CN113912884A - Preparation method of flexible electromagnetic shielding polyether sulfone membrane - Google Patents
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- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
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Abstract
The invention discloses a preparation method of a flexible electromagnetic shielding polyether sulfone film, which comprises the following steps: embedding conductive nanoparticles and magnetic nanoparticles; and step two, preparing the flexible electromagnetic shielding polyether sulfone film. The invention has the following beneficial effects: the flexible electromagnetic shielding polyether sulfone film prepared by the invention can weaken reflection to electromagnetic waves, enhance absorption and improve electromagnetic shielding performance in the application of the electromagnetic shielding field.
Description
Technical Field
The invention relates to the technical field of preparation of electromagnetic shielding films, in particular to a preparation method of a flexible electromagnetic shielding polyether sulfone film.
Background
With the wide application of electronic communication technology in various fields, the pollution of electromagnetic radiation generated thereby is increased, and therefore, there is a need to develop a high-performance electromagnetic interference (EMI) shielding material to suppress or reduce the interference of electromagnetic radiation on electronic components and human health threats. Polymer-based electromagnetic shielding composites have gained much attention in the industry and scientific community by virtue of their light weight, corrosion resistance, and ease of processing. However, the existing polymer-based electromagnetic shielding composite material has the defects of low conductivity, poorer electromagnetic shielding performance than a metal material and the like. How to improve the electromagnetic shielding performance through the structural design becomes a key scientific and technical problem which needs to be solved urgently.
The porous polymer-based electromagnetic shielding composite material is prepared by taking a polymer matrix as a supporting material and loading a conductive filler. Compared with homogeneous and isolated polymer-based electromagnetic shielding composite materials, the porous polymer-based electromagnetic shielding composite material has the advantages of low cost, low density, good toughness and the like. Meanwhile, the porous structure is more beneficial to multiple reflection and absorption of electromagnetic waves, and the electromagnetic shielding performance of the electromagnetic shielding material can be further improved. At present, the commonly used method for preparing the porous polymer-based electromagnetic shielding composite material comprises the following steps: foaming, sol-gel and templating. Foaming methods include chemical foaming and physical foaming. The EMI SE improvement effect of the pure foaming on the polymer-based composite material is limited and is far from the EMI SE of the metal material, and other methods are combined in practical application to further improve the electromagnetic shielding performance of the composite material. The sol-gel method is that conductive filler and polymer monomer are uniformly mixed in a liquid phase to form a stable sol system, three-dimensional network structure gel is formed in a solution through hydrolysis, condensation reaction, hydrogen bond action and the like, and the porous polymer-based electromagnetic shielding composite material is prepared through freeze drying. But the network connection strength of the polymer matrix is not high, so that the mechanical property of the polymer matrix is poor. The template method is to uniformly attach conductive fillers on the surface of a porous framework by taking a porous polymer matrix as the framework through chemical plating, Chemical Vapor Deposition (CVD), electrostatic adsorption and other modes to prepare the porous polymer-based electromagnetic shielding composite material. If the composite material prepared by the method deforms in the using process, the conductive filler of the composite material is easy to fall off from the polymer matrix framework, so that the electromagnetic shielding performance and the service life of the composite material are influenced.
Disclosure of Invention
The invention provides a preparation method of a flexible electromagnetic shielding polyether sulfone film, which can solve the technical problems related to the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a flexible electromagnetic shielding polyethersulfone membrane comprises the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with the molecular weight of 500-5000 and the anhydride content of 20-50 wt%, distilled water and sodium hydroxide are heated and stirred for 1-24 hours at the temperature of 40-60 ℃ according to a certain mass ratio to form a uniform SMA salt solution;
respectively mixing the conductive nanoparticles and the magnetic nanoparticles with an SMA salt solution in a mass ratio of 1: 0.11-0.8, adding the mixture into 50-250 ml of distilled water, carrying out ultrasonic treatment for a certain time, then placing the mixture in a vacuum drying oven at 60-80 ℃ for drying until the weight is constant to obtain embedded nanoparticles, and placing the embedded nanoparticles in a ball mill for grinding for 2-8 hours;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 1-40 wt%, placing SMA with the molecular weight of 100000-300000 in the sodium hydroxide solution for 1-24 h, collecting SMA sodium salt in a manner of filtering and cleaning at the same time, and drying the collected SMA sodium salt in a vacuum drying box at the temperature of 60-100 ℃;
dissolving polyether sulfone, the ground nano particles, the dried SMA sodium salt, polyethylene glycol, dimethylacetamide and distilled water in a certain mass ratio at the temperature of 70-100 ℃ for 24-48 hours to obtain a uniform casting solution;
defoaming the casting solution for 3-10 h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, standing in the air for 1-5 min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the obtained composite membrane out of the coagulating bath, and then placing the composite membrane in distilled water for cleaning to obtain the flexible electromagnetic shielding polyether sulfone membrane.
As a preferable improvement of the present invention, in the first step, the mass ratio of the SMA, the distilled water and the sodium hydroxide is 35: 65: 11.
as a preferable improvement of the present invention, in the step one, the conductive nanoparticles include carbon nanotubes, reduced graphene and MXene, and the magnetic nanoparticles include magnetic MOF.
As a preferred improvement of the present invention, in the step one, the time for the ultrasonic treatment is 30 min.
In the second step, the mass ratio of the polyether sulfone to the ground nanoparticles to the dried SMA sodium salt to the polyethylene glycol to the dimethylacetamide to the distilled water is 12 (1-3) to 2:8 (70-72) to 5.
The invention has the following beneficial effects: the flexible electromagnetic shielding polyether sulfone film prepared by the invention can weaken reflection to electromagnetic waves, enhance absorption and improve electromagnetic shielding performance in the application of the electromagnetic shielding field.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a schematic view of a film scraping process according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides a preparation method of a flexible electromagnetic shielding polyether sulfone film, which comprises the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with the molecular weight of 500-5000 and the anhydride content of 20-50 wt%, distilled water and sodium hydroxide are heated and stirred for 1-24 hours at the temperature of 40-60 ℃ according to a certain mass ratio to form a uniform SMA salt solution;
respectively mixing conductive nanoparticles and magnetic nanoparticles (MOF) with an SMA salt solution in a mass ratio of 1: 0.11-0.8, adding the mixture into 50-250 ml of distilled water, carrying out ultrasonic treatment for a certain time, then placing the mixture in a vacuum drying oven at 60-80 ℃ for drying until the weight is constant to obtain embedded nanoparticles, and placing the embedded nanoparticles in a ball mill for grinding for 2-8 hours;
it is further noted that the mass ratio of the SMA to the distilled water to the sodium hydroxide is 35: 65: 11; the conductive nanoparticles include Carbon Nanotubes (CNTs), reduced graphene (rGO), and MXene, and the magnetic nanoparticles include magnetic MOFs.
Preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 1-40 wt%, placing SMA with the molecular weight of 100000-300000 in the sodium hydroxide solution for 1-24 h, collecting SMA sodium salt in a manner of filtering and cleaning at the same time, and drying the collected SMA sodium salt in a vacuum drying box at the temperature of 60-100 ℃;
dissolving polyether sulfone, the ground nano particles, the dried SMA sodium salt, polyethylene glycol, dimethylacetamide and distilled water in a certain mass ratio at the temperature of 70-100 ℃ for 24-48 hours to obtain a uniform casting solution;
defoaming the casting solution for 3-10 h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, standing in the air for 1-5 min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles, which can be seen in fig. 1;
and taking the obtained composite membrane out of the coagulating bath, and then placing the composite membrane in distilled water for cleaning to remove the residual solvent, thereby obtaining the flexible electromagnetic shielding polyethersulfone membrane.
Specifically, the mass ratio of the polyether sulfone to the ground nano particles to the dried SMA sodium salt to the dried polyethylene glycol to the dried dimethylacetamide to the distilled water is 12 (1-3) to 2:8 (70-72) to 5.
The following describes in detail a method for preparing a flexible electromagnetic shielding polyethersulfone membrane provided by the invention with specific examples.
Example 1
The embodiment 1 provides a preparation method of a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA having a molecular weight of 1000 and an acid anhydride content of 50 wt% was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11, heating and stirring for 8 hours at the temperature of 40 ℃ to form uniform SMA salt solution;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: 0.11, adding the mixture into 100 ml of distilled water for ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 60 ℃ for drying to constant weight to obtain embedded nanoparticles, and finally placing the embedded nanoparticles in a ball mill for grinding for 4 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a 10 wt% sodium hydroxide solution, then placing SMA with the molecular weight of 140000 in the sodium hydroxide solution for 4 hours, collecting SMA sodium salt in a manner of filtering and cleaning at the same time, and drying in a vacuum drying oven at the temperature of 60 ℃;
dissolving 12 wt% of polyether sulfone, 0.5 wt% of ground carbon nano-tubes, 0.5 wt% of ground magnetic nano-particles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 72 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 24 hours to obtain a uniform casting solution;
defoaming the casting solution for 4h, coating the casting solution on a glass plate or a non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, standing in the air for 1min, and then putting the glass plate or the non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 2
The embodiment 2 provides a preparation method of a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 2000, an anhydride content of 40 wt%, was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11 is heated and stirred for 16 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: 0.3 of the mass ratio is added into 200 ml of distilled water for ultrasonic treatment for 30min, then the mixture is placed in a vacuum drying oven at 70 ℃ and dried to constant weight to obtain embedded nanoparticles, and finally the embedded nanoparticles are put in a ball mill for grinding for 6 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 20 wt%, then placing SMA with the molecular weight of 200000 in the sodium hydroxide solution for 6 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyether sulfone, 1 wt% of ground carbon nano-tube, 0.5 wt% of ground magnetic nano-particle, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 71.5 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 36 hours to obtain a uniform casting solution;
defoaming the casting solution for 6h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, standing in the air for 3min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 3
The embodiment 3 provides a preparation method of a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 3500 and an anhydride content of 28 wt% was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: the mass ratio of 11 is within the temperature range of 60 ℃, and the uniform SMA salt solution is formed after the mixture is heated and stirred for 24 hours;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: 0.5, adding the mixture into 200 ml of distilled water for ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 80 ℃ for drying to constant weight to obtain embedded nanoparticles, and finally placing the embedded nanoparticles in a ball mill for grinding for 8 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 30 wt%, then placing SMA with the molecular weight of 250000 in the sodium hydroxide solution for 12 hours, collecting SMA sodium salt in a manner of filtering and cleaning at the same time, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyether sulfone, 1.5 wt% of ground carbon nano-tubes, 0.8 wt% of ground magnetic nano-particles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 70.7 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 36 hours to obtain a uniform casting solution;
defoaming the casting solution for 8h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 4
This embodiment 4 provides a method for preparing a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 4800 and an anhydride content of 21 wt% was mixed with distilled water, sodium hydroxide at a ratio of 35: 65: 11 is heated and stirred for 24 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: adding 0.8 mass ratio of the nano particles into 200 ml of distilled water, carrying out ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 80 ℃ for drying until the weight is constant to obtain embedded nano particles, and finally placing the embedded nano particles in a ball mill for grinding for 10 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 40 wt%, then placing SMA with the molecular weight of 300000 in the sodium hydroxide solution for 24 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 90 ℃;
dissolving 12 wt% of polyether sulfone, 2.0 wt% of ground carbon nano-tubes, 1.0 wt% of ground magnetic nano-particles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 70 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 48 hours to obtain a uniform casting solution;
defoaming the casting solution for 10h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 5
This embodiment 5 provides a method for preparing a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 2000, an anhydride content of 40 wt%, was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11 is heated and stirred for 16 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: adding 0.55 mass ratio of the nano particles into 200 ml of distilled water, carrying out ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 70 ℃ for drying until the weight is constant to obtain embedded nano particles, and finally placing the embedded nano particles in a ball mill for grinding for 6 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 20 wt%, then placing SMA with the molecular weight of 200000 in the sodium hydroxide solution for 6 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyether sulfone, 1. wt% of ground carbon nano-tubes, 0.8 wt% of ground magnetic nano-particles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 71.2 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 30 hours to obtain a uniform casting solution;
defoaming the casting solution for 6h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 6
This embodiment 6 provides a method for preparing a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 2000, an anhydride content of 40 wt%, was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11 is heated and stirred for 16 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
respectively mixing reduced graphene oxide (rGO) and magnetic nanoparticles (MOF) with an SMA salt solution in a proportion of 1: adding 0.55 mass ratio of the nano particles into 200 ml of distilled water, carrying out ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 70 ℃ for drying until the weight is constant to obtain embedded nano particles, and finally placing the embedded nano particles in a ball mill for grinding for 6 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 20 wt%, then placing SMA with the molecular weight of 200000 in the sodium hydroxide solution for 6 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyethersulfone, 1 wt% of ground reduced graphene oxide (rGO), 0.8 wt% of ground magnetic nanoparticles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 71.2 wt% of dimethylacetamide and 5 wt% of distilled water at a temperature range of 80 ℃ for 30 hours to obtain a uniform casting solution;
defoaming the casting solution for 6h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Example 7
This embodiment 7 provides a method for preparing a flexible electromagnetic shielding polyethersulfone membrane, which is implemented by the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 2000, an anhydride content of 40 wt%, was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11 is heated and stirred for 16 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
mixing MXene and magnetic nanoparticles (MOF) with an SMA salt solution in a ratio of 1: adding 0.55 mass ratio of the nano particles into 200 ml of distilled water, carrying out ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 70 ℃ for drying until the weight is constant to obtain embedded nano particles, and finally placing the embedded nano particles in a ball mill for grinding for 6 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 20 wt%, then placing SMA with the molecular weight of 200000 in the sodium hydroxide solution for 6 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyethersulfone, 1 wt% of ground MXene, 0.8 wt% of ground magnetic nanoparticles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 71.2 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 30 hours to obtain a uniform casting solution;
defoaming the casting solution for 6h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
Comparative example 1
The construction of the polyethersulfone conductive separation membrane was continued without applying a magnetic field and an electric field during the membrane scraping process according to the preparation method in example 5. The method specifically comprises the following steps:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with a molecular weight of 2000, an anhydride content of 40 wt%, was mixed with distilled water, sodium hydroxide in a ratio of 35: 65: 11 is heated and stirred for 16 hours at the temperature of 50 ℃ to form uniform SMA salt solution;
respectively mixing carbon nano-tubes (CNT) and magnetic nano-particles (MOF) with an SMA salt solution in a ratio of 1: adding 0.55 mass ratio of the nano particles into 200 ml of distilled water, carrying out ultrasonic treatment for 30min, then placing the mixture in a vacuum drying oven at 70 ℃ for drying until the weight is constant to obtain embedded nano particles, and finally placing the embedded nano particles in a ball mill for grinding for 6 h;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 20 wt%, then placing SMA with the molecular weight of 200000 in the sodium hydroxide solution for 6 hours, collecting SMA sodium salt in a manner of suction filtration and cleaning, and drying in a vacuum drying oven at the temperature of 80 ℃;
dissolving 12 wt% of polyethersulfone, 1 wt% of ground carbon nano-tubes (CNT), 0.8 wt% of ground magnetic nano-particles, 2 wt% of SMA sodium salt, 8 wt% of polyethylene glycol, 72 wt% of dimethylacetamide and 5 wt% of distilled water at the temperature of 80 ℃ for 30 hours to obtain a uniform casting solution;
defoaming the casting solution for 6h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, staying in the air for 5min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the prepared composite membrane out of the coagulating bath, placing the composite membrane in distilled water, cleaning to remove residual solvent to obtain the flexible electromagnetic shielding polyether sulfone membrane, and analyzing and detecting.
The performance of the polyethersulfone membrane prepared by the preparation method of the flexible electromagnetic shielding polyethersulfone membrane provided by the above examples 1-7 and comparative example 1 is shown in table 1, and the test method is as follows:
conductivity of the film: the test was performed using a four-probe resistivity tester (ST2258C multifunctional digital four-probe tester, suzhou lattice electronics ltd).
The electromagnetic shielding properties of the film; the test was carried out by the coaxial method using a vector network analyzer (Agilent E5071C) and the film thickness was 0.5 mm.
TABLE 1
It can be seen from examples 1-4 that the electrical conductivity and electromagnetic shielding performance are gradually enhanced with the increase of the conductive nanoparticles CNT and the magnetic nanoparticles MOF. However, example 5 shows that by regulating the compatibility of the casting solution and the dispersion distribution of the nanoparticles therein, it can be achieved that relatively excellent electrical conductivity and electromagnetic shielding performance can be obtained with the addition of a small amount of conductive nanoparticles CNT and magnetic nanoparticles MOF. By using the conductive nanoparticles rGO (example 6) and MXene (example 7) instead of CNT, excellent conductive performance and electromagnetic shielding performance can be obtained under the same formula and process conditions. In addition, as can be seen from comparative example 1, the electromagnetic shielding performance of the prepared film was significantly reduced without applying electric and magnetic fields. The results show that the electric field and the magnetic field can form different gradient distribution in the film by inducing the conductive nano particles and the magnetic nano particles, thereby improving the electromagnetic shielding performance of the film material.
The invention has the following beneficial effects: the flexible electromagnetic shielding polyether sulfone film prepared by the invention can weaken reflection to electromagnetic waves, enhance absorption and improve electromagnetic shielding performance in the application of the electromagnetic shielding field.
While embodiments of the invention have been disclosed above, it is not limited to the applications set forth in the specification and the embodiments, which are fully applicable to various fields of endeavor for which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (5)
1. The preparation method of the flexible electromagnetic shielding polyethersulfone membrane is characterized by comprising the following steps of:
embedding conductive nanoparticles and magnetic nanoparticles;
SMA with the molecular weight of 500-5000 and the anhydride content of 20-50 wt%, distilled water and sodium hydroxide are heated and stirred for 1-24 hours at the temperature of 40-60 ℃ according to a certain mass ratio to form a uniform SMA salt solution;
respectively mixing the conductive nanoparticles and the magnetic nanoparticles with an SMA salt solution in a mass ratio of 1: 0.11-0.8, adding the mixture into 50-250 ml of distilled water, carrying out ultrasonic treatment for a certain time, then placing the mixture in a vacuum drying oven at 60-80 ℃ for drying until the weight is constant to obtain embedded nanoparticles, and placing the embedded nanoparticles in a ball mill for grinding for 2-8 hours;
preparing a flexible electromagnetic shielding polyether sulfone film;
preparing a sodium hydroxide solution with the concentration of 1-40 wt%, placing SMA with the molecular weight of 100000-300000 in the sodium hydroxide solution for 1-24 h, collecting SMA sodium salt in a manner of filtering and cleaning at the same time, and drying the collected SMA sodium salt in a vacuum drying box at the temperature of 60-100 ℃;
dissolving polyether sulfone, the ground nano particles, the dried SMA sodium salt, polyethylene glycol, dimethylacetamide and distilled water in a certain mass ratio at the temperature of 70-100 ℃ for 24-48 hours to obtain a uniform casting solution;
defoaming the casting solution for 3-10 h, coating the casting solution on a glass plate or non-woven fabric by using an automatic film scraping machine with an electric field and magnetic field device, standing in the air for 1-5 min, and then putting the glass plate or non-woven fabric into coagulating bath water for phase exchange to obtain a composite film with gradient distribution of magnetic nanoparticles and conductive nanoparticles;
and taking the obtained composite membrane out of the coagulating bath, and then placing the composite membrane in distilled water for cleaning to obtain the flexible electromagnetic shielding polyether sulfone membrane.
2. The method for preparing a flexible electromagnetic shielding polyethersulfone film as claimed in claim 1, wherein the method comprises the following steps: in the first step, the mass ratio of the SMA to the distilled water to the sodium hydroxide is 35: 65: 11.
3. the method for preparing the flexible electromagnetic shielding polyethersulfone film of claim 1, wherein in the first step, the conductive nanoparticles comprise carbon nanotubes, reduced graphene and MXene, and the magnetic nanoparticles comprise magnetic MOF.
4. The method for preparing flexible electromagnetic shielding polyethersulfone film according to claim 1, wherein in step one, the time of ultrasonic treatment is 30 min.
5. The preparation method of the flexible electromagnetic shielding polyethersulfone film as claimed in claim 1, wherein in the second step, the mass ratio of polyethersulfone to ground nanoparticles to dried SMA sodium salt to polyethylene glycol to dimethylacetamide to distilled water is 12 (1-3): 2:8 (70-72): 5.
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