CN114773655B - MXene mud composite film and preparation method and application thereof - Google Patents
MXene mud composite film and preparation method and application thereof Download PDFInfo
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- CN114773655B CN114773655B CN202210295017.9A CN202210295017A CN114773655B CN 114773655 B CN114773655 B CN 114773655B CN 202210295017 A CN202210295017 A CN 202210295017A CN 114773655 B CN114773655 B CN 114773655B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 76
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims description 84
- 238000001035 drying Methods 0.000 claims description 50
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000010382 chemical cross-linking Methods 0.000 claims description 28
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 20
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- 229910021641 deionized water Inorganic materials 0.000 claims description 18
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- 239000007787 solid Substances 0.000 claims description 12
- -1 polymethylene Polymers 0.000 claims description 11
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
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- 239000004971 Cross linker Substances 0.000 description 1
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- 229920002125 Sokalan® Polymers 0.000 description 1
- MKRNVBXERAPZOP-UHFFFAOYSA-N Starch acetate Chemical compound O1C(CO)C(OC)C(O)C(O)C1OCC1C(OC2C(C(O)C(OC)C(CO)O2)OC(C)=O)C(O)C(O)C(OC2C(OC(C)C(O)C2O)CO)O1 MKRNVBXERAPZOP-UHFFFAOYSA-N 0.000 description 1
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/146—Conductive polymers, e.g. polyethylene, thermoplastics
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- 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
- C08K3/10—Metal compounds
- C08K3/14—Carbides
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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
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Abstract
The invention relates to an MXene mud composite film and a preparation method and application thereof, the method utilizes waste MXene mud as a raw material to be compounded with a high polymer through a physical and chemical double crosslinking method, so that the original waste MXene mud is changed into valuables, and the prepared MXene mud composite film material has excellent mechanical property, oxidation resistance and hydrophobicity, and has excellent conductivity and electromagnetic shielding property.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to an MXene mud composite film, a preparation method and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Most of the existing methods use layered MXene nanoplatelets in the preparation of MXene-based composites, which allows 80-90% of the non-exfoliated multi-layered MXene nanoplatelets (MXene mud) to be discarded. Furthermore, in the preparation of macroscopic structures based on MXene materials using conventional methods, the centrifugation process is often severely demanding in order to increase the concentration of single-layer MXene nanoplatelets. The disadvantages of these preparation processes are very disadvantageous for mass production and industrial application of MXene-based materials.
Therefore, the MXene mud is compounded with other materials by a construction effective method, and on the premise that each performance meets the requirement, the waste of the MXene mud is changed into valuable, so that the cost of the MXene-based material is reduced. Meanwhile, the full utilization of the MXene mud means that most of raw materials can be fully utilized, the product yield is obviously improved, and the method is favorable for large-scale production and application of the MXene-based material. However, in comparison with the MXene materials which have been widely used at present, the MXene slurry material alone is in a powder form after drying, and it is difficult to form a film-like or block-like self-supporting structure, which is disadvantageous for the application of MXene slurry as a functional material or a structural material in various fields. This requires that the mechanical strength and oxidation resistance of the macrostructure material based on the MXene material be enhanced by compounding the MXene mud with other materials. The method has important significance for overcoming the defects of the MXene material and expanding the use scene of the MXene material. Research on the properties of the material and utilization of its advantages to achieve high performance, high durability products produced on an industrial scale have also been a major research and challenge in this field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the MXene mud composite film, the preparation method and the application thereof, the method utilizes the waste MXene mud as the raw material to be compounded with the polymer by a physical-chemical double crosslinking method, so that the original waste MXene mud is changed into valuables, the prepared MXene mud composite film material has excellent mechanical property, oxidation resistance and hydrophobicity, and has excellent conductivity and electromagnetic shielding property.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for preparing an MXene mud composite film, which comprises the following steps:
(1) Dispersing the MXene mud in deionized water to obtain an MXene mud aqueous dispersion;
(2) Fully and uniformly mixing the MXene mud aqueous dispersion and the water-soluble polymer aqueous dispersion to obtain a mixed aqueous dispersion;
(3) Pouring the mixed aqueous dispersion into a mould, and drying the mould containing the mixed aqueous dispersion to obtain a physical cross-linked MXene mud composite film sample;
(4) And (3) placing the MXene mud composite film sample in a solvent containing a cross-linking agent for chemical cross-linking, and drying to obtain the MXene mud composite film.
Filling the sheets of the multilayer MXene with a high polymer macromolecule achieves physical crosslinking of the MXene slurry, which enhances interactions between the MXene sheets; and simultaneously, a chemical cross-linking agent is used to react with the macromolecule polymer and the hydroxyl groups on the surface of the multilayer MXene lamellar layer to form covalent bonds between the multilayer MXene and the macromolecule polymer. Meanwhile, the hydrophobic skeleton of the chemical cross-linking agent can modify the composite film, and the hydrophobicity, oxidation resistance and mechanical strength of the MXene mud composite film can be improved simultaneously. Under the synergistic effect between two different crosslinking modes, the two-dimensional layered structure of the multi-layer MXene in the MXene mud is wrapped and reinforced, and is not easy to damage, so that the oxidation resistance and the mechanical strength of the MXene-based material are further improved.
Further, the MXene mud is a multi-layer MXene obtained by incomplete etching in the process of converting the MAX material into the MXene material.
Preferably, the MXene slurry is a carbide, nitride or carbonitride of a two-dimensional transition metal.
Wherein, the mass percent of the MXene mud can be 30-90 percent based on the total solid content in the raw materials.
The mass percentage of the water-soluble polymer is 5-65% based on the total solid content in the raw materials.
The mass percentage of the cross-linking agent is 0.1-10% based on the total solid content in the raw materials.
The mass percentage content of the MXene mud in the MXene mud aqueous dispersion liquid is 0.01-30%.
Preferably, the water-soluble polymer comprises any one or a combination of at least two of gelatin, cellulose, hydroxymethyl cellulose, carboxymethyl cellulose, lignin, starch, hydroxymethyl starch, starch acetate, vegetable gum, animal glue, polyacrylamide, polyvinylpyrrolidone (PVP), aqueous polyurethane (WPU), polyacrylic acid, polyacrylate, polyvinyl alcohol (PVA), polyaniline (PANI), polylactic acid, polymaleic anhydride or polyethylene glycol; further preferred is any one or a combination of at least two of polyvinyl alcohol, gelatin or aqueous polyurethane.
As a preferable technical scheme of the invention, the polymer such as polyvinyl alcohol and water-based polyurethane is used as a water-soluble polymer, so that the dispersibility of the MXene mud in water can be improved, and the physical crosslinking of the MXene sheet layer is further promoted to form the MXene composite material with high strength.
Preferably, the crosslinker is an isocyanate;
the isocyanate includes any one or a combination of at least two of polymethylene polyphenyl Polyisocyanate (PMDI), diphenylmethane-4, 4 '-diisocyanate (4, 4' -MDI), toluene-2, 4-diisocyanate, hexamethylene diisocyanate and the like, and PMDI is preferable.
Isocyanate and the MXene-based composite film are subjected to chemical crosslinking, and-NCO groups in isocyanate molecules react with groups such as-OH and the like on the MXene and the high polymer, so that the oxidation stability, mechanical strength, hydrophobicity and waterproofness of the MXene composite film are greatly improved.
Preferably, the water-soluble polymer is dissolved in the aqueous solution under a certain condition and uniformly dispersed to obtain the water-soluble polymer aqueous dispersion with a certain concentration, wherein the condition is that the temperature is 75-95 ℃ for 2-6 hours, and more preferably 90 ℃ for 4 hours.
In the invention, the dispersing processes in the steps (1) - (2) can be assisted by combining the magnetic stirring, ultrasonic and other modes, so as to be beneficial to uniformly dispersing the components in the aqueous solution.
Preferably, the thickness of the mold in step (3) is 100 μm to 3500 μm, more preferably 500 μm to 2000 μm.
Preferably, the drying temperature in step (3) is 15-90 ℃, further preferably 50 ℃.
Preferably, the organic solvent in the step (4) comprises any one or a combination of several of acetonitrile, methyl caproate, acetone, hexane, ethyl acetate, hexyl acetate, butanone, toluene, octane, butyl acetate, cyclohexanone, hexyl formate and the like, preferably acetonitrile and methyl caproate. The reaction temperature is related to the boiling point of the organic solvent selected, and the high temperature increases the reaction rate, typically 25℃to 120℃and preferably 70 ℃. The reaction time is 30min to 12h, and the specific preferred time is determined according to the desired degree of crosslinking and the reaction temperature.
Preferably, the temperature of the drying in step (4) is 15-180 ℃, and more preferably 20-100 ℃.
Preferably, the drying time in step (4) is 0.1 to 24 hours, more preferably 0.5 to 6 hours.
In a second aspect, the invention provides an MXene mud composite film prepared by the preparation method.
In the preparation method provided by the invention, two dispersion solutions are mixed and stirred uniformly to form a mixed aqueous dispersion; placing the mixed aqueous dispersion into a mould according to different thickness or quality, and drying the mixed aqueous dispersion in a blast drying box together with the mould to remove the water solvent, so as to prepare a single physically cross-linked MXene composite film pretreatment sample; and (3) placing the composite membrane material into an organic solvent containing a chemical crosslinking agent, performing chemical crosslinking treatment, and drying in a blast drying box to obtain the MXene mud composite membrane material.
The method has simple process flow and easy operation, does not need to operate under specific gas atmosphere, pressure intensity, temperature and humidity, does not need to use precise and expensive special instruments and equipment, greatly reduces the operation threshold and the production cost, and provides a brand new idea for large-scale industrial production of the composite film material based on the MXene mud.
In a third aspect, the present invention provides an application of the MXene mud composite film in electromagnetic shielding material, electrothermal material, fireproof material, waterproof material or support material.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a composite film material based on MXene mud, wherein a plurality of layers of MXene contained in the MXene mud can form a conductive path in a film, and the composite film material has good conductivity, hydrophobicity, electric heating property, oxidation resistance and mechanical strength, and has certain flexibility and excellent electromagnetic shielding performance;
the invention adopts the MXene mud which is not used in the prior art as the raw material, improves the utilization rate of the raw material, changes waste into valuable and is environment-friendly.
(2) The MXene mud composite film has good mechanical property, oxidation stability, hydrophobicity and the like through physical and chemical crosslinking.
(3) The thickness, the filler ratio and the crosslinking degree of the composite film material based on the MXene mud are adjustable, and the thickness, the filler ratio and the crosslinking degree can be adjusted according to practical purposes; the material can be applied to the related fields of mechanics, electricity, heat and the like;
(4) The method has simple process flow and easy operation, does not need to operate under specific gas atmosphere, pressure intensity, temperature and humidity, does not need to use precise and expensive special instruments and equipment, greatly reduces the operation threshold and the production cost, and provides a brand new idea for large-scale industrial production of the composite film material based on the MXene mud.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application.
FIG. 1 is an optical image of the MXene mud composite film material provided in example 1;
FIG. 2 is an optical image of a curved display of the MXene mud composite film material provided in example 2;
FIG. 3 is a cross-sectional scanning electron microscope image of the MXene mud composite film material provided in example 2;
FIG. 4 is a graph of the conductivity test results of the MXene mud composite film material provided in example 2;
FIG. 5 is a surface contact angle test chart of the MXene mud composite film material provided in example 2;
FIG. 6 is a graph of photo-induced thermal test results of the MXene mud composite film material provided in example 2;
FIG. 7 is an electromagnetic shielding effectiveness chart of the MXene mud composite film material provided in example 1.
FIG. 8 is a curled display optical image of the MXene mud composite film material provided in example 5;
FIG. 9 is a cross-sectional scanning electron microscope image of the MXene mud composite film material provided in example 6;
FIG. 10 is a graph of the conductivity test results of the MXene mud composite film material provided in example 6;
FIG. 11 is a graph of the results of an electro-thermal test of the MXene mud composite film material provided in example 6;
FIG. 12 is a graph of the results of an electro-thermal test of the MXene mud composite film material provided in example 6;
FIG. 13 is a graph of the photo-induced thermal test results of the MXene composite film material provided in example 6;
FIG. 14 is an electromagnetic shielding effectiveness chart of the MXene composite film material provided in example 5.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
4g of polyvinyl alcohol 124 (PVA) particles (national medicine group chemical reagent Co., ltd.) are completely dissolved in deionized water at 90 ℃ for 4 hours to obtain 200mL of aqueous solution, and uniformly dispersed to obtain 2% concentration polyvinyl alcohol aqueous solution;
dispersing MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion with a mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion with a mass fraction of 17.5% with a 2% polyvinyl alcohol aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion;
pouring the dispersed and mixed aqueous dispersion into a polytetrafluoroethylene mold with the thickness of 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off redundant dispersion by using a scraper to ensure that the dispersion is strictly flush with the upper surface of the mold and the mass of the added dispersion is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
The optical picture of the prepared MXene mud composite film material is shown in figure 1. FIG. 7 is an electromagnetic shielding effectiveness chart of the MXene mud composite film material provided in example 1, which shows that this example has excellent electromagnetic shielding performance.
In this example, the mass percent content of MXene mud was 90%, the mass percent content of polyvinyl alcohol was 5% and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 2
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
4g of polyvinyl alcohol 124 (PVA) particles (national medicine group chemical reagent Co., ltd.) are completely dissolved in deionized water at 90 ℃ for 4 hours to obtain 200mL of aqueous solution, and uniformly dispersed to obtain 2% concentration polyvinyl alcohol aqueous solution;
dispersing MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion with a mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion with a mass fraction of 17.5% with a 2% polyvinyl alcohol aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion;
pouring the dispersed and mixed aqueous dispersion into a polytetrafluoroethylene mold with the thickness of 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off redundant dispersion by using a scraper to ensure that the dispersion is strictly flush with the upper surface of the mold and the mass of the added dispersion is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
The optical picture of the curved display of the obtained MXene mud composite film material is shown in FIG. 2. As can be seen from fig. 2, the material has good flexibility and can be bent at will. FIG. 3 is a cross-sectional scanning electron microscope image of the MXene mud composite film material provided in example 2, and it can be seen from the image that the film thickness is uniform. FIG. 4 is a graph of the conductivity test results of the MXene mud composite film material provided in example 2, demonstrating that the sample of this example has good conductivity. Fig. 5 is a surface contact angle test chart of the MXene mud composite film material provided in example 2, and it can be seen that the surface of the sample after chemical crosslinking is hydrophobic. Fig. 6 is a graph showing the photo-induced heat test results of the MXene slurry composite film material provided in example 2, and it can be seen that the sample has excellent photo-thermal properties.
In this example, the mass percent content of MXene mud was 70%, the mass percent content of polyvinyl alcohol was 25%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 3
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
4g of polyvinyl alcohol 124 (PVA) particles (national medicine group chemical reagent Co., ltd.) are completely dissolved in deionized water at 90 ℃ for 4 hours to obtain 200mL of aqueous solution, and uniformly dispersed to obtain 2% concentration polyvinyl alcohol aqueous solution;
dispersing MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion with a mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion with a mass fraction of 17.5% with a 2% polyvinyl alcohol aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion;
pouring the dispersed and mixed aqueous dispersion into a polytetrafluoroethylene mold with the thickness of 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off redundant dispersion by using a scraper to ensure that the dispersion is strictly flush with the upper surface of the mold and the mass of the added dispersion is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
In this example, the mass percent content of MXene mud was 50%, the mass percent content of polyvinyl alcohol was 45%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 4
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
4g of polyvinyl alcohol 124 (PVA) particles (national medicine group chemical reagent Co., ltd.) are completely dissolved in deionized water at 90 ℃ for 4 hours to obtain 200mL of aqueous solution, and uniformly dispersed to obtain 2% concentration polyvinyl alcohol aqueous solution;
dispersing the MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion liquid with the mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion with a mass fraction of 17.5% with a 2% polyvinyl alcohol aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion;
pouring the dispersed and mixed aqueous dispersion into a polytetrafluoroethylene mold with the thickness of 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off redundant dispersion by using a scraper to ensure that the dispersion is strictly flush with the upper surface of the mold and the mass of the added dispersion is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
In this example, the mass percent content of MXene mud was 30%, the mass percent content of polyvinyl alcohol was 65%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 5
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
100mL of 30% aqueous polyurethane aqueous solution (Shenzhen Jitian chemical Co., ltd.) is completely dissolved in deionized water to obtain 200mL of aqueous solution, and the aqueous solution is uniformly dispersed to obtain 15% aqueous polyurethane aqueous solution;
dispersing the MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion liquid with the mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion liquid with the mass fraction of 17.5% and a 15% aqueous polyurethane aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion liquid;
pouring the dispersion liquid into a mold of polytetrafluoroethylene with the thickness of 100 mu m, 200 mu m, 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off the excessive dispersion liquid by using a scraper to ensure that the dispersion liquid is strictly flush with the upper surface of the mold, and the mass of the added dispersion liquid is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample. FIG. 8 is a crimped display optical image of the MXene mud composite film material provided in example 5. FIG. 14 is an electromagnetic shielding effectiveness chart of the MXene composite film material provided in example 5, which is seen to have excellent electromagnetic shielding performance.
In this example, the mass percent content of MXene mud was 90%, the mass percent content of aqueous polyurethane was 5% and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 6
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
100mL of 30% aqueous polyurethane aqueous solution (Shenzhen Jitian chemical Co., ltd.) is completely dissolved in deionized water to obtain 200mL of aqueous solution, and the aqueous solution is uniformly dispersed to obtain 15% aqueous polyurethane aqueous solution;
dispersing the MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion liquid with the mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion liquid with the mass fraction of 17.5% and a 15% aqueous polyurethane aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion liquid;
pouring the dispersion liquid into a mold of polytetrafluoroethylene with the thickness of 100 mu m, 200 mu m, 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off the excessive dispersion liquid by using a scraper to ensure that the dispersion liquid is strictly flush with the upper surface of the mold, and the mass of the added dispersion liquid is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample. FIG. 9 is a cross-sectional scanning electron microscope image of the MXene mud composite film material provided in example 6, and it can be seen from the image that the film thickness is uniform. FIG. 10 is a graph of the conductivity test results of the MXene mud composite film material provided in example 6, demonstrating that the sample of this example has excellent conductivity. FIG. 11 is a graph showing the results of an electro-thermal test of the MXene mud composite film material provided in example 6. FIG. 12 is a graph of the results of an electro-thermal test of the MXene mud composite film material provided in example 6. FIG. 13 is a graph showing the results of a photo-induced thermal test of the MXene composite film material provided in example 6. It can be seen from fig. 11 to 13 that the samples have excellent electrothermal and photo-thermal properties.
In this example, the mass percent content of MXene mud was 70%, the mass percent content of aqueous polyurethane was 25%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 7
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
100mL of 30% aqueous polyurethane aqueous solution (Shenzhen Jitian chemical Co., ltd.) is completely dissolved in deionized water to obtain 200mL of aqueous solution, and the aqueous solution is uniformly dispersed to obtain 15% aqueous polyurethane aqueous solution;
dispersing the MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion liquid with the mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion liquid with the mass fraction of 17.5% and a 15% aqueous polyurethane aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion liquid;
pouring the dispersion liquid into a mold of polytetrafluoroethylene with the thickness of 100 mu m, 200 mu m, 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off the excessive dispersion liquid by using a scraper to ensure that the dispersion liquid is strictly flush with the upper surface of the mold, and the mass of the added dispersion liquid is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
In this example, the mass percent content of MXene mud was 50%, the mass percent content of aqueous polyurethane was 45%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
Example 8
The composite film based on the MXene mud through physical and chemical double crosslinking is prepared by the following method:
100mL of 30% aqueous polyurethane aqueous solution (Shenzhen Jitian chemical Co., ltd.) is completely dissolved in deionized water to obtain 200mL of aqueous solution, and the aqueous solution is uniformly dispersed to obtain 15% aqueous polyurethane aqueous solution;
dispersing the MXene mud with a certain concentration in deionized water to obtain an MXene mud aqueous dispersion liquid with the mass fraction of 17.5%;
mixing an MXene mud aqueous dispersion liquid with the mass fraction of 17.5% and a 15% aqueous polyurethane aqueous solution according to a certain amount, and fully and uniformly mixing by using magnetic stirring to obtain a dispersed mixed aqueous dispersion liquid;
pouring the dispersion liquid into a mold of polytetrafluoroethylene with the thickness of 100 mu m, 200 mu m, 500 mu m, 1000 mu m, 1500 mu m and 2000 mu m respectively, and scraping off the excessive dispersion liquid by using a scraper to ensure that the dispersion liquid is strictly flush with the upper surface of the mold, and the mass of the added dispersion liquid is the same under the same mold thickness;
drying a die containing the mixed aqueous dispersion in a blast drying oven at 50 ℃ for 12 hours, and removing the water solvent to obtain a physically cross-linked MXene mud composite film pretreatment sample;
the composite film pretreatment sample is placed in a chemical cross-linking agent with acetonitrile and methyl caproate as solvents (volume ratio is 4:1) and PMDI as solute for a period of time to carry out chemical cross-linking reaction. The reaction temperature was 70℃and the reaction time was 2h. And (3) after the reaction, placing the mixture in a 70 ℃ blast drying oven for drying for 4 hours to obtain the physical and chemical double-crosslinked MXene mud composite film sample.
In this example, the mass percent content of MXene mud was 30%, the mass percent content of aqueous polyurethane was 65%, and the mass percent of PMDI was 5% based on the total solid mass of the feedstock.
By combining the above embodiments, the method adopted by the invention has simple process flow and easy operation, does not need to operate under specific gas atmosphere, pressure, temperature and humidity and use precise and expensive special instruments and equipment, greatly reduces the operation threshold and the production cost, and provides a brand new idea for large-scale industrial production of composite film materials based on MXene mud. The composite film based on the MXene mud has wide application prospect in the fields of electromagnetic shielding materials, electrothermal materials, fireproof materials, waterproof materials or supporting materials and the like.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. The preparation method of the MXene mud composite film is characterized by comprising the following steps of:
(1) Dispersing the MXene mud in deionized water to obtain an MXene mud aqueous dispersion; the MXene mud is a multi-layer MXene which is obtained by incomplete etching in the process of converting the MAX material into the MXene material; the mass percentage content of the MXene mud in the MXene mud aqueous dispersion liquid is 0.01-30%;
(2) Fully and uniformly mixing the MXene mud aqueous dispersion and the water-soluble polymer aqueous dispersion to obtain a mixed aqueous dispersion; the water-soluble polymer is any one of polyvinyl alcohol or aqueous polyurethane;
(3) Pouring the mixed aqueous dispersion into a mould, and drying the mould containing the mixed aqueous dispersion to obtain a physical cross-linked MXene mud composite film sample;
(4) Placing a physically crosslinked MXene mud composite film sample in an organic solvent containing a crosslinking agent for chemical crosslinking, and drying to obtain the MXene mud composite film; the cross-linking agent is isocyanate; the organic solvent comprises acetonitrile and methyl caproate; the MXene mud composite film is a physical and chemical double cross-linked MXene mud composite film;
wherein, based on the total solid content in the raw materials, the mass percentage of the MXene mud is 30-90%, the mass percentage of the water-soluble polymer is 5-65%, and the mass percentage of the cross-linking agent is 0.1-10%.
2. The method of claim 1, wherein the MXene slurry is a carbide, nitride or carbonitride of a two-dimensional transition metal.
3. The method according to claim 1, wherein the isocyanate comprises any one or a combination of at least two of polymethylene polyphenyl polyisocyanate, diphenylmethane-4, 4' -diisocyanate, toluene-2, 4-diisocyanate, and hexamethylene diisocyanate.
4. A method of preparation according to claim 3, wherein the isocyanate is polymethylene polyphenyl polyisocyanate.
5. The method according to claim 1, wherein the dispersion in the steps (1) and (2) is assisted by a combination of magnetic stirring and ultrasound;
the thickness of the die in the step (3) is 100-3500 μm;
the drying temperature in the step (3) is 15-90 ℃;
the drying temperature in the step (4) is 15-180 ℃;
the drying time in the step (4) is 0.1-24h.
6. The method according to claim 5, wherein the thickness of the mold in step (3) is 500 μm to 2000 μm;
the drying temperature in the step (3) is 50 ℃;
the drying temperature in the step (4) is 20-100 ℃;
the drying time in the step (4) is 0.5-6h.
7. The method of claim 1, wherein the chemical crosslinking temperature in step (4) is 25 ℃ to 120 ℃; the chemical crosslinking time is 30min-12h.
8. The process of claim 7, wherein the chemical crosslinking temperature in step (4) is 70 ℃.
9. The MXene mud composite film prepared by the preparation method according to any one of claims 1 to 8.
10. The use of the MXene mud composite film according to claim 9 in electromagnetic shielding material, electrothermal material, fire-proof material, water-proof material or support material.
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