CN111393838B - High-strength electric-conduction heat-conduction nylon composite material and preparation method thereof - Google Patents
High-strength electric-conduction heat-conduction nylon composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of high polymer materials, and provides a high-strength electric-conduction heat-conduction nylon composite material and a preparation method thereof, wherein the high-strength electric-conduction heat-conduction nylon composite material is prepared from the following components in parts by weight: 50-100 parts of PA6 microsphere, 10-50 parts of PA6-12 microsphere, 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. According to the invention, the conductive nylon composite material with the isolation structure is prepared by adopting a mechanical blending and compression molding mode, so that the conductive performance of the material can be obviously improved under the condition of lower conductive filler content; the composite material is compounded by adopting conductive and heat-conductive fillers with different dimensions, and the nano-scale 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
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 be applied to various fields by changing the types of the polymer matrix and the conductive filler, improving the processing conditions and the like while maintaining the excellent characteristics of the polymer material. Meanwhile, the conductive polymer composite material has been widely focused because of low cost, simple processing technology and suitability for mass production. The PA6 is engineering plastic with excellent performance, has the advantages of good mechanical property, strong wear resistance, solvent resistance, corrosion resistance, self-lubricating property, good processability and the like, and is applied to the fields of mechanical manufacturing, packaging industry, electronic communication, automobile industry and the like. However, in many practical applications, there is a certain requirement on the conductivity, so it is of great importance to construct the conductive nylon composite material.
Among them, direct melt blending of nylon matrix with conductive filler is the simplest method for preparing CPCs, but more conductive filler is often needed to obtain satisfactory effect. And too much conductive filler can increase the melt viscosity of the composite material, so that the processability is reduced, which restricts the application and industrial development of CPCs. It has been found that by controlling the distribution of the conductive filler, the filler usage can be significantly reduced by constructing an isolation structure at the polymer interface. However, the existence of the isolation structure makes the conductive filler dispersed at the polymer interface play a role in preventing 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 while ensuring good mechanical properties of the composite material needs to be further studied. In addition, the conductive material often generates certain heat in the use process, and if the heat cannot be timely eliminated, the use precision and the service life of the product can be obviously affected, so that the development of the high-strength conductive nylon composite material with excellent heat conduction performance has important significance.
Disclosure of Invention
The invention provides a high-strength electric-conduction heat-conduction nylon composite material with excellent mechanical property and heat-conduction property, which aims to solve the problem that the traditional electric-conduction nylon composite material is poor in processability, mechanical property and heat-conduction property.
The invention also provides a preparation method of the high-strength electric-conduction heat-conduction nylon composite material, which adopts a mechanical blending and compression molding mode to prepare the electric-conduction nylon composite material with the isolation structure, so that the electric conduction performance of the material can be obviously improved under the condition of lower electric-conduction filler content.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a high-strength electric-conduction heat-conduction nylon composite material is prepared from the following components in parts by weight:
50 to 100 parts of PA6 microsphere,
10 to 50 parts of PA6-12 microsphere,
1 to 6 parts of crystalline 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 microsphere is prepared from Caprolactam (CL) and Polystyrene (PS) by in situ anionic polymerization according to a volume ratio of 70:30.
Preferably, the PA6-12 microsphere is prepared from Caprolactam (CL), laurolactam (LL) and Polystyrene (PS) by in situ anionic polymerization according to a volume ratio of 56:24:20.
Preferably, the scale graphite has a size of 5 to 10 μm.
Preferably, the size of the spherical graphite is 400 to 600nm.
According to the invention, the electric conduction and heat conduction fillers with different dimensions are adopted for compounding, and the nanoscale spherical graphite can fill gaps caused by the micron-scale flake graphite, so that the mechanical property of the composite material is improved.
The preparation method of the high-strength electric-conduction heat-conduction nylon composite material comprises the following steps:
(1) According to the proportion, the PA6 microsphere, the PA6-12 microsphere, the crystalline flake graphite and the spherical graphite are mechanically mixed at a high speed to obtain PA6/PA 6-12/graphite composite particles; in the step, graphite is uniformly coated on the surfaces of the PA6 microsphere and the PA6-12 microsphere under the action of mechanical force;
(2) And (3) 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.
The PA6-12 microsphere with a lower melting point is used as the binder, and the PA6 microsphere is still solid particles at the molding temperature, and the PA6-12 microsphere is in a molten state, so that the interfacial binding force among all components in the material is improved, and the mechanical property of the material is improved.
Preferably, in step (1), the PA6 microspheres and PA6-12 microspheres are dried in vacuo at 50-80℃for 12-24 hours prior to high speed mechanical mixing.
Preferably, in the step (1), high-speed mechanical mixing is performed by a high-speed mixer, wherein the stirring speed of the high-speed mixer is 800-1000 r/min, and the stirring time is 5-10 min.
Preferably, in the step (2), the temperature of the compression molding is 180-230 ℃, and the pressure of the compression molding is 5-15 MPa. The too low molding temperature can lead the PA6-12 microsphere to be still in a solid state, so that the bonding force between the PA6 microsphere and graphite cannot be improved; too high a molding temperature can cause PA6 microspheres to be in a molten state as well, thereby causing collapse of the isolation structure and making formation of the conductive network difficult; too low molding pressure can cause excessive pores in the nylon composite material, increased interfaces, reduced conductivity and mechanical properties of the material, and too high molding pressure can cause graphite to permeate into a nylon matrix to damage a conductive network.
Preferably, in the step (2), the time of the compression molding is 5 to 10 minutes.
Therefore, the invention has the following beneficial effects:
(1) According to the invention, the conductive nylon composite material with the isolation structure is prepared by adopting a mechanical blending and compression molding mode, so that the conductive performance of the material can be obviously improved under the condition of lower conductive filler content;
(2) According to the invention, the conductive and heat-conductive fillers with different dimensions are adopted for compounding use, and the nano-scale spherical graphite can fill gaps caused by the 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 adopted as the binder, and at the molding temperature, PA6 is still solid particles, and PA6-12 is in a molten state, so that the interfacial binding force among all components in the material is improved, and the mechanical property of the material is improved.
Drawings
FIG. 1 shows DSC temperature rise curves of PA6 microsphere (a) and PA6-12 microsphere (b).
FIG. 2 is a scanning electron microscope image of a high strength, electrically and thermally conductive nylon composite sample prepared in example 1.
FIG. 3 is a scanning electron microscope image of a nylon composite sample prepared in comparative example 7.
Detailed Description
The technical scheme of the invention is further specifically described below through specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
In the following examples of the invention, the PA6 microsphere is prepared from caprolactam and polystyrene by in situ anionic polymerization according to a volume ratio of 70:30; the PA6-12 microsphere is prepared from caprolactam, laurolactam and polystyrene by in-situ anionic polymerization according to the volume ratio of 56:24:20.
Example 1
(1) Vacuum drying PA6 microsphere and PA6-12 microsphere at 80deg.C for 12 hr, mechanically mixing 50.0g of PA6 microsphere, 50.0g of PA6-12 microsphere, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at 1000r/min for 5min to obtain PA6/PA6-12/graphite composite particles;
(2) And (3) 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 heat-conduction nylon composite material, wherein a scanning electron microscope diagram of the high-strength electric-conduction heat-conduction nylon composite material is shown as figure 2.
Example 2
(1) Vacuum drying PA6 microsphere and PA6-12 microsphere at 70deg.C for 18 hr, mechanically mixing 60.0g of PA6 microsphere, 40.0g of PA6-12 microsphere, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at 800r/min for 10min to obtain PA6/PA6-12/graphite composite particles;
(2) And (3) hot-pressing 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) Vacuum drying PA6 microsphere and PA6-12 microsphere at 60deg.C for 24 hr, mechanically mixing 70.0g PA6 microsphere, 30.0g PA6-12 microsphere, 3.0g flake graphite and 2.0g spherical graphite in a high-speed mixer at 900r/min for 8min to obtain PA6/PA 6-12/graphite composite particle;
(2) And (3) hot-pressing 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) Vacuum drying PA6 microsphere and PA6-12 microsphere at 80deg.C for 12 hr, mechanically mixing 80.0g of PA6 microsphere, 20.0g of PA6-12 microsphere, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at 800r/min for 8min to obtain PA6/PA6-12/graphite composite particles;
(2) And (3) hot-pressing the composite particles prepared in the step (1) at 210 ℃ and 12MPa for 8min, and cooling to room temperature to prepare the composite material.
Example 5
(1) Vacuum drying PA6 microsphere and PA6-12 microsphere at 80deg.C for 12 hr, mechanically mixing 90.0g of PA6 microsphere, 10.0g of PA6-12 microsphere, 3.0g of flake graphite and 2.0g of spherical graphite in a high-speed mixer at 900r/min for 6min to obtain PA6/PA6-12/graphite composite particles;
(2) And (3) hot-pressing the composite particles prepared in the step (1) at 220 ℃ and 10MPa for 10min, and cooling to room temperature to obtain the composite material.
Comparative example 1
(1) Preparation of PA6 microspheres: weighing quantitative CL and PS, preparing PA6 microsphere by in-situ anion polymerization method, and vacuum drying at 80deg.C for 12 hr;
(2) Compression molding: and (3) hot-pressing the PA6 microsphere prepared in the step (1) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to obtain the PA6 board.
Comparative example 2 (flake graphite to spherical graphite mass ratio 1/1)
(1) Preparation of PA6 and PA6-12 microspheres: weighing quantitative CL and PS and preparing PA6 microspheres by an in-situ anion polymerization method; quantitative CL, LL, PS are weighed and PA6-12 microspheres are prepared by an in situ anionic polymerization method. Vacuum drying PA6 and PA6-12 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 50.0g of PA6, 50.0g of PA6-12, 2.5g of crystalline flake graphite and 2.5g of spherical graphite are mechanically mixed in a high-speed mixer at the speed of 1000r/min for 5min to prepare PA6/PA 6-12/graphite composite particles;
(3) Compression molding: and (3) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 3 (no spherical graphite added)
(1) Preparation of PA6 and PA6-12 microspheres: weighing quantitative CL and PS and preparing PA6 microspheres by an in-situ anion polymerization method; quantitative CL, LL, PS are weighed and PA6-12 microspheres are prepared by an in situ anionic polymerization method. Vacuum drying PA6 and PA6-12 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 50.0g of PA6, 50.0g of PA6-12 and 5.0g of crystalline flake graphite are mechanically mixed for 5min at the speed of 1000r/min in a high-speed stirrer to prepare PA6/PA 6-12/graphite composite particles;
(3) Compression molding: and (3) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 4 (non-added flake graphite)
(1) Preparation of PA6 and PA6-12 microspheres: weighing quantitative CL and PS and preparing PA6 microspheres by an in-situ anion polymerization method; quantitative CL, LL, PS are weighed and PA6-12 microspheres are prepared by an in situ anionic polymerization method. Vacuum drying PA6 and PA6-12 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 50.0g of PA6, 50.0g of PA6-12 and 5.0g of spherical graphite are mechanically mixed for 5min at the speed of 1000r/min in a high-speed stirrer to prepare PA6/PA 6-12/graphite composite particles;
(3) Compression molding: and (3) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 5 (no PA6-12 microsphere and spherical graphite added)
(1) Preparation of PA6 microspheres: quantitative CL, PS were weighed and PA6 microspheres were prepared by in situ anionic polymerization. Vacuum drying PA6 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 100.0g of PA6 and 1.0g of crystalline flake graphite are mechanically mixed for 5min at the speed of 1000r/min in a high-speed stirrer to prepare PA 6/graphite composite particles;
(3) Compression molding: and (3) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 6 (no PA6-12 microsphere and flake graphite added)
(1) Preparation of PA6 microspheres: quantitative CL, PS were weighed and PA6 microspheres were prepared by in situ anionic polymerization. Vacuum drying PA6 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 100.0g of PA6 and 3.0g of spherical graphite are mechanically mixed for 5min at the speed of 1000r/min in a high-speed stirrer to prepare PA 6/graphite composite particles;
(3) Compression molding: and (3) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 7 (no PA6-12 microsphere added, 3/2 of the mass ratio of crystalline flake graphite to spherical graphite)
(1) Preparation of PA6 microspheres: quantitative CL, PS were weighed and PA6 microspheres were prepared by in situ anionic polymerization. Vacuum drying PA6 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 100.0g of PA6, 3.0g of crystalline flake graphite and 2.0g of spherical graphite are mechanically mixed 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) hot-pressing 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 diagram of the composite material is shown in figure 2.
Comparative example 8 (no PA6-12 microsphere added, the mass ratio of crystalline flake graphite to spherical graphite is 4/3)
(1) Preparation of PA6 microspheres: quantitative CL, PS were weighed and PA6 microspheres were prepared by in situ anionic polymerization. Vacuum drying PA6 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 100.0g of PA6, 4.0g of crystalline flake graphite and 3.0g of spherical graphite are mechanically mixed 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) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
Comparative example 9 (no PA6-12 microsphere added, the mass ratio of crystalline flake graphite to spherical graphite is 2/1)
(1) Preparation of PA6 microspheres: quantitative CL, PS were weighed and PA6 microspheres were prepared by in situ anionic polymerization. Vacuum drying PA6 microsphere at 80deg.C for 12 hr;
(2) Preparation of conductive composite particles: 100.0g of PA6, 6.0g of crystalline flake graphite and 3.0g of spherical graphite are mechanically mixed 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) hot-pressing the composite particles prepared in the step (2) at 200 ℃ and 10MPa for 8min, and cooling to room temperature to prepare the composite material.
The samples of inventive examples 1 to 5 and comparative examples 1 to 9 were subjected to mechanical properties and electric and thermal conductivity tests, and the test results are shown in 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 does not have electrical conductivity. It can be seen from the heat conductivity data of comparative examples 5 to 9 that the conductivity and the heat conductivity of the PA6 composite material are obviously improved along with the addition of graphite, and the PA6 composite material has certain conductivity and heat conductivity, and meanwhile, the heat conductivity data of comparative examples 2 to 4 can be used for further improving the heat conductivity of the composite material by compounding flake crystalline graphite and three-dimensional spherical graphite. In addition, as can be seen from the mechanical property data of comparative example 7 and examples 1-5, the addition of PA6-12 microspheres can significantly improve the tensile strength and notched impact strength of the composite.
The DSC heating curves of the PA6 microsphere (a) and the PA6-12 microsphere (b) are shown in the figure 1, wherein the PA6 microsphere has two melting points, namely about 210 ℃ and 220 ℃, and the PA6-12 microsphere only has one melting point and about 180 ℃, and the melting point of the PA6-12 microsphere is obviously lower than that of the PA6 microsphere, so that when the die pressing temperature of about 200 ℃ is selected, the PA6 is still solid particles, and the PA6-12 is in a molten state, thereby being beneficial to improving the interfacial bonding force among all components in the material and further improving the mechanical property of the material.
Fig. 2 and 3 are scanning electron microscope images of samples of example 1 and comparative example 7, respectively, and it can be seen from fig. 2 and 3 that the nylon microspheres of example 1 and the microspheres and graphite are tightly bonded, while the microspheres of comparative example 7 and the microspheres and graphite have obvious boundaries and have a small gap, so that the sample of example 1, which is tightly bonded, has better mechanical properties than the sample of comparative example 7.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the invention in any way, but other variations and modifications are possible without departing from the technical solution described 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,
1-6 parts of crystalline flake graphite,
2-5.0 parts of spherical graphite,
the mass ratio of the crystalline flake graphite to the spherical graphite is 3/2-2/1;
the high-strength electric conduction heat conduction nylon composite material is prepared by the following steps:
(1) According to the proportion, the PA6 microsphere, the PA6-12 microsphere, the crystalline flake graphite and the spherical graphite are mechanically mixed at a high speed to obtain PA6/PA 6-12/graphite composite particles;
(2) Compression molding the PA6/PA 6-12/graphite composite particles prepared in the step (1), and cooling to room temperature to obtain a high-strength electric-conduction heat-conduction nylon composite material;
in the step (2), the temperature of compression molding is 180-230 ℃, and the pressure of compression molding is 5-15 MPa.
2. The nylon composite with high strength and electric conductivity and heat conduction according to claim 1, wherein the PA6 microsphere is prepared from caprolactam and polystyrene by in-situ anionic polymerization according to a volume ratio of 70:30.
3. The high-strength electric-conduction heat-conduction nylon composite material according to claim 1, wherein the PA6-12 microsphere is prepared from caprolactam, laurolactam and polystyrene according to a volume ratio of 56:24:20 by an in-situ anionic polymerization method.
4. The nylon composite material with high strength and electric conduction and heat conduction as claimed in claim 1, wherein the size of the crystalline flake graphite is 5-10 μm.
5. The nylon composite material with high strength and electric conduction and heat conduction as claimed in claim 1, wherein the size of the spherical graphite is 400-600 nm.
6. A method for preparing the high-strength electric-conduction heat-conduction nylon composite material as claimed in any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) According to the proportion, the PA6 microsphere, the PA6-12 microsphere, the crystalline flake graphite and the spherical graphite are mechanically mixed at a high speed to obtain PA6/PA 6-12/graphite composite particles;
(2) And (3) 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 method for preparing the high-strength, electric-conduction and heat-conduction nylon composite material according to claim 6, wherein in the step (1), before high-speed mechanical mixing, the PA6 microspheres and the PA6-12 microspheres are dried in vacuum for 12-24 hours at 50-80 ℃.
8. The method for preparing the high-strength, electric-conduction and heat-conduction nylon composite material according to claim 6, wherein in the step (1), high-speed mechanical mixing is performed by adopting a high-speed stirrer, the stirring speed of the high-speed stirrer is 800-1000 r/min, and the stirring time is 5-10 min.
9. The method for preparing a high-strength, electrically and thermally conductive nylon composite material according to claim 6, wherein in the step (2), the temperature of compression molding is 180-230 ℃, and the pressure of compression molding is 5-15 mpa.
10. The method for preparing the high-strength, electric-conduction and heat-conduction nylon composite material according to claim 6, wherein in the step (2), the compression molding time is 5-10 min.
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