAMPLE 3 (without addition of spheroidal graphite)
(1) PA6 and PA6-12 microspheres are prepared by weighing quantitative C L and PS, preparing PA6 microspheres by in-situ anion polymerization, weighing quantitative C L, LL and PS, preparing PA6-12 microspheres by in-situ anion polymerization, and drying PA6 and PA6-12 microspheres for 12 hours in vacuum at 80 ℃;
(2) preparation of conductive composite particles: mechanically mixing 50.0gPA6, 50.0gPA6-12 and 5.0g of crystalline flake graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA6/PA 6-12/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
Comparative example 4 (without flake graphite)
(1) PA6 and PA6-12 microspheres are prepared by weighing quantitative C L and PS, preparing PA6 microspheres by in-situ anion polymerization, weighing quantitative C L, LL and PS, preparing PA6-12 microspheres by in-situ anion polymerization, and drying PA6 and PA6-12 microspheres for 12 hours in vacuum at 80 ℃;
(2) preparation of conductive composite particles: mechanically mixing 50.0gPA6, 50.0gPA6-12 and 5.0g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA6/PA 6-12/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
COMPARATIVE EXAMPLE 5 (without addition of PA6-12 microspheres and spheroidal graphite)
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the PA6 microspheres at 80 ℃ for 12 hours in vacuum;
(2) preparation of conductive composite particles: mechanically mixing 100.0gPA6 and 1.0g of flake graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA 6/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
Comparative example 6 (without PA6-12 microspheres and flake graphite)
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the PA6 microspheres at 80 ℃ for 12 hours in vacuum;
(2) preparation of conductive composite particles: mechanically mixing 100.0gPA6 and 3.0g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA 6/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
Comparative example 7 (No PA6-12 microsphere added, weight ratio of flake graphite to spherical graphite 3/2)
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the PA6 microspheres at 80 ℃ for 12 hours in vacuum;
(2) preparation of conductive composite particles: mechanically mixing 100.0g of 100.0gPA6, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA 6/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material, wherein a scanning electron microscope image of the composite material is shown in figure 2.
Comparative example 8 (No PA6-12 microsphere added, weight ratio of flake graphite to spherical graphite 4/3)
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the PA6 microspheres at 80 ℃ for 12 hours in vacuum;
(2) preparation of conductive composite particles: mechanically mixing 100.0g of 100.0gPA6, 4.0g of flake graphite and 3.0g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA 6/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
Comparative example 9 (No PA6-12 microsphere added, weight ratio of flake graphite to spherical graphite 2/1)
(1) Preparing PA6 microspheres, namely weighing quantitative C L and PS, preparing PA6 microspheres by an in-situ anion polymerization method, and drying the PA6 microspheres at 80 ℃ for 12 hours in vacuum;
(2) preparation of conductive composite particles: mechanically mixing 100.0g of 100.0gPA6, 6.0g of flake graphite and 3.0g of spherical graphite in a high-speed stirrer at the speed of 1000r/min for 5min to prepare PA 6/graphite composite particles;
(3) compression molding: and (3) carrying out hot pressing on the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the composite material.
Mechanical property and electric and heat conduction performance tests are carried out on the samples of the examples 1-5 and the comparative examples 1-9, and the test results are shown in the following table 1:
TABLE 1 measurement results of examples 1 to 5 and comparative examples 1 to 9
As can be seen from the data of comparative example 1 in Table 1, the pure PA6 material has poor mechanical properties and thermal conductivity and has no conductivity. The thermal conductivity data of comparative examples 5-9 show that the electrical conductivity and thermal conductivity of the PA6 composite material are significantly improved with the addition of graphite, and the PA6 composite material has certain electrical conductivity and thermal conductivity, and the thermal conductivity data of comparative examples 2-4 show that the heat conductivity of the composite material is further improved due to the compounding of the flake crystalline flake graphite and the three-dimensional spherical graphite. In addition, the mechanical property data of the comparative example 7 and the examples 1 to 5 show that the tensile strength and the notch impact strength of the composite material can be obviously improved by adding the PA6-12 microspheres.
FIG. 1 is a DSC temperature rise curve of PA6 microsphere (a) and PA6-12 microsphere (b), and it can be seen from FIG. 1 that PA6 microsphere has two melting points, which are respectively about 210 ℃ and 220 ℃, while PA6-12 microsphere only has one melting point and about 180 ℃, and the melting point of PA6-12 microsphere is obviously lower than that of PA6 microsphere, therefore, when we select a molding temperature of about 200 ℃, PA6 is still a solid particle, and PA6-12 is in a molten state, which is beneficial to improving the interfacial bonding force among the components in the material, thereby improving the mechanical properties of the material.
Fig. 2 and 3 are scanning electron micrographs of the samples of example 1 and comparative example 7, respectively, and it can be seen from fig. 2 and 3 that the nylon microspheres and the microspheres and graphite in example 1 are tightly bonded, and the microspheres and graphite in comparative example 7 have distinct boundaries and have a few voids, so that the tightly bonded sample of example 1 has better mechanical properties than the sample of comparative example 7.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The high-strength electric-conduction heat-conduction nylon composite material is characterized by being prepared from the following components in parts by weight:
50-100 parts of PA6 microspheres,
10-50 parts of PA6-12 microspheres,
1 to 6 parts of flake graphite,
2 to 5.0 parts of spherical graphite,
the mass ratio of the crystalline flake graphite to the spherical graphite is 3/2-2/1.
2. The nylon composite material as claimed in claim 1, wherein the PA6 microspheres are prepared from caprolactam and polystyrene by in-situ anionic polymerization at a volume ratio of 70: 30.
3. The nylon composite material as claimed in claim 1, wherein the PA6-12 microspheres are prepared from caprolactam, laurolactam and polystyrene by in-situ anionic polymerization at a volume ratio of 56:24: 20.
4. The nylon composite material as claimed in claim 1, wherein the scale graphite has a size of 5-10 μm.
5. The nylon composite material as claimed in claim 1, wherein the spherical graphite has a size of 400-600 nm.
6. A preparation method of a high-strength electric-conductive heat-conductive nylon composite material as claimed in any one of claims 1 to 5, characterized by comprising the following steps:
(1) according to the proportion, mechanically mixing PA6 microspheres, PA6-12 microspheres, crystalline flake graphite and spherical graphite at a high speed to obtain PA6/PA 6-12/graphite composite particles;
(2) and (2) carrying out compression molding on the PA6/PA 6-12/graphite composite particles prepared in the step (1), and cooling to room temperature to obtain the high-strength electric-conduction heat-conduction nylon composite material.
7. The preparation method of the high-strength electric-conductive heat-conductive nylon composite material as claimed in claim 6, wherein in the step (1), the PA6 microspheres and the PA6-12 microspheres are dried in vacuum at 50-80 ℃ for 12-24 h before high-speed mechanical mixing.
8. The preparation method of the high-strength electric-conductive heat-conductive nylon composite material as claimed in claim 6, wherein in the step (1), the high-speed stirrer is adopted for high-speed mechanical mixing, the stirring speed of the high-speed stirrer is 800-1000 r/min, and the stirring time is 5-10 min.
9. The preparation method of the high-strength electricity-conducting heat-conducting nylon composite material as claimed in claim 6, wherein in the step (2), the compression molding temperature is 180-230 ℃, and the compression molding pressure is 5-15 MPa.
10. The preparation method of the high-strength electric-conductive heat-conductive nylon composite material according to claim 6, wherein in the step (2), the compression molding time is 5-10 min.
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