CN113912905B - Preparation method of polyaniline/MXene/porous nylon film - Google Patents
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- CN113912905B CN113912905B CN202111262198.7A CN202111262198A CN113912905B CN 113912905 B CN113912905 B CN 113912905B CN 202111262198 A CN202111262198 A CN 202111262198A CN 113912905 B CN113912905 B CN 113912905B
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/365—Coating
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
A preparation method of a polyaniline/MXene/porous nylon film relates to a preparation method of a polyaniline/MXene/porous nylon film. The invention aims to solve the problems that the cost of the existing conductive material for constructing the polyaniline-based electrochromic film is high, and the application of polyaniline is limited. The method comprises the following steps: 1. preparing MXene solution; 2. preparing polyaniline dispersion liquid; 3. preparing MXene/porous nylon film; 4. preparing the polyaniline/MXene/porous nylon film. The preparation method is simple to operate, low in price and capable of being used for large-area preparation. The invention can obtain the polyaniline/MXene/porous nylon film.
Description
Technical Field
The invention relates to a preparation method of a polyaniline/MXene/porous nylon film.
Background
With the rapid development of wireless communication technology and the arrival of the high-frequency and high-speed 5G era, various electronic devices are in operation, however, the environment is flooded with a large amount of electromagnetic radiation due to a large amount of electromagnetic waves emitted by these electronic products during use. This not only affects the proper operation of the precision equipment, but can even be potentially harmful to the health of humans and animals. And in modern war, the leakage of electromagnetic wave may endanger national security, cause casualties and damage to equipment. In order to effectively prevent the unnecessary diffusion and interference of electromagnetic waves, a high-performance electromagnetic shielding material becomes a key technology for solving the electromagnetic wave pollution. In addition, electronic equipment and the like inevitably generate heat radiation in the using process, so that the electronic equipment is very easy to be found by infrared detection equipment, and an infrared heat radiation regulation and control technology for regulating and controlling the infrared characteristics of the electronic equipment and the like to be fused with the external environment is very important for stealth and anti-reconnaissance. How to prepare the functional film to have two functions of electromagnetic shielding and infrared thermal radiation regulation and control simultaneously so as to ensure that electronic equipment can normally operate in a complex external environment is a major challenge at present.
Polyaniline, as a typical conductive polymer, has been widely studied as an electrochromic material due to its advantages of low cost, good environmental stability, short response time, abundant color change, and the like. With the rapid development of military technology, space technology and the fields of energy conservation and environmental protection, the regulation and control range of the electrochromic material is expanded from a visible light wave band to an infrared wave band, and the infrared transmittance of polyaniline in a fading state is changed to realize the regulation and control of the infrared emissivity. For polyaniline-based electrochromic films, the films are composed of infrared high-reflection conductive materials and polyaniline materials. The polyaniline materials have different infrared transmittances under different voltages, and dynamic modulation of the infrared emissivity is achieved. Gold plated nylon porous films are often used as conductive materials, but the huge cost of evaporation gold plating limits their large area preparation. Therefore, it is highly desirable to provide a novel conductive material with low cost.
Disclosure of Invention
The invention aims to solve the problems that the cost of the existing conductive material for constructing the polyaniline-based electrochromic film is high and the application of polyaniline is limited, and provides a preparation method of a polyaniline/MXene/porous nylon film.
A preparation method of polyaniline/MXene/porous nylon film is completed according to the following steps:
1. preparing MXene solution:
dissolving MXene powder into deionized water, and magnetically stirring until the MXene powder is completely dissolved to obtain an MXene solution;
2. preparing polyaniline dispersion liquid:
dispersing polyaniline powder into an ethanol solution, and magnetically stirring to obtain a polyaniline dispersion liquid;
3. preparation of MXene/porous nylon films:
placing the porous nylon membrane on a heating plate of spraying equipment, taking out a certain amount of MXene solution prepared in the first step by using an injector, coating the MXene solution on the porous nylon membrane in a spraying manner to obtain an MXene/porous nylon membrane, and then placing the membrane in an oven for drying;
4. preparing a polyaniline/MXene/porous nylon film:
and (3) placing the dried MXene/porous nylon film obtained in the third step on a heating plate of spraying equipment again, taking out a certain amount of the polyaniline dispersion liquid prepared in the second step by using a syringe, coating the MXene/porous nylon film by a spraying mode, and then placing the MXene/porous nylon film in an oven for drying to obtain the polyaniline/MXene/porous nylon film.
The principle and the advantages of the invention are as follows:
1. the method adopts the porous nylon film as the substrate of the film, and sequentially coats the MXene layer and the polyaniline layer on the substrate in a spraying way to obtain the polyaniline/MXene/porous nylon film, wherein the polyaniline shows optical modulation characteristics under the action of an external electric field to enable the film to have infrared heat radiation regulation and control capability, and the MXene material enables the film to have electromagnetic shielding capability due to the advantages of large specific surface area and high conductivity;
2. the polyaniline/MXene/porous nylon film prepared by the method has the emissivity regulation and control capability of 0.32 in an infrared band (2.5-25 mu m) and the electromagnetic shielding capability of 23.4dB in an X band (8.2-12.4 GHz), and the preparation method is simple to operate, low in cost and capable of being used for large-area preparation.
The invention can obtain the polyaniline/MXene/porous nylon film.
Drawings
FIG. 1 is an SEM image of a porous nylon membrane in step three of the example;
FIG. 2 is an optical photograph of a polyaniline/MXene/porous nylon film prepared by one step four of the example;
FIG. 3 is a graph showing the change in the infrared emissivity of a polyaniline/MXene/porous nylon film prepared in step four of the example;
FIG. 4 is the electromagnetic shielding curve of the polyaniline/MXene/porous nylon film prepared in step four of the example.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting thereof. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
The first specific implementation way is as follows: the preparation method of the polyaniline/MXene/porous nylon film in the embodiment is completed according to the following steps:
1. preparing MXene solution:
dissolving MXene powder into deionized water, and magnetically stirring until the MXene powder is completely dissolved to obtain an MXene solution;
2. preparing a polyaniline dispersion liquid:
dispersing polyaniline powder into an ethanol solution, and magnetically stirring to obtain a polyaniline dispersion liquid;
3. preparation of MXene/porous nylon film:
placing the porous nylon membrane on a heating plate of spraying equipment, taking out a certain amount of MXene solution prepared in the first step by using an injector, coating the MXene solution on the porous nylon membrane in a spraying manner to obtain an MXene/porous nylon membrane, and then placing the membrane in an oven for drying;
4. preparing a polyaniline/MXene/porous nylon film:
and (2) placing the dried MXene/porous nylon film obtained in the third step on a heating plate of spraying equipment again, taking out a certain amount of the polyaniline dispersion liquid prepared in the second step by using a syringe, coating the MXene/porous nylon film by a spraying mode, and then placing the MXene/porous nylon film in an oven for drying to obtain the polyaniline/MXene/porous nylon film.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: MXene in the first step is Ti 3 C 2 、Ti 2 C、Nb 3 C 4 、Nb 2 C、V 3 C 2 、V 2 C、Ta 4 C 3 、Ta 2 C and Mo 2 C. Other steps and embodimentsThe same is true.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is: the mass concentration of the MXene solution in the step one is 0.1-0.9 mg/mL; the magnetic stirring speed in the step one is 100 r/min-1000 r/min. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the mass fraction of the ethanol solution in the second step is 99 percent; the speed of the magnetic stirring in the step two is 100 r/min-1000 r/min. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the mass concentration of the polyaniline dispersion liquid in the step two is 2 mg/mL-7 mg/mL. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode is as follows: the difference between this embodiment and one of the first to fifth embodiments is: the weight average molecular weight of the polyaniline in the step two is 50000 g/mol-150000 g/mol. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the temperature of the heating plate in the third step is 80-140 ℃; the specification of the injector in the third step is 25mL; the temperature of the oven in the third step is 50-120 ℃. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode eight: the difference between this embodiment and the first to seventh embodiments is: the volume ratio of the surface area of the porous nylon membrane to the MXene solution in the third step is (5 cm) 2 ～7cm 2 ) (5 mL-15 mL). The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the temperature of the heating plate in the fourth step is 60-120 ℃; the specification of the injector in the fourth step is 25mL; in the fourth step, the temperature of the oven is 40-100 ℃. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the volume ratio of the surface area of the porous nylon membrane to the polyaniline dispersion liquid in the fourth step is (5 cm) 2 ～7cm 2 ) (20 mL-40 mL). The other steps are the same as those in the first to ninth embodiments.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The first embodiment is as follows: a preparation method of polyaniline/MXene/porous nylon film is completed according to the following steps:
1. preparing MXene solution:
dissolving MXene powder into deionized water, and stirring at a magnetic stirring speed of 500r/min until the MXene powder is completely dissolved to obtain an MXene solution with a mass concentration of 0.5 mg/mL;
in the step one, MXene is Ti 3 C 2 ；
2. Preparing a polyaniline dispersion liquid:
dispersing polyaniline powder into an ethanol solution with the mass fraction of 99%, and stirring for 10min at the magnetic stirring speed of 500r/min to obtain polyaniline dispersion liquid with the mass concentration of 5 mg/mL;
the weight average molecular weight of the polyaniline in the step two is 100000g/mol;
3. preparation of MXene/porous nylon film:
placing the porous nylon membrane on a heating plate of spraying equipment, wherein the temperature of the heating plate is 100 ℃, taking out a certain amount of MXene solution prepared in the first step by using an injector, coating the MXene solution on the porous nylon membrane in a spraying manner to obtain an MXene/porous nylon membrane, and then placing the membrane in an oven at the temperature of 80 ℃ for drying;
the specification of the injector in the third step is 25mL;
the size of the porous nylon membrane in the third step is 2 x 3cm (length is 3cm, width is 2 cm);
the volume ratio of the surface area of the porous nylon membrane to the MXene solution in the third step is 6cm 2 :10mL；
4. Preparing a polyaniline/MXene/porous nylon film:
placing the dried MXene/porous nylon film obtained in the third step on a heating plate of spraying equipment again, wherein the temperature of the heating plate is 100 ℃, taking out a certain amount of the polyaniline dispersion liquid prepared in the second step by using an injector, coating the polyaniline dispersion liquid on the MXene/porous nylon film in a spraying manner, and then placing the MXene/porous nylon film in an oven at the temperature of 80 ℃ for drying to obtain the polyaniline/MXene/porous nylon film;
the specification of the injector in the fourth step is 25mL;
the volume ratio of the surface area of the porous nylon membrane to the polyaniline dispersion liquid in the fourth step is 6cm 2 :30mL。
FIG. 1 is an SEM image of a porous nylon membrane in step three of the example;
as can be seen from fig. 1, the base porous nylon membrane has a porous structure.
FIG. 2 is an optical photograph of a polyaniline/MXene/porous nylon film prepared by one step four of the example;
as can be seen from fig. 2, the color of the polyaniline/MXene/porous nylon film is black.
FIG. 3 is a graph showing the change in the infrared emissivity of a polyaniline/MXene/porous nylon film prepared in step four of the example;
as can be seen from FIG. 3, the change of the infrared emissivity of the polyaniline/MXene/porous nylon film in the infrared band (2.5-25 μm) is 0.32.
FIG. 4 is the electromagnetic shielding curve of the polyaniline/MXene/porous nylon film prepared in step four of the example.
As can be seen from FIG. 4, the electromagnetic shielding capability of the polyaniline/MXene/porous nylon film is 23.4dB.
Claims (7)
1. A preparation method of a polyaniline/MXene/porous nylon film is characterized by comprising the following steps:
1. preparing MXene solution:
dissolving MXene powder into deionized water, and magnetically stirring until the MXene powder is completely dissolved to obtain an MXene solution;
the mass concentration of the MXene solution in the first step is 0.1-0.9 mg/mL;
2. preparing polyaniline dispersion liquid:
dispersing polyaniline powder into an ethanol solution, and magnetically stirring to obtain a polyaniline dispersion liquid;
the mass concentration of the polyaniline dispersion liquid in the second step is 2-7 mg/mL;
3. preparation of MXene/porous nylon film:
placing the porous nylon membrane on a heating plate of spraying equipment, taking out a certain amount of MXene solution prepared in the first step by using an injector, coating the MXene solution on the porous nylon membrane in a spraying manner to obtain an MXene/porous nylon membrane, and then placing the membrane in an oven for drying;
the volume ratio of the surface area of the porous nylon membrane to the MXene solution in the third step is (5 cm) 2 ~7cm 2 ):(5mL~15mL)；
4. Preparing a polyaniline/MXene/porous nylon film:
placing the dried MXene/porous nylon film obtained in the third step on a heating plate of spraying equipment again, taking out a certain amount of the polyaniline dispersion liquid prepared in the second step by using an injector, coating the polyaniline dispersion liquid on the MXene/porous nylon film in a spraying way, and then placing the MXene/porous nylon film in an oven for drying to obtain the polyaniline/MXene/porous nylon film;
the volume ratio of the surface area of the porous nylon membrane to the polyaniline dispersion liquid in the fourth step is (5 cm) 2 ~7cm 2 ):(20mL~40mL)。
2. The method according to claim 1, wherein the MXene is Ti 3 C 2 、Ti 2 C、Nb 3 C 4 、Nb 2 C、V 3 C 2 、V 2 C、Ta 4 C 3 、Ta 2 C and Mo 2 C.
3. The method as claimed in claim 1, wherein the magnetic stirring speed in step one is 100r/min to 1000r/min.
4. The method for preparing polyaniline/MXene/porous nylon membrane as claimed in claim 1, wherein the ethanol solution in step two is 99% by weight; the speed of the magnetic stirring in the step two is 100 r/min-1000 r/min.
5. The method of claim 1, wherein the weight average molecular weight of the polyaniline in the second step is 50000g/mol to 150000g/mol.
6. The method for preparing the polyaniline/MXene/porous nylon film as claimed in claim 1, wherein the temperature of the heating plate in step three is 80-140 ℃; the specification of the injector in the third step is 25mL; the temperature of the oven in the third step is 50-120 ℃.
7. The method for preparing the polyaniline/MXene/porous nylon film as claimed in claim 1, wherein the temperature of the heating plate in step four is 60 ℃ to 120 ℃; the specification of the injector in the fourth step is 25mL; the temperature of the oven in the fourth step is 40-100 ℃.
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Citations (3)
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| CN111809439A (en) * | 2020-06-30 | 2020-10-23 | 陕西科技大学 | Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof |
| CN112647107A (en) * | 2020-11-30 | 2021-04-13 | 哈尔滨工业大学 | Preparation method of polyaniline/gold particle composite film with high infrared radiation regulation and control capability |
| CN113136102A (en) * | 2021-04-21 | 2021-07-20 | 成都大学 | Titanium carbide-polyaniline composite material with high electrochromic performance and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111809439A (en) * | 2020-06-30 | 2020-10-23 | 陕西科技大学 | Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof |
| CN112647107A (en) * | 2020-11-30 | 2021-04-13 | 哈尔滨工业大学 | Preparation method of polyaniline/gold particle composite film with high infrared radiation regulation and control capability |
| CN113136102A (en) * | 2021-04-21 | 2021-07-20 | 成都大学 | Titanium carbide-polyaniline composite material with high electrochromic performance and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Highly-flexible monolithic integrated infrared electrochromic device based on polyaniline conducting polymer;Shanshan Song et al.;《Synthetic Metals》;20210525;第278卷;第1-8页 * |
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