CN113024871A - Preparation method of MXene/polymer composite material capable of being heated by radiation - Google Patents
Preparation method of MXene/polymer composite material capable of being heated by radiation Download PDFInfo
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Abstract
The invention relates to the field of flexible wearable heating materials, in particular to a preparation method of a radiation-heatable MXene/polymer composite material, which comprises the following steps: carrying out surface hydroxylation treatment or polarity modification treatment on the polymer material, washing with deionized water, and drying to obtain a pretreated polymer material; and uniformly spraying the MXene solution on the pretreated polymer material, and drying to obtain the MXene/polymer composite material capable of being radiated and heated. The preparation method is simple and safe, has mild conditions, and can be used for large-scale batch preparation; the prepared MXene/polymer composite material has three heating modes of radiation heating, electric heating and optical heating, wherein the highest temperature in the radiation heating mode can reach 45.2 ℃, the highest temperature in the electric heating mode can reach 85.0 ℃, and the highest temperature in the optical heating mode can reach 90.0 ℃, so that the MXene/polymer composite material has great application value in the field of new-generation energy-saving heating flexible heat-insulating fabrics or films.
Description
Technical Field
The invention relates to the field of flexible wearable heating materials, in particular to a preparation method of a radiation-heatable MXene/polymer composite material.
Background
The maintenance of a relatively stable and proper body temperature is a prerequisite for the normal performance of various functions of a human body, and if the human body cannot reach heat balance in a short time, symptoms such as dehydration, cold and the like can be caused, so that the immunity is reduced. Generally, the temperature suitable for the human body to do activities can be met by using functional clothes or a method for adjusting indoor temperature. For indoor temperature regulation, huge resources are consumed every year when air conditioners or heating systems are used, and a large part of energy is wasted in heating vacant buildings and inanimate objects; in outdoor environments, human body warmth retention is equally important. The outdoor heating mainly depends on sunlight and electricity, the solar energy is used as clean energy, under the condition of sufficient sunlight, certain heat can be generated by depending on the light heating conversion characteristics of the material, and the heating requirement of a human body can be met in the daytime; while electrical heating relies on the electrical conductivity of the material itself to conduct joule conversion to obtain heat.
Generally, the skin temperature of a human body is about 34 ℃, the mid-infrared radiation emitted by the skin is mainly in the wavelength range (atmospheric window) of 7-14 μm, and about 50% of heat generated by the human body is lost through the infrared radiation. However, the mid-ir emissivity of conventional textiles is high, resulting in high heat loss. By controlling the emissivity of the textile in the middle infrared band, the infrared radiation loss can be reduced, and the passive radiation heating of the human body is realized. At present, researchers add metal fillers with low emissivity into fabrics to prepare composite fabrics with certain radiation heating effect, but the preparation process is complex, the density is high, the wearability is poor, and the electric heating and light heating effect of the fabrics is general, so that the application of the fabrics in the field of indoor and outdoor wearable heating is limited. Therefore, the development of polymer composites with multiple heating modes remains a significant challenge.
MXene is a novel two-dimensional nano material, which is a carbon/nitride nano layered structure material prepared by etching and stripping an A atomic layer in MAX phase by HF and other etching agents, and the general formula is Mn+1XnTxWherein M represents a transition metal element, X represents carbon or nitrogen element, and T represents a functional group (-OH, -F, ═ O, etc.) generated on the surface of the MAX phase during etching. Due to the characteristics of the layered structure, rich functional groups, ultra-high specific surface area and the like of MXene, the MXene has great application value in the fields of composite materials, adsorption, energy storage, electromagnetic shielding and the like. However, there is relatively little research on MXene in radiant heating and multiple heating mode polymer fabrics. The development of polymer composite materials with various heating modes based on MXene has important significance and great value.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a preparation method of a radiation-heatable MXene/polymer composite material, which solves the problem that the polymer fabric mentioned in the background art cannot simultaneously have radiation heating, electric heating and light heating modes.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method of making a radiation-heatable MXene/polymer composite comprising the steps of: carrying out surface hydroxylation treatment or polarity modification treatment on the polymer material, washing with deionized water, and drying to obtain a pretreated polymer material; and uniformly spraying the MXene solution on the pretreated polymer material, and drying to obtain the MXene/polymer composite material capable of being radiated and heated.
Preferably, the solution used for the surface hydroxylation treatment is a dopamine hydrochloride solution.
Preferably, the concentration of the dopamine hydrochloride solution is 1-10 mg/mL.
Preferably, the temperature of the dopamine hydrochloride solution treatment is 1-30 ℃, and the time is 1-36 h.
Preferably, the solution used for the polarity modification treatment consists of potassium dichromate, concentrated sulfuric acid and water, and the mass ratio of the potassium dichromate to the concentrated sulfuric acid to the water is (1-10): (80-120): 8.
preferably, the temperature of the polarity modification treatment is 40-70 ℃, and the time is 0.5-1.5 h.
Preferably MXene is Ti3C2Tx、Ti2CTx、Ti3CNTx、Nb2CTx、V2CTxThe solution is prepared by the following steps:
(1) dissolving 1-200 g LiF in 20-4000 mL of 5-20 mol/L HCl solution, and stirring for 20-60 min to prepare etching solution; at 35-50 deg.C, adding 1-200 g Ti3AlC2Adding the etching solution, etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH value is 6-7, pouring out the supernatant to obtain Ti3C2TxPrecipitating; mixing the above Ti3C2TxAdding the precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Ti3C2TxA solution;
(2) uniformly mixing 20-4000 mL of 5-20 mol/L HCL solution, 2-200 mL of 15-30 mol/L HF solution and 100-1000 mL of deionized water to prepare etching solution; at room temperature, adding 1-200 g of Ti2Adding AlC into the etching solution for etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH value is 6-7, pouring out the supernatant to obtain Ti2CTxPrecipitating; mixing the above Ti2CTxAdding the precipitate into 50-3000 mL of deionized water, oscillating, centrifuging at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Ti2CTxA solution;
(3) will be provided withDissolving 1-200 g LiF in 20-4000 mL of 5-20 mol/L HCl solution to prepare etching solution; at 25-40 deg.C, adding 1-200 g Ti3Adding AlCN into the etching solution, etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH value is 6-7, pouring out the supernatant to obtain Ti3CNTxPrecipitating; adding the MXene precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Ti3CNTxA solution;
(4) at 35-50 deg.C, adding 1-200 g Nb2Dissolving AlC in 20-4000 mL of 15-30 mol/L hydrofluoric acid etching solution, etching for 36-72 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH value is 6-7, pouring out the supernatant to obtain Nb2CTxPrecipitating; mixing the above Nb2Adding the C precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Nb2CTxA solution;
(5) at 35-50 deg.C, mixing 1-200 g V2Dissolving AlC in 20-4000 mL of 20-30 mol/L hydrofluoric acid etching solution, etching for 36-72 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH value is 6-7, pouring out the supernatant to obtain V2CTxPrecipitating; the above V is mixed2Adding the C precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain V2CTxAnd (3) solution.
Preferably, the concentration of the MXene solution is 0.1-25 mg/mL.
Preferably, the polymeric material is a polymer composite fabric or nonwoven or film.
Preferably, the polymer is at least one of polyethylene, polyvinyl chloride, polypropylene, acrylic fiber, polyurethane, aramid fiber, spandex, vinylon, polyester, nylon and cellulose acetate.
The invention provides a preparation method of a radiation-heatable MXene/polymer composite material, which has the following beneficial effects: the preparation method is simple and safe, has mild conditions, and can be used for large-scale batch preparation; the prepared MXene/polymer composite material has three heating modes of radiation heating, electric heating and optical heating, wherein the highest temperature in the radiation heating mode can reach 45.2 ℃, the highest temperature in the electric heating mode can reach 85.0 ℃, and the highest temperature in the optical heating mode can reach 90.0 ℃, so that the MXene/polymer composite material has great application value in the field of new-generation energy-saving heating flexible heat-insulating fabrics or films.
Drawings
FIG. 1 is a graph showing the water contact angle of the NanoPE film before pretreatment in example 1;
FIG. 2 is a graph showing the water contact angle of the pretreated NanoPE film in example 1;
FIG. 3 is a surface scanning electron microscope image of an MXene/NanoPE composite film prepared according to example 1;
FIG. 4 is an interface scanning electron microscope image of the MXene/NanoPE composite film prepared in example 1;
FIG. 5 is a graph showing the test of the radiation heating property of the MXene/NanoPE composite film prepared in example 1;
FIG. 6 is a photo-heating performance test chart of MXene/PVC composite fabric prepared in example 5;
FIG. 7 is an electrical heating performance test chart of MXene/PA-6 composite nonwoven fabric prepared in example 7.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the 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.
Example 1
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking a nano-porous polyethylene film (NanoPE) in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked NanoPE film with deionized water, and drying at 25 ℃ to obtain a pretreated NanoPE film;
(2) adding 30g LiF into 300mL of 25mol/L HCl solution at room temperature, and stirring for 30min to prepare etching solution; 20g of Ti3AlC2Adding the phase powder into the etching solution, and stirring for 24 hours at 35 ℃ to obtain a reaction product; diluting the reaction product, pouring into a centrifuge tube, centrifuging at 3500rpm for 5min, separating supernatant, repeatedly centrifuging until pH is not less than 6 to obtain precipitate Ti3C2TxIn the precipitate Ti3C2TxAdding deionized water, shaking by hand for 7min, centrifuging at 3500rpm for 7min, and performing ultrasonic treatment for 2 hr to obtain Ti of 4.3mg/mL3C2TxA solution;
(3) mixing Ti3C2TxUniformly spraying the solution on the pretreated nano PE film by using a spray gun, and drying at 25 ℃ for 5 hours to prepare the MXene/nano PE composite film capable of being heated by radiation; the MXene/NanoPE composite film has the electron microscope images and the radiation heating performance shown in figures 1-3.
Example 2
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
referring to example 1, an MXene/NanoPE composite film was obtained; different from the embodiment 1, the concentration of the dopamine hydrochloride solution is 3.5 mg/mL; the concentration of MXene solution was 5.2 mg/mL.
Example 3
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
referring to example 1, an MXene/NanoPE composite film was obtained; different from the embodiment 1, the concentration of the dopamine hydrochloride solution is 4.7 mg/mL; the concentration of MXene solution was 6.1 mg/mL.
Example 4
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking nylon 6(PA6) non-woven fabric in potassium dichromate, concentrated sulfuric acid and water solution in a mass ratio of 5:100:8 for 45min at 60 ℃, washing the soaked PA6 non-woven fabric with deionized water, and drying at room temperature to obtain a pretreated PA6 non-woven fabric;
(2) referring to example 1, MXene solution with concentration of 4.3mg/mL was prepared; the MXene solution is uniformly sprayed on the pretreated PA6 non-woven fabric by a spray gun and dried for 5 hours at room temperature to prepare the MXene/PA6 composite non-woven fabric capable of being heated by radiation.
Example 5
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking a polyvinyl chloride (PVC) fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PVC fabric with deionized water, and drying at room temperature to obtain a pretreated PVC fabric;
(2) uniformly mixing 240mL of 18mol/L HCL solution, 50mL of 28mol/L HF solution and 200mL of deionized water to prepare etching solution; at room temperature, add 10g of Ti2Adding AlC into the etching solution for etching for 36h, cleaning with deionized water, centrifuging at 4000rpm until the pH is 6, and removing the supernatant to obtain Ti2CTxPrecipitating; mixing the above Ti2CTxAdding 200mL deionized water into the precipitate, shaking for 7min, centrifuging at 3500rpm for 5min, and collecting supernatant to obtain 4.7mg/mL Ti3C2TxA solution;
(3) mixing Ti2CTxUniformly spraying the solution on the pretreated PVC fabric by using a spray gun, and drying at room temperature for 5 hours to obtain the MXene/PVC composite fabric capable of being heated by radiation; the photo-heating performance test chart of the MXene/PVC composite fabric is shown in FIG. 6.
Example 6
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking a polyvinyl chloride (PVC) fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PVC fabric with deionized water, and drying at room temperature to obtain a pretreated PVC fabric;
(2) at room temperature, adding 20g LiF into 240mL of 18mol/L HCl solution, and stirring for 30min to prepare etching solution; 20g of Ti3Adding AlCN powder into the etching solution, stirring at 35 deg.C for 24h to obtain reaction product, diluting the reaction product, pouring into a centrifuge tube, centrifuging at 3500rpm for 5min, separating supernatant, and repeatedly centrifuging until pH is not less than 6 to obtain the final productTi2CTxPrecipitating, adding deionized water into the precipitate, shaking by hand for 8min, centrifuging at 3500rpm for 7min, and performing ultrasonic treatment for 2 hr to obtain 4.9mg/mL Ti3CNTxA solution;
(3) mixing Ti3CNTxThe solution is sprayed on the pretreated PVC fabric uniformly by a spray gun and dried for 5 hours at 25 ℃ to prepare the MXene/PVC composite fabric capable of being heated by radiation.
Example 7
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking nylon 6(PA6) non-woven fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PA6 non-woven fabric with deionized water, and drying at room temperature to obtain pretreated PA6 non-woven fabric;
(2) 20g of Nb2Dissolving AlC in 200mL of 25mol/L hydrofluoric acid etching solution, stirring at 35 ℃ for 24h to obtain a reaction product, diluting the reaction product, pouring the diluted reaction product into a centrifuge tube, centrifuging at 3500rpm for 5min, separating supernatant, and repeatedly centrifuging until the pH is more than or equal to 6 to obtain Nb2CTx precipitation, adding deionized water into the precipitate, shaking by hand for 8min, centrifuging at 3500rpm for 7min, and subjecting to ultrasonic treatment for 2 hr to obtain 4.5mg/mL Nb2CTx solution;
(3) mixing the above Nb2Uniformly spraying the CTx solution on the pretreated PA-6 non-woven fabric by using a spray gun, and drying at room temperature for 5 hours to obtain MXene/PA6 composite non-woven fabric capable of being heated by radiation; the test chart of the electrical heating performance of the MXene/PA6 composite non-woven fabric is shown in FIG. 7.
Example 8
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
(1) soaking nylon 6(PA6) non-woven fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PA6 non-woven fabric with deionized water, and drying at room temperature to obtain pretreated PA6 non-woven fabric;
(2) 20g V2Dissolving AlC in 200mL of 25mol/L hydrofluoric acid etching solution, stirring at 35 ℃ for 24h to obtain a reaction product, and reacting the reaction productDiluting, pouring into centrifuge tube, centrifuging at 3500rpm for 5min, separating supernatant, and repeatedly centrifuging until pH is not less than 6 to obtain V2CTxPrecipitating, adding deionized water into the precipitate, shaking by hand for 8min, centrifuging at 3500rpm for 7min, and performing ultrasonic treatment for 2 hr to obtain 4.1mg/mL V2CTxA solution;
(3) the above V is mixed2CTxThe solution is uniformly sprayed on the pretreated PA-6 non-woven fabric by a spray gun and dried for 5 hours at room temperature to prepare the MXene/PA6 composite non-woven fabric capable of being heated by radiation.
Comparative example 1
nanoPE film without any treatment.
Comparative example 2
PVC fabric without any treatment.
Comparative example 3
PA6 nonwoven without any treatment.
Comparative example 4
Soaking a nano-porous polyethylene film (NanoPE) in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked NanoPE film with deionized water, and drying at 25 ℃ to obtain the pretreated NanoPE film.
Comparative example 5
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
referring to example 1, MXene solution with concentration of 4.3mg/mL was prepared; the MXene solution is evenly sprayed on a nano PE film by a spray gun and dried for 5 hours at room temperature to prepare the MXene/nano PE composite film capable of being heated by radiation.
Comparative example 6
And (2) soaking the PVC fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PVC fabric with deionized water, and drying at room temperature to obtain the pretreated PVC fabric.
Comparative example 7
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
referring to example 5, MXene solution with concentration of 4.7mg/mL was prepared; the MXene solution is sprayed on PVC fabric uniformly by a spray gun and dried for 5h at room temperature to prepare the MXene/PVC composite fabric capable of being heated by radiation.
Comparative example 8
And (2) soaking the PA6 non-woven fabric in 2mg/mL dopamine hydrochloride solution at room temperature, washing the soaked PA6 non-woven fabric with deionized water, and drying at room temperature to obtain the pretreated polymer non-woven fabric.
Comparative example 9
Soaking nylon 6(PA6) non-woven fabric in potassium dichromate, concentrated sulfuric acid and water solution in a mass ratio of 5:100:8 at 60 ℃ for 45min, washing the soaked PA6 non-woven fabric with deionized water, and drying at room temperature to obtain the pretreated PA6 non-woven fabric.
Comparative example 10
A method of making a radiation-heatable MXene/polymer composite comprising the steps of:
referring to example 7, MXene solution with concentration of 4.5mg/mL was prepared; and uniformly spraying the MXene solution on the PA-6 non-woven fabric by using a spray gun, and drying at room temperature for 5 hours to obtain the MXene/PA-6 composite non-woven fabric capable of being heated by radiation.
Testing and analysis
(1) Water contact Angle analysis
As can be seen from fig. 1, the water contact angle of the nanoPE film before pretreatment was 109 °, and as can be seen from fig. 2, the water contact angle of the nanoPE film after dopamine pretreatment was 41 °, and the smaller the water contact angle, the higher the hydrophilicity (adhesiveness) of the polymer substrate, in other words, the hydrophilicity (adhesiveness) of the surface of the polymer substrate after dopamine hydrochloride pretreatment was increased.
(2) Analysis by scanning Electron microscope
As can be seen from FIG. 3, the surface of the MXene/NanoPE film has been coated with the nanosheets, which shows that the MXene solution has been successfully attached to the surface of the NanoPE film; by scanning the interface of the MXene/NanoPE film prepared in example 1, it can be seen from FIG. 4 that the MXene layer and the NanoPE layer are bonded very tightly.
(3) Analysis of heating Properties
The polymer composites prepared in the above examples and comparative examples were tested for maximum temperature in different heating modes, respectively, as follows:
radiation heating performance test
And (3) heating by radiation, wherein the room temperature is 22-27 ℃, the temperature of the artificial skin is 33-36 ℃, and the highest temperature is achieved, namely the room temperature is 27 ℃ and the skin temperature is 36 ℃.
The thickness obtained in the above example was 12 μm and the area was 5X 5cm2Covering the film on a 4X 4cm piece2A2 mm gap is left in the middle of the silicon rubber heating plate, the surface temperature of the heating plate is controlled to be 36 ℃ before a film is not covered, and the real-time temperature of the surface of the heating plate is measured by a thermocouple after the film is covered.
② testing electrical heating performance
Electric heating condition: the environment temperature is 10-20 ℃, the applied voltage is 1-6V, the electric heating temperature can reach 30-85 ℃, and the highest temperature condition is as follows: ambient temperature 20 ℃ and 6V voltage was applied.
The film having a thickness of 12 μm obtained in the above example was cut into 2.5X 1.5cm2The sample (2) adopts a small direct current power supply machine as an external power supply, and leads (with crocodile clips) are respectively connected with the two sides of the film; the power supply is turned on (the output voltage is adjusted in advance), and the thermal infrared imager is used for recording the change of the temperature of the surface of the film along with the time (the power supply is turned off after the voltage is added for 2 min).
Thirdly, testing the optical heating performance
The method comprises the following steps of (1) heating by light, wherein the outdoor illumination is sufficient, the ambient temperature is 8-40 ℃, and the highest temperature is as follows: sufficient illumination, ambient temperature: 35-40 ℃. The film having a thickness of 12 μm obtained in the above example was cut into 2.5X 1.5cm2The sample is placed outdoors at the temperature of 15-35 ℃, and the temperature of the inner surface of the film is recorded by a thermocouple for 0: 00-24: 00.
As shown in FIG. 5, the MXene/NanoPE composite film obtained in example 1 was heated with increasing time under irradiation, and 30min later, the maximum temperature of the surface of the heated plate reached 42.1 ℃.
As shown in FIG. 6, the MXene/PVC composite fabric obtained in example 5 has a temperature rise under light heating with the intensity of sunlight, and the maximum temperature can reach 85.2 ℃.
The maximum temperature of the electric heating was measured by applying different voltage, as shown in fig. 7, the surface temperature of the MXene/PA6 composite nonwoven fabric obtained in example 7 was higher with increasing voltage, and the maximum temperature of the MXene/PA6 composite nonwoven fabric reached 81.4 ℃ when the voltage of the power supply was increased to 6V.
The composites prepared in the above examples and comparative examples were tested for maximum temperature in different heating modes and the results were as follows:
TABLE 1 highest temperature of Polymer composites in different heating modes
As can be seen from Table 1, as the concentration of dopamine hydrochloride and MXene increases, the highest temperature of the MXene/NanoPE composite film increases under three heating modes; as can be seen from the data of examples 1-8, the maximum temperature of the MXene/polymer composite in the three heating modes is not greatly affected by the polymer species; as can be seen from the data of the examples, comparative example 4, comparative example 6, comparative example 8 and comparative example 9, the introduction of MXene has a significant effect on the maximum temperature of the composite material in the optical heating and electric heating modes; the MXene has a three-dimensional porous structure (nano-layered structure), so that ion transmission and electron conduction are facilitated, and mass transfer of gas and liquid phases to the MXene surface is facilitated, so that the energy storage effect is good; the introduction of MXene increases the heat energy storage effect of the MXene/polymeric composite material. In addition, as for the radiation heating performance, as the infrared emissivity of MXene is low, part of radiation heat of a human body can be reflected.
As can be seen from the data of the examples, the comparative example 1, the comparative example 2, the comparative example 3, the comparative example 5, the comparative example 7 and the comparative example 10, the dopamine hydrochloride pretreatment has an effect on the highest temperature of the MXene/polymer composite material in three heating modes, and has a particularly remarkable effect on the highest temperature of the MXene/polymer composite material in the optical heating mode and the electric heating mode; this is because: the dopamine hydrochloride pretreatment can affect the adhesion (hydrophilicity) of the surface of the polymer substrate, namely the adhesion (hydrophilicity) of the surface of the polymer substrate after the dopamine hydrochloride pretreatment is enhanced, the adhesion of the polymer substrate and MXene solution is increased, and the radiation heating performance, the electric heating performance and the photo-heating performance can be improved simultaneously. From the data of the examples, the maximum temperature of the MXene/polymer composite after the polar modification treatment in the three heating modes is lower than that of the MXene/polymer composite after the polar modification treatment in the three heating modes.
In conclusion, the MXene/polymer composite material prepared by the method has the highest temperature of 45.2 ℃ in a radiation heating mode, 85.0 ℃ in an electric heating mode and 90.0 ℃ in a light heating mode, and has great application value in the field of new-generation energy-saving heating flexible heat-insulating fabrics or films.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method of making a radiation-heatable MXene/polymer composite comprising the steps of: carrying out surface hydroxylation treatment or polarity modification treatment on the polymer material, washing with deionized water, and drying to obtain a pretreated polymer material; and uniformly spraying the MXene solution on the pretreated polymer material, and drying to obtain the MXene/polymer composite material capable of being radiated and heated.
2. The method for preparing MXene/polymer composite capable of being heated by radiation according to claim 1, wherein the solution for surface hydroxylation treatment is dopamine hydrochloride solution.
3. The preparation method of the MXene/polymer composite capable of being heated by radiation according to claim 2, wherein the concentration of the dopamine hydrochloride solution is 1-10 mg/mL.
4. The method for preparing the MXene/polymer composite material capable of being heated by radiation according to claim 3, wherein the temperature of the dopamine hydrochloride solution treatment is 1-30 ℃ and the time is 1-36 h.
5. The preparation method of the MXene/polymer composite material capable of being heated by radiation according to claim 1, wherein the solution used for the polarity modification treatment consists of potassium dichromate, concentrated sulfuric acid and water, and the mass ratio of the potassium dichromate to the concentrated sulfuric acid to the water is (1-10): (80-120): 8.
6. the method for preparing MXene/polymer composite material capable of being heated by radiation according to claim 5, wherein the temperature of polar modification treatment is 40-70 ℃ and the time is 0.5-1.5 h.
7. The method for preparing MXene/polymer composite material capable of being heated by radiation according to claims 1-6, wherein MXene is Ti3C2Tx、Ti2CTx、Ti3CNTx、Nb2CTx、V2CTxThe solution is prepared by the following steps:
dissolving 1-200 g LiF in 20-4000 mL of 5-20 mol/L HCl solution, and stirring for 20-60 min to prepare etching solution; at 35-50 deg.C, adding 1-200 g Ti3AlC2Adding the etching solution, etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH is = 6-7, and pouring out the supernatant to obtain Ti3C2TxPrecipitating; mixing the above Ti3C2TxAdding the precipitate into 50-6000 mL of deionized water and shaking for 5-30 min, 3500-50Centrifuging at the rotating speed of 00rpm for 5-20 min, and collecting supernatant to obtain Ti3C2TxA solution;
uniformly mixing 20-4000 mL of 5-20 mol/L HCL solution, 2-200 mL of 15-30 mol/L HF solution and 100-1000 mL of deionized water to prepare etching solution; at room temperature, adding 1-200 g of Ti2Adding AlC into the etching solution for etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH is = 6-7, pouring out the supernatant to obtain Ti2CTxPrecipitating; mixing the above Ti2CTxAdding the precipitate into 50-3000 mL of deionized water, oscillating, centrifuging at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Ti2CTxA solution;
dissolving 1-200 g LiF in 20-4000 mL of 5-20 mol/L HCl solution to prepare etching solution; at 25-40 deg.C, adding 1-200 g Ti3Adding AlCN into the etching solution, etching for 18-36 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH is = 6-7, pouring out the supernatant to obtain Ti3CNTxPrecipitating; adding the MXene precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Ti3CNTxA solution;
at 35-50 deg.C, adding 1-200 g Nb2Dissolving AlC in 20-4000 mL of 15-30 mol/L hydrofluoric acid etching solution, etching for 36-72 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH is = 6-7, pouring out the supernatant to obtain Nb2CTxPrecipitating; mixing the above Nb2Adding the C precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, centrifuging for 5-20 min at the rotating speed of 3500-5000 rpm, and collecting supernatant to obtain Nb2CTxA solution;
at 35-50 deg.C, mixing 1-200 g V2Dissolving AlC in 20-4000 mL of 15-30 mol/L hydrofluoric acid etching solution, etching for 36-72 h, cleaning with deionized water, centrifuging at the rotating speed of 3500-5000 rpm until the pH is = 6-7, and pouring out the supernatant to obtain V2CTxPrecipitating; the above V is mixed2Adding the C precipitate into 50-6000 mL of deionized water, oscillating for 5-30 min, and centrifuging at a rotating speed of 3500-5000 rpm for 5-20 min, collecting the supernatant to obtain V2CTxAnd (3) solution.
8. The method for preparing the MXene/polymer composite material capable of being heated by radiation according to claim 7, wherein the concentration of the MXene solution is 0.1-25 mg/mL.
9. The method of preparing a radiation heatable MXene/polymer composite as claimed in claim 1, wherein the polymer material is a polymer composite fabric or a nonwoven fabric or a film.
10. The method of claim 9, wherein the polymer is at least one of polyethylene, polyvinyl chloride, polypropylene, acrylic, polyurethane, aramid, spandex, vinylon, polyester, nylon, and cellulose acetate.
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