CN117230655A - Aramid fiber-based composite electric heating material and preparation method thereof - Google Patents
Aramid fiber-based composite electric heating material and preparation method thereof Download PDFInfo
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- CN117230655A CN117230655A CN202311272746.3A CN202311272746A CN117230655A CN 117230655 A CN117230655 A CN 117230655A CN 202311272746 A CN202311272746 A CN 202311272746A CN 117230655 A CN117230655 A CN 117230655A
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- 239000000463 material Substances 0.000 title claims abstract description 108
- 239000002131 composite material Substances 0.000 title claims abstract description 107
- 238000005485 electric heating Methods 0.000 title claims abstract description 106
- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004760 aramid Substances 0.000 claims abstract description 78
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 78
- 239000006185 dispersion Substances 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 48
- 238000007731 hot pressing Methods 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000011248 coating agent Substances 0.000 claims abstract description 32
- 239000000835 fiber Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 238000003825 pressing Methods 0.000 claims description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 19
- 230000007935 neutral effect Effects 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 15
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 9
- 239000002585 base Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000002135 nanosheet Substances 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
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- 239000007769 metal material Substances 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 239000011150 reinforced concrete Substances 0.000 description 2
- 238000001931 thermography Methods 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention provides an aramid fiber-based composite electric heating material and a preparation method thereof, comprising the following steps: mixing the fibrid of the meta-aramid with the chopped fiber of the meta-aramid, and sequentially carrying out fluffing dispersion, wet forming, squeezing and drying treatment to obtain meta-aramid paper; coating MXene dispersion liquid on the meta-position aramid paper to obtain m-position aramid paper coated with MXene; carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; the preparation process is simple, and the composite electric heating material has the advantages of high strength, good electric heating performance, high safety coefficient, wide application scene, simple production process and the like, and meets the requirement of large-scale production.
Description
Technical Field
The invention belongs to the technical field of electric heating materials, and particularly relates to an aramid fiber-based composite electric heating material and a preparation method thereof.
Background
An electrothermal material, which is a functional material capable of generating joule heat under an applied voltage; the metal material is used as the traditional electric heating material, and the general metal material cannot meet the application on a precise instrument due to the characteristics of large mass, high rigidity and the like; composite electrocaloric materials as emerging electrocaloric materials, typically including a base layer and a conductive layer; the base layer is used for ensuring high strength and flexibility of the composite material, and the conductive layer provides low resistance and joule heating performance for the composite material; secondly, the composite electric heating material generally has the advantages of light weight, good flexibility, strong designability and the like; therefore, the composite electric heating material has great application prospect.
Currently, two main categories are classified: (1) The conductive filler and the adhesive are directly mixed and then coated or sprayed, but the conductive performance of the conductive layer is easily reduced greatly, so that the electric heating performance of the composite electric heating material is reduced; (2) The conductive material is covered after the adhesive is coated on the surface of the matrix, but the adhesive has higher requirements on the stability and high temperature resistance of the adhesive in long-term operation, the bonding force between the composite electric heating material base layer and the conductive layer is reduced due to aging or failure of the adhesive, and finally the conductive layer is dropped off, so that the electric heating performance of the composite electric heating material is seriously affected.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides an aramid fiber-based composite electric heating material and a preparation method thereof, so as to solve the technical problem of lower electric heating performance of the traditional composite electric heating material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
mixing the fibrid of the meta-aramid with the chopped fiber of the meta-aramid, and sequentially carrying out fluffing dispersion, wet forming, squeezing and drying treatment to obtain meta-aramid paper;
coating MXene dispersion liquid on the meta-position aramid paper to obtain m-position aramid paper coated with MXene;
and carrying out hot pressing treatment on the meta-position aramid paper coated with MXene to obtain the aramid-based composite electric heating material.
Further, the fibrid of the meta-aramid is mixed with the chopped fiber of the meta-aramid according to the mass ratio of (9-4) to (1-6).
Further, a cold pressing treatment process is adopted during the squeezing treatment; wherein the cold pressing pressure is 0.2-0.5MPa, and the cold pressing time is 5-15min.
Further, the concentration of the MXene dispersion is 5-10mg/mL.
Further, the process of coating the MXene dispersion liquid on the meta-aramid paper to obtain the meta-aramid paper coated with MXene comprises the following steps:
coating the MXene dispersion liquid on the meta-aramid paper in a mode of mechanical coating for a plurality of times; after the water in the paper is removed by vacuum drying after each smearing is finished, the next smearing is carried out.
Further, the preparation process of the MXene dispersion liquid comprises the following specific steps:
lithium fluoride, hydrochloric acid solution and Ti 3 AlC 2 Mixing, and carrying out etching reaction to obtain a mixed solution after the reaction;
washing and centrifuging the reacted mixed solution for a plurality of times to remove supernatant until the pH value is neutral, thereby obtaining a neutral solution;
and carrying out ultrasonic treatment and centrifugation on the central solution to obtain the MXene dispersion liquid.
Further, in the process of carrying out hot pressing treatment on the meta-position aramid paper coated with MXene, the hot pressing pressure is 1-11MPa, the hot pressing temperature is 150-250 ℃ and the time is 3-15min.
The invention also provides an aramid fiber-based composite electric heating material, which is prepared by adopting the preparation method of the aramid fiber-based composite electric heating material according to any one of claims 1-7.
Further, the tensile strength of the aramid fiber-based composite electric heating material is 40-80MPa, and the conductivity is 400-4500Sm -1 。
Furthermore, the temperature of the aramid fiber-based composite electric heating material can be raised to 50-140 ℃ within 27-30s under 5V voltage.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides an aramid fiber-based composite electric heating material and a preparation method thereof, wherein meta-aramid fiber paper with high strength, high modulus, good temperature resistance and flame retardant property is used as a substrate, MXene coated on the meta-aramid fiber paper is used as a conductive coating, and the substrate and the conductive layer are tightly combined through hot pressing treatment, so that the binding force between the substrate and the conductive layer is ensured, and the thermal stability of the composite electric heating material is further ensured; secondly, the MXene nano-sheets on the surface of the meta-aramid paper can be more tightly connected through hot pressing treatment, so that the conductivity and the electric heating performance of the composite electric heating material are improved; in addition, after the meta-aramid paper is subjected to hot pressing treatment, the fibrid and the chopped fiber of the meta-aramid can be softened and bonded together, so that the interface bonding strength between the chopped fiber and the fibrid of the aramid is remarkably improved, a compact reinforced concrete structure is constructed, and the mechanical property of the composite material is effectively ensured; the preparation process is simple, and the composite electric heating material has the advantages of high strength, good electric heating performance, high safety coefficient, wide application scene, simple production process and the like, and meets the requirement of large-scale production; the light and high-performance meta-aramid paper is used as a base layer, and provides necessary conditions for the application of the composite electric heating material in a precise instrument; in addition, the excellent flexibility can also be applied to the special-shaped piece, so that the application scene of the composite electric heating material is further expanded; in addition, the excellent high temperature resistance and flame retardant property of the aramid fiber provide necessary guarantee for the safety of the composite electrothermal paper.
Furthermore, the MXene dispersion liquid is coated on meta-aramid paper through a plurality of mechanical coating processes, the mechanical coating can accurately control the coating amount of the MXene dispersion liquid, the coating position can be freely controlled, the designability is high, and in addition, the thickness of the conductive coating can be controlled by controlling the concentration of the MXene dispersion liquid; the MXene nano-sheet with metal level electronic conductivity can realize the rapid heating of the composite electrothermal paper, the composite electrothermal paper can be heated to the highest temperature of 140 ℃ within 27-30s under 5V voltage, and the lower driving pressure can realize the rapid heating under complex environment through self-powered.
Drawings
FIG. 1 is an SEM image of MXene nanoplatelets of examples 1-6;
FIG. 2 is a surface SEM image of the composite electric heating material prepared in example 2;
FIG. 3 is an infrared thermogram of the composite electric heating material prepared in example 3;
FIG. 4 is an infrared thermogram of the composite electric heating material prepared in example 4;
FIG. 5 is a graph showing the temperature change with time of the composite electric heating material prepared in example 6 at different voltages.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the invention more clear, the following specific embodiments are used for further describing the invention in detail. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, mixing fibrid of meta-aramid fiber and chopped fiber of meta-aramid fiber according to the mass ratio of (9-4) to (1-6), and sequentially carrying out fluffing dispersion, wet forming, squeezing and drying treatment to obtain meta-aramid fiber paper;
specifically, a mixture of fibrid of meta-aramid fiber and chopped fiber of meta-aramid fiber is placed in a fiber fluffer, and uniform dispersion liquid is obtained under the condition that the rotating speed is 10000-50000 r/min; then, the uniform dispersion liquid is utilized to obtain a wet paper web through a wet forming process; then, carrying out cold pressing treatment on the wet paper web under the condition that the cold pressing pressure is 0.2-0.5MPa, wherein the cold pressing time is 5-15min; and then, vacuum drying is carried out for 10-15min under the condition of 105-120 ℃ to obtain the meta-aramid paper.
Step 2, lithium fluoride, hydrochloric acid solution and Ti 3 AlC 2 Mixing, and carrying out etching reaction to obtain a mixed solution after the reaction; washing and centrifuging the reacted mixed solution for a plurality of times to remove supernatant until the pH value is neutral, thereby obtaining a neutral solution; carrying out ultrasonic treatment and centrifugation on the central solution to obtain MXene dispersion liquid; wherein the concentration of the MXene dispersion liquid is 5-10mg/mL.
Step 3, smearing MXene dispersion liquid on the meta-position aramid paper to obtain m-position aramid paper smeared with MXene; specifically, the MXene dispersion liquid is coated on the meta-aramid paper in a mode of mechanical coating for a plurality of times; after the water in the paper is removed by vacuum drying after each smearing is finished, the next smearing is carried out.
Step 4, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 1-11MPa, the hot pressing temperature is 150-250 ℃, and the time is 3-15min.
Working principle:
according to the preparation method of the aramid fiber-based composite electric heating material, meta-aramid fiber paper is used as a substrate, and MXene coated on the meta-aramid fiber paper is used as a conductive coating; the meta-aramid paper is used as a high-strength high-modulus, high-temperature-resistant, flame-retardant and acid-alkali-resistant high-performance fiber, and the MXene is used as a two-dimensional nanomaterial which has metal-level electronic conductivity; uniformly coating the MXene dispersion liquid on the aramid paper through mechanical coating, drying and then carrying out a hot-pressing process to tightly combine the substrate and the conductive layer, so that the bonding force between the substrate and the conductive layer is ensured, and the thermal stability of the composite electric heating material is further ensured; the composite electrothermal material has higher mechanical property and conductivityWherein the tensile strength of the aramid fiber-based composite electric heating material is 40-80MPa, and the conductivity is 400-4500Sm -1 The method comprises the steps of carrying out a first treatment on the surface of the The aramid fiber-based composite electric heating material can be heated to 50-140 ℃ within 27-30 seconds under 5V voltage.
Example 1
The embodiment 1 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 5mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 9:1, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition that the rotating speed is 15000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 5min under the condition that the cold pressing pressure is 0.2 MPa; and then, vacuum drying is carried out for 15min under the condition of 105 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a 1-time mechanical coating mode; after the MXene dispersion was applied, vacuum drying was performed at 105 ℃ for 15 minutes to remove moisture in the paper, to obtain MXene-applied meta-aramid paper.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 1MPa, the hot pressing temperature is 150 ℃ and the time is 3min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 1 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 1 has the characteristics of higher mechanical property, good conductivity and stability, low driving voltage and high heating rate; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 40MPa, and the conductivity reaches 400Sm -1 The temperature may be raised to 50℃after 27s at 5V.
Example 2
The embodiment 2 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 6mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 8:2, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition that the rotating speed is 20000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 10min under the condition that the cold pressing pressure is 0.3 MPa; and then, vacuum drying is carried out for 14min under the condition of 108 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a 3-time mechanical coating mode; after each application of the MXene dispersion, vacuum drying is carried out for 14min at 108 ℃ to remove the moisture in the paper, so as to obtain the m-aramid paper coated with MXene.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 3MPa, the hot pressing temperature is 170 ℃, and the time is 5min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 2 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 2 has the characteristics of higher mechanical property, good conductivity and stability, low driving voltage and high heating rate; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 45MPa, and the conductivity reaches 900Sm -1 The temperature may be raised to 65℃after 27s at 5V.
Example 3
The embodiment 3 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 7mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 7:3, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition that the rotating speed is 20000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 10min under the condition that the cold pressing pressure is 0.4 MPa; and then, drying in vacuum for 13min at the temperature of 111 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a mechanical coating mode for 5 times; after each application of the MXene dispersion, vacuum drying is performed for 13min at 111 ℃ to remove the moisture in the paper, so as to obtain the m-aramid paper coated with MXene.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 5MPa, the hot pressing temperature is 190 ℃, and the time is 7min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 3 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 3 has the characteristics of higher mechanical property, good conductivity and stability, low driving voltage and high heating rate; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 50MPa, and the conductivity reaches 1500Sm -1 The temperature can be raised to 82.6℃after 28s at 5V.
Example 4
The embodiment 4 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 8mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 6:4, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition of the rotating speed of 30000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 10min under the condition that the cold pressing pressure is 0.5 MPa; and then, vacuum drying is carried out for 12min under the condition of 115 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a 7-time mechanical coating mode; after each application of the MXene dispersion, vacuum drying is carried out for 12min at 115 ℃ to remove the moisture in the paper, so as to obtain the m-aramid paper coated with MXene.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 7MPa, the hot pressing temperature is 210 ℃, and the time is 10min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 4 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 4 has the characteristics of higher mechanical property, good conductivity and stability, low driving voltage and high heating rate; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 60MPa, and the conductivity reaches 2500Sm -1 The temperature may be raised to 105℃after 28s at 5V.
Example 5
The embodiment 5 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 9mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 5:5, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition that the rotating speed is 40000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 15min under the condition that the cold pressing pressure is 0.5 MPa; and then vacuum drying is carried out for 11min at the temperature of 118 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a 9-time mechanical coating mode; after each application of the MXene dispersion, vacuum drying is performed for 11min at 118 ℃ to remove the moisture in the paper, so as to obtain the m-aramid paper coated with MXene.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 9MPa, the hot pressing temperature is 230 ℃, and the time is 12min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 5 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 5 has higher mechanical property, conductivity and stabilityThe driving voltage is low, and the temperature rising rate is high; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 70MPa, and the conductivity reaches 3500Sm -1 The temperature can be raised to 135℃after 30s at 5V.
Example 6
The embodiment 6 provides a preparation method of an aramid fiber-based composite electric heating material, which comprises the following steps:
step 1, 1.6g of lithium fluoride (LiF) is added into 25mL of hydrochloric acid solution, and after 5min of magnetic stirring, 1g of Ti is added 3 AlC 2 Adding the mixture for multiple times, and then magnetically stirring the mixture for etching for 36 hours at the temperature of 40 ℃ to obtain a mixed solution after the reaction; wherein the mass concentration of the hydrochloric acid solution is 37%, and the Ti is 3 AlC 2 The mesh number of (2) is 400 mesh.
Step 2, performing centrifugal treatment on the reacted mixed solution for a plurality of times to remove supernatant until the pH value reaches neutrality, so as to obtain a neutral solution; then carrying out ultrasonic treatment on the neutral solution under ice bath condition, and finally centrifuging to obtain MXene dispersion liquid; wherein, during ultrasonic treatment, the ultrasonic power is 80W, and the ultrasonic treatment time is 1h; the concentration of the MXene dispersion was 11mg/mL.
Step 3, mixing the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber according to the mass ratio of 4:6, and putting the mixture into a fiber fluffer to be dispersed and fluffed under the condition that the rotating speed is 50000r/min to obtain uniform dispersion liquid; obtaining a wet paper web by utilizing the uniform dispersion liquid through a wet forming process; then, carrying out cold pressing treatment on the wet paper web for 15min under the condition that the cold pressing pressure is 0.5 MPa; and then, vacuum drying is carried out for 10min at the temperature of 120 ℃ to obtain the meta-aramid paper.
Step 4, smearing the MXene dispersion liquid in the step 2 on the meta-aramid paper in the step 3 in a mechanical coating mode for 11 times; after each application of the MXene dispersion, vacuum drying is carried out for 10min at 120 ℃ to remove the moisture in the paper, so as to obtain the m-aramid paper coated with MXene.
Step 5, carrying out hot pressing treatment on the m-aramid paper coated with MXene to obtain the aramid-based composite electric heating material; wherein the hot pressing pressure is 11MPa, the hot pressing temperature is 250 ℃, and the time is 15min.
And (3) material performance detection:
the performance of the aramid fiber-based composite electric heating material prepared in example 6 was tested, and the test result found that: the aramid fiber-based composite electric heating material prepared in the embodiment 6 has the characteristics of higher mechanical property, good conductivity and stability, low driving voltage and high heating rate; wherein the tensile strength of the aramid fiber-based composite electric heating material reaches 80MPa, and the conductivity reaches 4500Sm -1 The temperature may be raised to 140℃after 30s at 5V.
As shown in FIG. 1, SEM images of MXene nanoplatelets of examples 1-6 are shown in FIG. 1, from FIG. 1 it can be seen that Ti will be present in a mixed solution of lithium fluoride and hydrochloric acid 3 AlC 2 Is etched into an accordion shape; as shown in fig. 2, a surface SEM image of the composite electric heating material prepared in example 2 is shown in fig. 2, and it can be seen from fig. 2 that the surface of the composite electric heating material after being coated with MXene and hot-pressed is very dense; as shown in fig. 3, an infrared thermal imaging diagram of the composite electric heating material prepared in example 3 is shown in fig. 3, and it can be seen from fig. 3 that the composite electric heating material prepared by mechanically coating 7mg/mL of MXene dispersion 5 times can be heated to 82.6 ℃ at 5V; as shown in fig. 4, an infrared thermal imaging diagram of the composite electric heating material prepared in example 4 is shown in fig. 4, and it can be seen from fig. 4 that the composite electric heating material prepared by mechanically coating 8mg/mL of MXene dispersion liquid 7 times can be heated to 105 ℃ at 5V; as shown in FIG. 5, a graph of the temperature of the composite electric heating material prepared in example 6 with time at different voltages is shown in FIG. 5, and it can be seen from FIG. 5 that the composite electric heating material prepared by mechanically coating 11mg/mL of MXene dispersion 11 times can be heated to 35-140 ℃ after 30s at 2-5V.
The aramid fiber-based composite electric heating material and the preparation method thereof are prepared by taking meta-aramid fiber paper with high strength, high modulus, good temperature resistance and flame retardance as a substrate and taking an MXene nano sheet with high conductivity as a conductive coating; the light and high-performance meta-aramid paper is adopted as a base layer, so that necessary conditions are provided for the application of the aramid-based composite electric heating material in a precise instrument; the excellent flexibility of the aramid fiber-based composite electric heating material can also be applied to special-shaped pieces, so that the application scene of the composite electric heating paper is further expanded; in addition, the excellent high temperature resistance and flame retardant property of the aramid fiber are utilized to provide necessary guarantee for the safety of the composite electric heating device.
In the invention, the MXene dispersion liquid is smeared on the meta-aramid paper in a mechanical coating mode, so that the coating amount of the MXene dispersion liquid can be accurately controlled, the coating position can be freely controlled, and the designability is strong; in addition, the control of the thickness of the conductive coating can also be achieved by controlling the concentration of the MXene dispersion; secondly, the MXene nano-sheet with metal-level electronic conductivity can realize the rapid heating of the composite electric heating material; the composite electrothermal material can be heated to the highest temperature of 50-140 ℃ within 27-30s under the voltage of 5V, and can be rapidly heated under a complex environment by self-powered by lower driving pressure.
In the invention, the composite electrothermal paper base layer and the conductive layer are tightly combined in a hot-pressing treatment mode, so that the problem of poor bonding force between the traditional composite electrothermal material base layer and the conductive layer is solved; specifically, through hot pressing, the MXene nano sheets on the surface of the paper can be connected more tightly, so that the conductivity and the electric heating performance of the composite electric heating paper are improved; after hot pressing, the aramid fibrids are softened and bonded together, so that the interface bonding strength between the aramid chopped fibers and the aramid fibrids is obviously improved, and a compact reinforced concrete structure is constructed, and the maximum pressure is 80MPa.
In conclusion, the aramid fiber-based composite electric heating material has the advantages of high strength, good electric heating performance, high safety coefficient, wide application scene, simple production process and the like, and can be produced on a large scale.
The above embodiment is only one of the implementation manners capable of implementing the technical solution of the present invention, and the scope of the claimed invention is not limited to the embodiment, but also includes any changes, substitutions and other implementation manners easily recognized by those skilled in the art within the technical scope of the present invention.
Claims (10)
1. The preparation method of the aramid fiber-based composite electric heating material is characterized by comprising the following steps of:
mixing the fibrid of the meta-aramid with the chopped fiber of the meta-aramid, and sequentially carrying out fluffing dispersion, wet forming, squeezing and drying treatment to obtain meta-aramid paper;
coating MXene dispersion liquid on the meta-position aramid paper to obtain m-position aramid paper coated with MXene;
and carrying out hot pressing treatment on the meta-position aramid paper coated with MXene to obtain the aramid-based composite electric heating material.
2. The method for preparing the aramid fiber-based composite electric heating material according to claim 1, wherein the fibrid of the meta-aramid fiber and the chopped fiber of the meta-aramid fiber are mixed according to the mass ratio of (9-4): 1-6.
3. The method for preparing an aramid fiber-based composite electric heating material according to claim 1, wherein a cold pressing treatment process is adopted during the pressing treatment; wherein the cold pressing pressure is 0.2-0.5MPa, and the cold pressing time is 5-15min.
4. The method for preparing an aramid fiber-based composite electric heating material according to claim 1, wherein the concentration of the MXene dispersion is 5-10mg/mL.
5. The method for preparing the aramid fiber-based composite electric heating material according to claim 4, wherein the process of coating the m-aramid fiber paper with the MXene dispersion liquid to obtain m-aramid fiber paper coated with MXene comprises the following steps:
coating the MXene dispersion liquid on the meta-aramid paper in a mode of mechanical coating for a plurality of times; after the water in the paper is removed by vacuum drying after each smearing is finished, the next smearing is carried out.
6. The preparation method of the aramid fiber-based composite electric heating material according to claim 1, wherein the preparation process of the MXene dispersion liquid is as follows:
lithium fluoride, hydrochloric acid solution and Ti 3 AlC 2 Mixing, and carrying out etching reaction to obtain a mixed solution after the reaction;
washing and centrifuging the reacted mixed solution for a plurality of times to remove supernatant until the pH value is neutral, thereby obtaining a neutral solution;
and carrying out ultrasonic treatment and centrifugation on the central solution to obtain the MXene dispersion liquid.
7. The method for preparing the aramid fiber-based composite electric heating material according to claim 1, wherein in the process of carrying out hot pressing treatment on the m-aramid fiber paper coated with MXene, the hot pressing pressure is 1-11MPa, the hot pressing temperature is 150-250 ℃, and the time is 3-15min.
8. An aramid fiber-based composite electric heating material, which is characterized in that the aramid fiber-based composite electric heating material is prepared by the preparation method of the aramid fiber-based composite electric heating material according to any one of claims 1 to 7.
9. The aramid fiber-based composite electric heating material according to claim 8, wherein the tensile strength of the aramid fiber-based composite electric heating material is 40-80MPa, and the electrical conductivity is 400-4500Sm -1 。
10. The aramid fiber-based composite electric heating material according to claim 8 or 9, wherein the aramid fiber-based composite electric heating material can be heated to 50-140 ℃ within 27-30s under 5V voltage.
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| KR20150076667A (en) * | 2013-12-27 | 2015-07-07 | 도레이케미칼 주식회사 | Porous fabriclike aramid heat sheet and preparation method thereof |
| CN113024871A (en) * | 2021-04-06 | 2021-06-25 | 郑州大学 | Preparation method of MXene/polymer composite material capable of being heated by radiation |
| CN113372765A (en) * | 2021-06-28 | 2021-09-10 | 武汉理工大学 | MXene-based electrothermal ink and preparation method and application thereof |
| CN116454534A (en) * | 2023-05-30 | 2023-07-18 | 陕西科技大学 | Aramid nanofiber/conductive coating coated polyolefin composite diaphragm and preparation method and application thereof |
| CN116657443A (en) * | 2023-06-30 | 2023-08-29 | 陕西科技大学 | Meta-aramid fiber functional paper and preparation method and application thereof |
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| KR20150076667A (en) * | 2013-12-27 | 2015-07-07 | 도레이케미칼 주식회사 | Porous fabriclike aramid heat sheet and preparation method thereof |
| CN113024871A (en) * | 2021-04-06 | 2021-06-25 | 郑州大学 | Preparation method of MXene/polymer composite material capable of being heated by radiation |
| CN113372765A (en) * | 2021-06-28 | 2021-09-10 | 武汉理工大学 | MXene-based electrothermal ink and preparation method and application thereof |
| CN116454534A (en) * | 2023-05-30 | 2023-07-18 | 陕西科技大学 | Aramid nanofiber/conductive coating coated polyolefin composite diaphragm and preparation method and application thereof |
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