CN110628213B - PA11/RGO composite material and preparation method thereof - Google Patents

PA11/RGO composite material and preparation method thereof Download PDF

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CN110628213B
CN110628213B CN201911085024.0A CN201911085024A CN110628213B CN 110628213 B CN110628213 B CN 110628213B CN 201911085024 A CN201911085024 A CN 201911085024A CN 110628213 B CN110628213 B CN 110628213B
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graphene
composite material
die
rgo
rgo composite
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CN110628213A (en
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王志强
王泓珺
李迎春
李洁
王文生
赵涛
张才渡
燕晓辉
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North University of China
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances

Abstract

The invention relates to a PA11/RGO composite material and a preparation method thereof, belonging to the technical field of composite materials. The PA11/RGO composite material is prepared by uniformly mixing pretreated PA11 and pretreated graphene to obtain a mixed material; then heating the upper die and the lower die of the molding press and the die to 200-220 ℃, taking out the die, placing the mixed material into the die, and then placing the die into the molding press for compression molding to obtain the product, wherein: the amount of the graphene is 0.05-1% of the mass of PA 11. According to the invention, graphene (RGO) particles are introduced into PA11, so that the crystal structure of PA11 is changed from an alpha crystal form to a gamma crystal form, the crystallization behavior of PA11 is promoted, the impact property, dielectric constant, magnetic permeability and return loss of PA11 are improved, and the production cost of PA11 is reduced.

Description

PA11/RGO composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a PA11/RGO composite material and a preparation method thereof.
Background
Due to the rapid development of human social productivity and scientific technology, people continuously put forth various new requirements on materials to meet the current needs, and the appearance of polymers and polymer composite materials gradually replaces other materials. Nylon is a thermoplastic polymer that can withstand loads and is used very widely in machinery. In the beginning of the 20 th century, DuPont in the United states first developed research and then achieved industrial production. Nylon is a new pet in the materials field at that time, has a plurality of excellent properties, and a plurality of products related to the nylon are developed and widely favored.
Nylon 11(PA11), the first commercial product of arkema, france, was produced in 1950. It has excellent physical and chemical properties, low water absorption, high size stability and other features, and is used in automobile, aviation, electronic and military industry.
PA11 is limited in practical use due to its low impact strength and high cost. Therefore, the PA11 needs to be modified to prepare a high-performance PA11 composite material, so that the production cost can be reduced, the application range can be expanded, and the excellent performance can be fully exerted.
The present application has been made for the above reasons.
Disclosure of Invention
Aiming at the problems or defects in the prior art, the invention aims to provide a PA11/RGO composite material and a preparation method thereof. According to the invention, the PA11/RGO composite material is prepared by adopting a compression molding process, and the graphene (RGO) particles are introduced into the PA11, so that the crystal structure of PA11 is changed from an alpha crystal form to a gamma crystal form, the crystallization behavior of PA11 is promoted, the impact property, dielectric constant, magnetic permeability and return loss of PA11 are improved, and the production cost of PA11 is reduced.
In order to achieve the above purpose of the present invention, the technical solution adopted by the present invention is as follows:
a preparation method of PA11/RGO composite material specifically comprises the following steps:
(1) pretreatment of
(a) Pretreatment of graphene: adding graphene into an ethanol water solution, performing ultrasonic dispersion and freeze drying treatment, and drying to obtain pretreated graphene;
(b) pretreatment of PA 11: putting the PA11 in a vacuum drying oven for drying treatment to obtain pretreated PA 11;
(2) uniformly mixing the PA11 pretreated in the step (1) and the pretreated graphene according to the proportion to obtain a mixed material; and then heating the upper die and the lower die of the molding press and the die to 200-220 ℃, taking out the die, placing the mixed material into the die, and then placing the die into the molding press for compression molding to obtain the PA11/RGO composite material.
Specifically, the specific process of the press forming in the step (2) is as follows: firstly, putting a die into a molding press, preheating for 2-6 min without pressurization, and melting the mixed material; then applying a pressure of 10-14 MPa, and performing air release once every 1-3 min, and pressurizing for 4-8; and taking out the mold and cooling.
Further, the drying treatment of the PA11 in the step (b) is baking for 10-15 hours at the temperature of 60-100 ℃. More preferably, the drying treatment is baking at 80 ℃ for 12 h.
Further, the amount of the graphene used in the step (2) is 0.05-1% of the mass of the PA 11.
More preferably, the amount of the graphene used in the step (2) is 0.2-1% of the mass of the PA 11.
More preferably, the amount of the graphene used in the step (2) is 0.2% by mass of the PA 11.
The second purpose of the invention is to provide the PA11/RGO composite material prepared by the preparation method of the PA11/RGO composite material.
Compared with the prior art, the PA11/RGO composite material and the preparation method thereof have the following beneficial effects:
(1) the PA11/RGO composite material prepared by the invention is prepared by a compression molding preparation method. Compression molding's advantage is easy operation, and the loss of raw materials is little, can not cause the loss of too much loss raw materials little, can not cause too much loss.
(2) XRD test results show that: the infrared spectrum characteristic peak of the PA 11/graphene composite material has no obvious change, which indicates that no new chemical bond is introduced by adding the graphene.
(3) The mechanical property test result shows that the impact property of the composite material is improved after the graphene is added. When the content of the graphene reaches 0.2%, the impact strength reaches the maximum and is 29.41KJ/m2At this time, the impact is strongThe degree is 2.3 times that of pure PA 11. In addition, as the content of graphene increases, the tensile strength and elongation at break of the composite material tend to increase first and then decrease. When the content of the graphene reaches 0.8%, the tensile strength and the elongation at break both reach the maximum, at the moment, the tensile strength reaches 35.9MPa, which is 1.7 times that of pure PA11, and the elongation at break is 26.4%, which is 3.6 times that of pure PA 11. Moreover, the addition of the graphene also improves the bending strength and the bending modulus of the composite material.
(4) Non-isothermal crystallization kinetics studies showed that: the addition of the graphene has an influence on nucleation and crystal growth of non-isothermal crystallization of PA11/, and when a small amount of graphene is added into PA11/, the non-isothermal crystallization process of the composite material is facilitated.
(5) The dielectric property research shows that: return loss R of PA11/RGO composite with increasing RGO contentLShowing a tendency to decrease first and then increase. And is minimized at an RGO content of 0.4 wt%. Therefore, the RGO content of 0.4 wt% can better satisfy the electromagnetic matching characteristic, so that more frequency bands of electromagnetic waves enter the composite material to be attenuated and lost.
Drawings
FIG. 1 is a process flow diagram of the present invention for preparing PA11/RGO composite.
FIG. 2 is an infrared spectrum of the PA11/RGO composite material and pure PA11 as raw materials prepared in example 1 of the present invention.
FIG. 3 is an XRD spectrum of PA11/RGO composite and pure PA11 prepared in example 1 of the present invention.
FIG. 4 is a scanning electron microscope image of an impact cross section of pure PA11 and PA11/RGO composite material; wherein (a) is a pure PA11 scanning electron micrograph; (b) scanning electron micrographs of the PA 11/graphene composite material prepared in example 1 of the invention.
FIG. 5 is a graph showing the change in impact strength of PA11/RGO composite materials prepared in examples 1-5 of the present invention.
FIG. 6 is a graph showing the change in tensile strength and elongation at break of PA11/RGO composite materials prepared in examples 1 to 5 of the present invention.
FIG. 7 is a graph showing the change in flexural strength and flexural modulus of PA11/RGO composite materials prepared in examples 1 to 5 of the present invention.
FIG. 8 is a graph of X (T) to t curves of PA11/RGO composite materials prepared in examples 1-5 of the present invention at different cooling rates.
FIG. 9 is a graph showing the dielectric constant of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions.
FIG. 10 is a graph showing the dielectric loss of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions.
FIG. 11 is a comparison graph of magnetic storage coefficients of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions.
FIG. 12 is a graph showing the comparison of magnetic loss coefficients of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions.
FIG. 13 shows the return loss R of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditionsLCompare the figures.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
The invention is to dry nylon 11 and graphene in advance and mix them uniformly according to the prescribed formulation ratio. The temperature preset by the molding press is raised, and both the press plate and the mold need to be heated. And after the specified temperature is reached, taking out the pressing plate and the die, uniformly spreading the material in the die, and coating silicone oil on the die and the pressing plate so as to be convenient for demoulding. And after all the materials are ready, putting the materials into a mould press for press forming. After the pressure is adjusted to a certain value, under the combined action of temperature and pressure, the mold is filled with the material (the gas is released for several times in the manufacturing process, the gas in the mold cavity is removed), and after the mold press is cooled to the room temperature, the template can be taken out, namely the PA 11/graphene composite material.
The performance test method of the composite material prepared by the invention comprises the following steps:
1. notched impact strength
Notched impact strength was tested according to GB/T1843-2008.
And cutting a V-shaped standard notch with the depth of 2mm on the universal test sampling machine, measuring the residual width and thickness of the sample strip, performing idle striking on the cantilever beam impact tester before testing, and recording energy loss data during the idle striking. And then testing the notched impact strength of the cantilever beam in a normal temperature environment.
2. Tensile strength and elongation at break
Tensile bars were tested in a room temperature (25 ℃) environment using a universal tester according to GB/T1040-2006 standard. The original gauge length of the test is 25mm, and the stretching speed is 50 mm/min.
3. Static bending Strength and bending modulus
The bent specimens were tested in an environment at room temperature (25 ℃) in accordance with GB/T9341-2008 using a universal tester. The test speed was 2 mm/min.
4. Fourier Infrared Spectroscopy testing
The test used a fourier transform infrared spectrometer. Selecting a flat surface of a sample as a test surface, and setting a scanning range to be 4000cm-1～650cm-1Resolution was set to 4cm-1。
X-ray diffractometer
An X-ray diffractometer was used. Voltage: 40 KV; current: 100 mA; cu target (k α 1 wavelength 0.15408 nm); scanning speed: 4 degree/min; scanning diffraction angle range: 2 theta is 5-60 degrees.
6. Scanning electron microscope
The test was carried out using a scanning electron microscope model SU-5000, manufactured by Hitachi high tech.
Selecting the standard sample after impact, sawing the standard sample into a test sample with a lower height, adhering the test sample on an aluminum disc by using conductive rubber, and performing gold plating treatment by using a vacuum gold plating instrument. Under a nitrogen atmosphere, an accelerating voltage of 20KV is used, and the image is photographed after the observation and scanning treatment by an electron scanning microscope.
7. Non-isothermal crystallization performance test: weigh 5mg of sample to differentialScanning Calorimeter (DSC) aluminum crucible, and adding Al2O3Taking a reference substance, and protecting with high-purity nitrogen at the flow rate of 50 mL/min; heating the sample from 100 ℃ to 230 ℃ at the heating rates of 2.5 ℃/min, 5 ℃/min, 10 ℃/min, 20 ℃/min and 40 ℃/min respectively, keeping the temperature for 10min, eliminating the thermal history, then rapidly cooling to 50 ℃ at the cooling rates of 2.5 ℃/min, 5 ℃/min, 10 ℃/min, 20 ℃/min and 40 ℃/min respectively, after the crystallization is finished, heating to 250 ℃ at the heating rate of 10 ℃/min, and recording all DSC curves for analysis.
Example 1
The preparation method of the PA11/RGO (0.2%) composite material of the embodiment specifically includes the following steps:
(1) pretreatment of
(a) Pretreatment of graphene: adding 15g of graphene into an ethanol aqueous solution with the volume fraction of 70%, performing ultrasonic dispersion for 20min, then performing freeze drying for 2h at the temperature of minus 40 ℃, and then placing in a drying oven at the temperature of 60 ℃ for baking for 2h to obtain pretreated graphene;
(b) pretreatment of PA 11: putting the PA11 in a vacuum drying oven at 80 ℃ for drying treatment for 12h to obtain pretreated PA 11;
(2) respectively weighing 200g of PA11 pretreated in the step (1) and 0.4g of pretreated graphene, uniformly mixing to obtain a mixed material, heating an upper die, a lower die and a die of a flat vulcanizing machine to 210 ℃, taking out the die, weighing 180g of the mixed material, putting the mixed material into the die, flattening, putting the die on the flat vulcanizing machine, preheating for 4min without pressurization, and melting the material; then 12MPa pressure is applied, air is released every 2min, and the pressure is increased for 6 min. The mold was then removed and placed on a cold press for cooling. In order to prevent the pressed plate from warping and deforming, the pressed plate can be taken out after being cooled to about 50 ℃ by a cold press. Test specimens were cut out using a cutting machine.
Example 2
The preparation method of the PA11/RGO (0.4%) composite material of the embodiment is basically the same as that of the embodiment 1, and the difference is only that: the amount of the graphene pretreated in step (2) of this embodiment is 0.8.
Example 3
The preparation method of the PA11/RGO (0.6%) composite material of the embodiment is basically the same as that of the embodiment 1, and the difference is only that: the amount of graphene pretreated in step (2) of this example was 1.2 g.
Example 4
The preparation method of the PA11/RGO (0.8%) composite material of the embodiment is basically the same as that of the embodiment 1, and the difference is only that: the amount of graphene pretreated in step (2) of this example was 1.6 g.
Example 5
The preparation method of the PA11/RGO (1.0%) composite material of the embodiment is basically the same as that of the embodiment 1, and the difference is only that: the amount of graphene pretreated in step (2) of this example was 2 g.
Structural characterization and performance test
Infrared, XRD testing of (mono) PA11/RGO composites
FIG. 2 is an infrared spectrum of the PA11/RGO composite material and pure PA11 as raw materials prepared in example 1 of the present invention. As can be seen from FIG. 2, at 3302cm-1In the presence of a stretch characteristic band of N-H, 2854cm-1And 2925cm-1The C-H stretching vibration characteristic peak is shown at 1636cm-1The characteristic band of C ═ O is amide band I, 1555cm-1The N-H bending vibration peak is an amide II band, and the N-H bending vibration peak is a characteristic peak of PA 11. The infrared spectrum characteristic peak of the PA 11/graphene composite material has no obvious change, which indicates that no new chemical bond is introduced by adding the graphene.
FIG. 3 is an XRD spectrum of PA11/RGO composite and pure PA11 prepared in example 1 of the present invention. As can be seen from fig. 3, pure PA11 has two diffraction peaks at 2 θ of 10 ° and 20.5 °, and the crystal structure at this time corresponds to the γ crystal form of PA11, and the two diffraction peaks correspond to the (001) and (100) crystal planes of PA11, respectively. After the graphene is added into PA11, the diffraction peak is split, and two diffraction peaks appear at 20.1 degrees and 22.37 degrees respectively, which shows that the crystal form of PA11 is changed, the diffraction peak at 22.37 degrees corresponds to the (010, 110) crystal face of the PA11 alpha crystal form, and the addition of the graphene plays a role in heterogeneous nucleation and changes the crystal form of PA 11.
FIG. 4 is a scanning electron microscope image of an impact cross section of pure PA11 and PA11/RGO composite material; wherein (a) is a pure PA11 scanning electron micrograph; (b) scanning electron micrographs of the PA 11/graphene composite material prepared in example 1 of the invention. It can be seen from fig. 4 (a) that the impact section of PA11 is smoother, indicating that PA11 is brittle fracture. Fig. 4 (b) shows that the impact section of the PA 11/graphene composite material is uneven, because the addition of graphene causes silver streaks to be generated when the sample is impacted by external force, which improves the impact strength of the material.
Mechanical property analysis of (II) PA11/RGO composite material
FIG. 5 is a graph showing the change of impact strength of the PA 11/graphene composite material prepared in embodiments 1-5 of the present invention. As can be seen from fig. 5, the impact performance of the composite material is improved after the graphene is added. When the content of the graphene reaches 0.2%, the impact strength reaches the maximum and is 29.41KJ/m2The impact strength at this time was 2.3 times that of pure PA 11. Thereafter, the higher the graphene content, the lower the impact strength of the composite. This is probably because when the content of graphene is low, graphene can be uniformly dispersed in a PA11 matrix, and when the graphene is subjected to an external force, the graphene acts as a stress concentrator, so that silver streaks are induced, a large amount of energy is absorbed, and the impact strength of the material is improved. When the content of the graphene is too high, the agglomeration phenomenon is easy to occur, so that the rigidity of the composite material is improved, and the impact strength is reduced.
Fig. 6 is a graph showing the change of the tensile strength and the elongation at break of the PA 11/graphene composite material prepared in embodiments 1 to 5 of the present invention. Observing the change of the curve in fig. 6, it can be seen that the tensile strength and the elongation at break of the composite material show a trend of increasing first and then decreasing as the content of the graphene increases. When the content of the graphene reaches 0.8%, the tensile strength and the elongation at break both reach the maximum, at the moment, the tensile strength reaches 35.9MPa, which is 1.7 times that of pure PA11, and the elongation at break is 26.4%, which is 3.6 times that of pure PA 11. After which the graphene content increases and the tensile properties of the material begin to decrease. The reason is that the graphene is uniformly dispersed in the PA11 at low content and is tightly combined with the matrix, and external stress can be transferred to the graphene, so that the tensile strength is improved, and the filler is easy to agglomerate at high content, so that the tensile strength is reduced. The optimum formulation for both properties is different because the force patterns for impact and tensile testing are not the same.
Fig. 7 is a graph showing the change of flexural strength and flexural modulus of the PA 11/graphene composite material prepared in examples 1 to 5 of the present invention. It can be seen from fig. 7 that the addition of graphene improves the flexural strength and flexural modulus of the composite material. The elastic modulus is the ratio of stress to strain, and after the graphene is added into a PA11 matrix, the material can reach the same deformation amount and needs a larger external force action, so that the rigidity of the material is improved, and the phenomenon of increasing the bending strength and the bending modulus is shown.
(III) non-isothermal crystallization kinetics study of composite Material
FIG. 8 is a graph of X (T) to t curves of PA11/RGO composite materials prepared in examples 1-5 of the present invention at different cooling rates. As can be seen from fig. 8, as the cooling rate is reduced, the time for the composite material to complete crystallization gradually increases, which shows that as the cooling rate is reduced, the nucleation rate of the composite material is reduced, and the nucleation rate directly affects the crystallization rate, so the time for completing crystallization increases. In addition, as can be seen from table 1, in the crystallization stage, the range of the Avrami index, i.e., the n value, of pure PA11/, is 2.73 to 3.69, while the range of the Avrami index value of PA11// graphene composite material is 1.10 to 2.60, which indicates that the addition of graphene has an influence on the nucleation and crystal growth of the non-isothermal crystallization of PA 11/. Compared with the crystallization rate constant Zc1 value of the composite material at the same cooling rate, when the content of graphene is gradually increased, the rate constant shows a trend that the rate constant is increased and then reduced, which shows that when a small amount of graphene is added into PA 11/the non-isothermal crystallization process of the composite material is facilitated.
TABLE 1 values of n, Zt and ZC for Nylon 11/graphene composites at different cooling rates
Figure GDA0003201567410000071
Figure GDA0003201567410000081
(IV) dielectric Property study
FIG. 9 is a graph showing the dielectric constant of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions. As can be seen from FIG. 9, the dielectric constant ε' of the PA11/RGO composite material increased with the increase in RGO content. At a frequency of 30Mhz, the dielectric constant ε 'of an RGO content of 0.2 wt% was 4.07, and ε' of a content of 1.0 wt% was increased to 5.29. The addition of graphene proved to produce dielectric polarization in the PA11 matrix. Under the action of an electric field, the carrier fluid generates interface polarization at a phase interface of two phases, and the dielectric property of the material is increased.
FIG. 10 is a graph showing the dielectric loss of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions. As can be seen from FIG. 10, the dielectric loss ε' of the PA11/RGO composite increased with increasing RGO content. The dielectric loss epsilon' of the composite material has a peak value in the frequency range of 2000-2500 Mfz. Due to the unique two-dimensional structure of the graphene, the graphene has a large specific surface area, so that the scattering and multiple reflection of electromagnetic waves can be promoted, and the wave absorbing performance of the graphene is improved; meanwhile, when the graphene is prepared by a reduction method, defects and residual oxygen-containing functional groups generated on the graphene sheet layer are easy to generate polarization relaxation and electric dipole relaxation under the action of an external electric field, so that the dielectric loss is increased.
FIG. 11 is a comparison graph of magnetic storage coefficients of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions. As shown in FIG. 11, the magnetic storage coefficient μ' of the PA11/RGO composite increased substantially with increasing RGOwt% content. At a frequency of 30MHz, the magnetic storage coefficient μ' increased from 5.09 at 0.2 wt% to 7.22 at 1.0 wt%. It can be seen that the greater the amount of RGO, the better the improvement in the magnetic storage capacity of the material.
FIG. 12 is a graph showing the comparison of magnetic loss coefficients of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditions. As shown in FIG. 12, the magnetic loss coefficient μ' of the PA11/RGO composite material substantially increases with the increase of RGOwt%, but the RGO content of 0.4 wt% shows a peak in the frequency range of 3800 to 5000 MHz.
FIG. 13 shows the return loss R of PA11/RGO composite materials prepared in examples 1-5 of the present invention under different frequency conditionsLCompare the figures. As shown in FIG. 13, the return loss R of the PA11/RGO compositeLAt the low frequency range of 0-3000 MHz, the return loss R of the RGO to the composite materialLThe influence is not great. However, in the high-frequency band of 3000-6000 MHz, the return loss R of the PA11/RGO composite material is increased along with the increase of the RGO contentLShowing a tendency to decrease first and then increase. And is minimized at an RGO content of 0.4 wt%. Therefore, the RGO content of 0.4 wt% can better satisfy the electromagnetic matching characteristic, so that more frequency bands of electromagnetic waves enter the composite material to be attenuated and lost.

Claims (4)

1. A preparation method of PA11/RGO composite material is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) pretreatment of
(a) Pretreatment of graphene: adding graphene into an ethanol water solution, performing ultrasonic dispersion and freeze drying treatment, and drying to obtain pretreated graphene;
(b) pretreatment of PA 11: putting the PA11 in a vacuum drying oven for drying treatment to obtain pretreated PA 11;
(2) uniformly mixing the PA11 pretreated in the step (1) and the pretreated graphene according to the proportion to obtain a mixed material; heating the upper die and the lower die of the molding press and the die to 200-220 ℃, taking out the die, placing the mixed material into the die, and then placing the die into the molding press for compression molding to obtain the PA11/RGO composite material; the specific process of the compression molding is as follows: firstly, putting a die into a molding press, preheating for 2-6 min without pressurization, and melting the mixed material; then applying a pressure of 10-14 MPa, and performing air release once every 1-3 min, and pressurizing for 4-8; taking out the mold and cooling; the amount of the graphene is 0.05-1% of the mass of PA 11.
2. The method of claim 1, wherein the PA11/RGO composite material is prepared by: the drying treatment of the PA11 in the step (b) is specifically baking for 10-15 hours at the temperature of 60-100 ℃.
3. The method of claim 1, wherein the PA11/RGO composite material is prepared by: the amount of the graphene used in the step (2) is 0.2-1% of the mass of PA 11.
4. PA11/RGO composite material prepared by the preparation method of PA11/RGO composite material as claimed in any one of claims 1 to 3.
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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN106977912A (en) * 2017-03-20 2017-07-25 复旦大学 A kind of preparation method of the graphene complex of nylon 6 with good electric conductivity and thermodynamic property
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Publication number Priority date Publication date Assignee Title
CN106977912A (en) * 2017-03-20 2017-07-25 复旦大学 A kind of preparation method of the graphene complex of nylon 6 with good electric conductivity and thermodynamic property
CN107739504A (en) * 2017-10-19 2018-02-27 青岛万林橡塑科技有限公司 A kind of preparation method of graphene/nylon enhancing composite

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