CN117051583A - MXene-based conductive cotton fabric and preparation method thereof - Google Patents
MXene-based conductive cotton fabric and preparation method thereof Download PDFInfo
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- CN117051583A CN117051583A CN202311140489.8A CN202311140489A CN117051583A CN 117051583 A CN117051583 A CN 117051583A CN 202311140489 A CN202311140489 A CN 202311140489A CN 117051583 A CN117051583 A CN 117051583A
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- 239000004744 fabric Substances 0.000 title claims abstract description 135
- 229920000742 Cotton Polymers 0.000 title claims abstract description 121
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title description 8
- 238000011282 treatment Methods 0.000 claims abstract description 52
- 238000001035 drying Methods 0.000 claims abstract description 33
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 26
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000004048 modification Effects 0.000 claims abstract description 21
- 238000012986 modification Methods 0.000 claims abstract description 21
- 238000005096 rolling process Methods 0.000 claims abstract description 17
- 238000007598 dipping method Methods 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 238000005406 washing Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 28
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 22
- 239000002356 single layer Substances 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000005119 centrifugation Methods 0.000 claims description 14
- 238000005530 etching Methods 0.000 claims description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 238000005374 membrane filtration Methods 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000000835 fiber Substances 0.000 abstract description 17
- 238000003825 pressing Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 239000004020 conductor Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
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- 238000001291 vacuum drying Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
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- 238000004321 preservation Methods 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides an MXene-based conductive cotton fabric and a preparation method thereof, and belongs to the technical field of conductive cotton fabric preparation. The cotton embryo cloth is subjected to pretreatment and modification treatment in sequence to obtain modified cotton fabric; sequentially carrying out dipping, ultrasonic treatment, rolling and pressing treatment and drying on the modified cotton fabric to obtain a cotton fabric covered with MXene; and (3) repeatedly carrying out the operations of dipping, ultrasonic treatment, rolling and pressing treatment and drying on the cotton fabric covered with the MXene for 5-15 times to obtain the MXene-based conductive cotton fabric. The results of the examples show that the conductivity of the MXene-based conductive cotton fabric prepared by the method is improved to about 80%, the uniformity is improved to about 90%, the MXene covered on the fiber surface of the MXene-based conductive cotton fabric is more, the MXene on the fiber surface is more uniform and is completely coated, and the MXene exists between the fibers to form a good conductive path.
Description
Technical Field
The invention relates to the technical field of conductive cotton fabric preparation, in particular to an MXene-based conductive cotton fabric and a preparation method thereof.
Background
MXene, a transition metal carbide, nitride, and carbonitride, was discovered in 2011 to be a new two-dimensional (2D) nanomaterial. MXene not only has ultra-high conductivity similar to metals, but also has excellent mechanical properties, its hydrophilic surface and highly tunable surface groups make it easier to form composites with other materials.
There are two main methods for preparing conductive textiles. The first method is a direct coating method, wherein a conductive material is coated on the surface of the fabric to enable the fabric to have conductivity, the process for preparing the conductive fabric by the method is simple, the conductive material has high selectivity and low cost, and the conductive fabric is suitable for mass production, but the conductive fabric prepared by the simple coating method has the defects of poor adhesion fastness of the conductive material on the fabric, easy falling off, poor conductive performance, poor washing resistance and influence on the air permeability of the fabric. The second is to blend the conductive fiber with the common fiber by a certain means to process the conductive fiber into the conductive fabric, the method has high cost and complex preparation process, and is not suitable for mass production.
Therefore, how to improve the adhesion fastness of the conductive material on the fabric, so that the conductive material has excellent conductivity and reduces the production cost is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide an MXene-based conductive cotton fabric and a preparation method thereof, and the MXene-based conductive cotton fabric prepared by the preparation method provided by the invention has excellent conductivity and uniformity, is more firmly combined with MXene, has a certain washing fastness, and is simple in preparation method and low in cost.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an MXene-based conductive cotton fabric, which comprises the following steps:
(1) Pretreating and modifying cotton embryo cloth in sequence to obtain modified cotton fabric;
(2) Sequentially carrying out dipping, ultrasonic treatment, rolling treatment and drying on the modified cotton fabric obtained in the step (1) to obtain a cotton fabric covered with MXene;
(3) Repeating the operation of the step (2) for 5-15 times to obtain the MXene-based conductive cotton fabric;
the modifier used in the modification treatment in the step (1) is an aqueous solution of gamma-aminopropyl triethoxysilane;
the impregnating solution used for the impregnation in the step (2) is a single-layer MXene dispersion solution.
Preferably, the pretreatment in the step (1) is as follows: soaking cotton embryo cloth in ethanol water solution for ultrasonic cleaning, and then drying.
Preferably, the volume ratio of ethanol to water in the aqueous solution of ethanol is (30-60): (100-150).
Preferably, the volume ratio of the gamma-aminopropyl triethoxysilane to water in the aqueous solution of the gamma-aminopropyl triethoxysilane in the step (1) is (5-10): (200-400).
Preferably, the temperature of the modification treatment in the step (1) is 60-80 ℃, and the time of the modification treatment is 1-5 h.
Preferably, the power of the ultrasonic treatment in the step (2) is 450-550W, the ultrasonic treatment time is 50-90 s, and the ultrasonic treatment is performed under the ice bath condition.
Preferably, the concentration of the monolayer MXene dispersion in the step (2) is (2-5) mg/mL.
Preferably, the preparation method of the single-layer MXene dispersion liquid in the step (2) comprises the following steps:
1) Will be front MAX phase Ti 3 AlC 2 Mixing with LiF hydrochloric acid solution for etching, and then sequentially carrying out centrifugation, acid washing, water washing, filter membrane filtration and drying treatment to obtain a multilayer MXene;
2) And (2) mixing the multi-layer MXene obtained in the step (1) with water, then carrying out gas washing treatment, and then sequentially carrying out ultrasonic dispersion and centrifugation to obtain a single-layer MXene dispersion liquid.
Preferably, the ratio of the mass of LiF in the hydrochloric acid solution of LiF in step 1) to the volume of hydrochloric acid is (3-4) g: (40-50) mL.
The invention provides the MXene-based conductive cotton fabric prepared by the preparation method.
The invention provides a preparation method of an MXene-based conductive cotton fabric, which comprises the following steps:
(1) Pretreating and modifying cotton embryo cloth in sequence to obtain modified cotton fabric; (2) Sequentially carrying out dipping, ultrasonic treatment, rolling treatment and drying on the modified cotton fabric obtained in the step (1) to obtain a cotton fabric covered with MXene; (3) Repeating the operation of the step (2) for 5-15 times to obtain the MXene-based conductive cotton fabric; the modifier used in the modification treatment in the step (1) is an aqueous solution of gamma-aminopropyl triethoxysilane; the impregnating solution used for the impregnation in the step (2) is a single-layer MXene dispersion solution. The cotton embryo cloth is pretreated, impurities on the surface of the cotton embryo cloth can be removed, then gamma-aminopropyl triethoxysilane (KH 550) is adopted to modify the cotton fabric, and the surface of the cotton fabric can be coupled with MXene, so that the MXene and the cotton fabric are better combined in the subsequent steps; the ultrasonic treatment can improve the adhesive force of the coating and the bonding fastness in the fabric impregnation process, can reduce the deposition amount of MXene on the surface of the fabric, is beneficial to improving the air permeability and comfort of the fabric, reduces the overall production cost, and can improve the drying rate and quality of the fabric in the later-stage fabric drying process; the MXene on the cotton fiber can be initially fixed by the rolling treatment, the adhesion force of the MXene on the cotton fiber surface can be further improved due to the rough surface of the fabric, and the friction force generated in the rolling process enables the MXene to be in close contact with the cotton fiber; the ultrasonic auxiliary padding method is adopted, and ultrasonic waves are utilized to carry out auxiliary dipping and matched rolling treatment, so that dipping efficiency can be improved, and coating quality and uniformity can be improved. The results of the examples show that the conductivity of the MXene-based conductive cotton fabric prepared by the preparation method provided by the invention is improved to about 80%, the uniformity is improved by about 90%, the surface of the prepared MXene-based conductive cotton fabric is more covered with MXene, the surface of the fiber is more uniform and is completely coated, and the MXene exists between the fibers to form a good conductive path.
Drawings
FIG. 1 is a scanning electron microscope image of an MXene-based conductive cotton fabric prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the MXene-based conductive cotton fabric prepared in comparative example 2.
Detailed Description
The invention provides a preparation method of an MXene-based conductive cotton fabric, which comprises the following steps:
(1) Pretreating and modifying cotton embryo cloth in sequence to obtain modified cotton fabric;
(2) Sequentially carrying out dipping, ultrasonic treatment, rolling treatment and drying on the modified cotton fabric obtained in the step (1) to obtain a cotton fabric covered with MXene;
(3) And (3) repeating the operation of the step (2) for 5-15 times to obtain the MXene-based conductive cotton fabric.
In the present invention, the raw materials used are commercially available products well known to those skilled in the art unless otherwise specified.
The cotton embryo cloth is subjected to pretreatment and modification in sequence to obtain the modified cotton fabric.
In the present invention, the cotton blanket preferably has a warp density of 5*5 to 60 and a weft density of 50 to 70, more preferably 5*5 to 70, and a weft density of 60. The invention is convenient to operate by controlling the size of the cotton embryo cloth.
In the present invention, the pretreatment is preferably performed by: soaking cotton embryo cloth in ethanol water solution for ultrasonic cleaning, and then drying; the power of the ultrasonic cleaning is preferably 450-550W, more preferably 450-500W; the ultrasonic cleaning time is preferably 30 to 60 minutes, more preferably 30 to 50 minutes, and even more preferably 30 to 40 minutes; the drying is preferably performed in a vacuum environment. The specific temperature and time of the drying are not particularly limited, and the product can be completely dried without damaging the product according to the technical common knowledge of the person skilled in the art. According to the invention, the cotton embryo cloth is pretreated, so that impurities on the surface of the cotton embryo cloth can be removed; by carrying out pretreatment under the ultrasonic condition and controlling ultrasonic parameters, impurities can be further removed, and the treatment effect is improved.
In the present invention, the volume ratio of ethanol to water in the aqueous ethanol solution is preferably (30 to 60): (100 to 150), more preferably 50:100. in the present invention, the water is preferably deionized water. The invention can further improve the treatment effect by controlling the volume ratio of ethanol to water.
The invention has no special limitation on the dosage relation of the cotton embryo cloth and the ethanol aqueous solution, and can ensure that the cotton embryo cloth is completely soaked in the ethanol aqueous solution.
In the invention, the modifier used in the modification treatment is an aqueous solution of gamma-aminopropyl triethoxysilane; the volume ratio of the gamma-aminopropyl triethoxysilane to water in the aqueous solution of the gamma-aminopropyl triethoxysilane is preferably (5-10): (200 to 400), more preferably (5 to 8): (200 to 300), more preferably 5:200. in the present invention, the water is preferably deionized water. According to the invention, the cotton fabric is modified by adopting gamma-aminopropyl triethoxysilane (KH 550), so that the surface of the cotton fabric can be coupled with MXene, and the MXene and the cotton fabric can be better combined in the subsequent steps; the bonding of MXene to cotton fabric can be further promoted by controlling the concentration of gamma-aminopropyl triethoxysilane.
In the present invention, the preparation method of the aqueous solution of gamma-aminopropyl triethoxysilane is preferably as follows: the vessel was preheated to 60-80 ℃ and then gamma-aminopropyl triethoxysilane (KH 550) and water were added to the vessel to mix. According to the invention, by adopting the mode, the gamma-aminopropyl triethoxysilane and water can be uniformly mixed, and the subsequent modification treatment is convenient.
The invention has no special limitation on the dosage relation of the cotton embryo cloth and the aqueous solution of the gamma-aminopropyl triethoxysilane, and can ensure that the cotton embryo cloth is completely soaked in the aqueous solution of the gamma-aminopropyl triethoxysilane.
In the present invention, the temperature of the modification treatment is preferably 60 to 80 ℃, more preferably 70 ℃; the time of the modification treatment is preferably 1 to 5 hours, more preferably 2 to 4 hours. The invention can further promote the combination of MXene and cotton fabrics by controlling the temperature and time of the modification treatment.
After the modification treatment is finished, the product of the modification treatment is preferably dried. In the present invention, the drying is preferably performed in a vacuum environment. The specific temperature and time of the drying are not particularly limited, and the product can be completely dried without damaging the product according to the technical common knowledge of the person skilled in the art.
After the modified cotton fabric is obtained, the modified cotton fabric is sequentially subjected to dipping, ultrasonic treatment, rolling treatment and drying, and the cotton fabric covered with MXene is obtained.
In the present invention, the impregnating solution used for the impregnation is a single-layer MXene dispersion solution, and the preparation method of the single-layer MXene dispersion solution preferably includes the following steps:
1) Will be front MAX phase Ti 3 AlC 2 Mixing with LiF hydrochloric acid solution for etching, and then sequentially carrying out centrifugation, acid washing, water washing, filter membrane filtration and drying treatment to obtain a multilayer MXene;
2) And (2) mixing the multi-layer MXene obtained in the step (1) with water, then carrying out gas washing treatment, and then sequentially carrying out ultrasonic dispersion and centrifugation to obtain a single-layer MXene dispersion liquid.
The invention preferably uses the pre-MAX phase Ti 3 AlC 2 Mixing with LiF hydrochloric acid solution for etching, and then sequentially carrying out centrifugation, acid washing, water washing, filter membrane filtration and drying treatment to obtain the multilayer MXene.
In the present invention, the ratio of the mass of LiF in the hydrochloric acid solution of LiF to the volume of hydrochloric acid is preferably (3 to 4) g: (40-50) mL, more preferably (3.2-3.5) g: (40-45) mL. The invention can better control the etching rate by controlling the mass of LiF and the volume ratio of hydrochloric acid, thereby avoiding the problems of over etching or under etching.
In the present invention, the concentration of the hydrochloric acid is preferably 9M. The invention can further control the etching rate by controlling the hydrochloric acid concentration, thereby improving the etching efficiency.
In the present invention, the preparation method of the hydrochloric acid solution of LiF preferably comprises: mixing hydrochloric acid and LiF, preheating in water bath, and stirring for 15-20 min. In the invention, the water bath preheating temperature is preferably 20-50 ℃, more preferably 30-40 ℃; the stirring mode is preferably magnetic stirring. According to the invention, the LiF hydrochloric acid solution is prepared in the mode, so that LiF and hydrochloric acid can be uniformly mixed, and a foundation can be laid for subsequent etching.
In the present invention, the pre-MAX phase Ti 3 AlC 2 The mass ratio to LiF is preferably (2-3): (3 to 4), more preferably (2 to 2.5): (3.2-3.5). The invention is realized by controlling the front MAX phase Ti 3 AlC 2 The etching effect can be further improved by the mass ratio with LiF.
In the present invention, the pre-MAX phase Ti 3 AlC 2 The mixing with the hydrochloric acid solution of LiF is preferably carried out under stirring; the stirring mode is preferably magnetic stirring; the stirring time is preferably 36 to 48 hours, more preferably 42 to 48 hours. The invention can ensure the mixing time of Ti by controlling the mixing time 3 AlC 2 And performing full etching.
In the present invention, the rate of centrifugation is preferably 3500 to 4000r/min, more preferably 3500 to 3600r/min; the time for the centrifugation is preferably 1 to 5 minutes, more preferably 3 to 4 minutes.
In the invention, the pickling agent used for pickling is preferably 2M hydrochloric acid; the number of times of the acidity is preferably 3 to 4.
In the present invention, the solvent used for the water washing is preferably deionized water; the number of times of water washing is preferably 6-8 times; the pH value of the water washing product is preferably 6 to 7.
In the present invention, the filter membrane used for the filtration is preferably a 0.22 μm aqueous filter membrane; the filter membrane is preferably used for filtering, and is preferably pumped by a circulating water vacuum pump.
In the present invention, the temperature of the drying treatment is preferably 40 to 80 ℃, more preferably 60 to 80 ℃; the drying treatment is preferably performed in a vacuum environment.
According to the invention, through sequentially carrying out centrifugation, acid washing, water washing, filter membrane filtration and drying treatment on the etched product, impurities in the product can be removed, so that the high-purity multilayer MXene is obtained.
After the multi-layer MXene is obtained, the multi-layer MXene is preferably placed into a plastic package bag, nitrogen is filled, then a layer of plastic package bag is sleeved, a drying agent is added, and the multi-layer MXene is placed into a drying bottle for storage. The invention can avoid the oxidation of the multi-layer MXene and prolong the preservation time of the multi-layer MXene by preserving in the mode.
After the multi-layer MXene is obtained, the multi-layer MXene and water are preferably mixed and then subjected to gas washing treatment, and then ultrasonic dispersion and centrifugation are sequentially carried out to obtain the single-layer MXene dispersion liquid.
In the present invention, the mass and water volume ratio of the multi-layered MXene is preferably (0.3 to 0.5) g:100mL, more preferably 0.4g:100mL. The invention can control the concentration of the single-layer MXene dispersion liquid by controlling the dosage relation of the two.
In the present invention, the gas washing treatment is preferably performed in a gas washing cylinder; preferably, nitrogen is continuously introduced in the gas washing treatment process; the time of the gas washing treatment is preferably 1 to 5 minutes, more preferably 1 to 3 minutes. The invention can reduce the oxidation of the MXene when preparing the single-layer MXene dispersion liquid through gas washing treatment.
In the present invention, the ultrasonic dispersion is preferably performed in an ice bath environment; the power of the ultrasonic dispersion is preferably 450-550W, more preferably 450-500W; the ultrasonic dispersion time is preferably 30-60 min, more preferably 30-40 min; in the ultrasonic dispersion process, the gas washing bottle is preferably rocked every 10-15 min to shake the bottom sediment uniformly.
In the present invention, the rate of centrifugation is preferably 2500 to 5000r/min, more preferably 3000 to 4500r/min, still more preferably 3500 to 4000r/min; the time for the centrifugation is preferably 20 to 50 minutes, more preferably 30 to 40 minutes.
The present invention allows the separation of multiple layers of MXene by ultrasonic dispersion and high speed centrifugation to form a single layer MXene dispersion.
In the present invention, the concentration of the monolayer MXene dispersion is preferably (2-5) mg/mL, more preferably (3-4) mg/mL.
In the present invention, the time for the impregnation is preferably 1 to 5 minutes, more preferably 2 to 4 minutes.
In the present invention, the power of the ultrasonic treatment is preferably 450 to 550W, more preferably 450 to 500W; the time of the ultrasonic treatment is preferably 50 to 90 seconds, more preferably 60 to 80 seconds, still more preferably 70 seconds; the sonication is preferably performed in an ice bath environment.
The specific operation of the rolling treatment is not particularly limited, and may be any operation known to those skilled in the art.
In the present invention, the temperature of the drying is preferably 60 to 90 ℃, more preferably 70 to 80 ℃; the drying time is preferably 5 to 20 minutes, more preferably 10 to 15 minutes.
After the MXene-covered cotton fabric is obtained, the method repeats the operations of dipping, ultrasonic treatment, rolling and pressing treatment and drying for 5 to 15 times on the MXene-covered cotton fabric to obtain the MXene-based conductive cotton fabric
In the present invention, the number of times of repeating the operations of immersing, ultrasonic treating, rolling and drying is preferably 8 to 12 times, more preferably 10 times. Through multiple treatments, the invention can lead the prepared MXene-based conductive cotton fabric to have more MXene covered on the fiber surface, lead the MXene on the fiber surface to be more uniform and completely cover, lead the MXene to exist among the fibers and form a good conductive path.
The cotton embryo cloth is pretreated, impurities on the surface of the cotton embryo cloth can be removed, then gamma-aminopropyl triethoxysilane (KH 550) is adopted to modify the cotton fabric, and the surface of the cotton fabric can be coupled with MXene, so that the MXene and the cotton fabric are better combined in the subsequent steps; the ultrasonic treatment can improve the adhesive force of the coating and the bonding fastness in the fabric impregnation process, can reduce the deposition amount of MXene on the surface of the fabric, is beneficial to improving the air permeability and comfort of the fabric, reduces the overall production cost, and can improve the drying rate and quality of the fabric in the later-stage fabric drying process; the MXene on the cotton fiber can be initially fixed by the rolling treatment, the adhesion force of the MXene on the cotton fiber surface can be further improved due to the rough surface of the fabric, and the friction force generated in the rolling process enables the MXene to be in close contact with the cotton fiber; the ultrasonic auxiliary padding method is adopted, and ultrasonic waves are utilized to carry out auxiliary dipping and matched rolling treatment, so that dipping efficiency can be improved, and coating quality and uniformity can be improved.
The invention provides the MXene-based conductive cotton fabric prepared by the preparation method. The MXene-based conductive cotton fabric provided by the invention has the advantages of good conductivity, high uniformity, more MXene covered on the fiber surface of the MXene-based conductive cotton fabric, more uniform MXene on the fiber surface, complete coating, existence of MXene between fibers, good conductive paths, and firm combination of the cotton fabric and the MXene, and certain washing fastness.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the MXene-based conductive cotton fabric comprises the following steps:
(1) Sequentially carrying out pretreatment and modification treatment on cotton embryo cloth, and finally carrying out vacuum drying to obtain modified cotton fabric; the size of the cotton blanket is 5*5 warp density 70 and weft density 60;
(2) Sequentially carrying out dipping, ultrasonic treatment, rolling treatment and vacuum drying on the modified cotton fabric obtained in the step (1) to obtain a cotton fabric covered with MXene;
(3) Repeating the operation of the step (2) 10 times for the MXene-covered cotton fabric obtained in the step (2) to obtain the MXene-based conductive cotton fabric;
the pretreatment mode in the step (1) is as follows: soaking cotton embryo cloth in ethanol water solution for ultrasonic cleaning, and then placing into a vacuum box for drying; the volume ratio of the ethanol to deionized water in the ethanol aqueous solution is 50:100; the power of the ultrasonic cleaning is 450W, and the time of the ultrasonic cleaning is 30min;
the modifier used in the modification treatment in the step (1) is an aqueous solution of gamma-aminopropyl triethoxysilane, and the volume ratio of the gamma-aminopropyl triethoxysilane to deionized water is 5:200; the temperature of the modification treatment is 70 ℃, and the time of the modification treatment is 2 hours; the preparation method of the aqueous solution of the gamma-aminopropyl triethoxysilane comprises the following steps: preheating a container to 70 ℃, and then adding gamma-aminopropyl triethoxysilane and deionized water into the container for mixing;
the dipping liquid used in the step (2) is single-layer MXene dispersion liquid with the concentration of 3mg/mL, and the dipping time is 2min; the power of the ultrasonic treatment is 450W, the ultrasonic treatment time is 70s, and the ultrasonic treatment is performed in an ice bath environment; the temperature of the vacuum drying is 80 ℃, and the time of the vacuum drying is 10min;
the preparation method of the single-layer MXene dispersion liquid comprises the following steps:
1) Mixing 40mL of 9M hydrochloric acid and 3.2g of LiF, preheating in water bath at 40deg.C, magnetically stirring for 15min to obtain LiF hydrochloric acid solution, and adding 2g of pre-MAX phase Ti 3 AlC 2 Mixing, etching, centrifuging in a centrifuge at 3500r/min for 1min, washing with 2M hydrochloric acid for 3 times, washing with deionized water for 7 times, drying with 0.22 μm water-based filter membrane by using a circulating water vacuum pump, and drying in a vacuum environment at 60deg.C to obtain multilayer MXene; the front MAX phase Ti 3 AlC 2 Mixing with LiF hydrochloric acid solution under magnetic stirring for 48h;
2) Taking 0.3g of the multilayer MXene obtained in the step 1) and 100mL of water, putting into a gas washing bottle, mixing to obtain a dispersion liquid, continuously introducing nitrogen to perform gas washing treatment for 1min, and performing ultrasonic dispersion and centrifugation under ice bath conditions to obtain a single-layer MXene dispersion liquid; the power of ultrasonic dispersion is 450W, the time of ultrasonic dispersion is 30min, and the bottom sediment is uniformly shaken by shaking the gas washing cylinder every 10min in the ultrasonic dispersion process; the centrifugal speed is 3500r/min, and the centrifugal time is 30min; the concentration of the monolayer MXene dispersion was 3mg/mL.
The performance of the MXene-based conductive cotton fabric prepared in example 1 was tested, the average resistance value of the conductive cotton fabric was used to represent the conductivity of the MXene-based conductive cotton fabric, the deviation value of the resistance value of each point on the surface of the MXene-based conductive cotton fabric was used to represent the uniformity of MXene distribution on the surface of the MXene-based conductive cotton fabric, and the average resistance value of the MXene-based conductive cotton fabric prepared in example 1 was tested to be 4kΩ, and the deviation value was 0.4.
Example 2
The time of the ultrasonic treatment in the step (2) was 50s, and the other conditions were the same as in example 1.
The performance of the MXene-based conductive cotton fabric prepared in example 2 was tested, and the MXene-based conductive cotton fabric prepared in example 2 had an average resistance value of 42kΩ and a deviation value of 28.
Comparative example 1
The time of the ultrasonic treatment in the step (2) was 40s, and the other conditions were the same as in example 1.
The performance of the MXene-based conductive cotton fabric prepared in comparative example 1 was tested, and the average resistance value of the MXene-based conductive cotton fabric prepared in comparative example 1 was 413kΩ and the deviation value was 382.
Comparative example 2
The operation of the ultrasonic treatment in the step (2) was omitted, and the other conditions were the same as in example 1.
The performance of the MXene-based conductive cotton fabric prepared in comparative example 2 was tested, and the MXene-based conductive cotton fabric prepared in comparative example 2 had an average resistance value of 11kΩ and a deviation value of 16.
As can be seen from the comparison of examples 1-2 and comparative examples 1-2, if the ultrasonic cleaning time is shorter, the conductivity and uniformity of the MXene-based conductive cotton fabric are worse, because the MXene is more dispersed on the surface of the fabric due to the ultrasonic effect, and as the ultrasonic time increases, more MXene is combined on the surface of the cotton fabric and uniformly distributed, part of MXene permeates into the pores of the cotton fabric to form conductive paths between fibers, thereby improving the conductivity, and being more superior to the MXene-based cotton fabric prepared in a mode of not performing ultrasonic treatment.
Fig. 1 is a scanning electron microscope image of an MXene-based conductive cotton fabric prepared in example 1 of the present invention, and fig. 2 is a scanning electron microscope image of an MXene-based conductive cotton fabric prepared in comparative example 2. As can be seen from a comparison of fig. 1 and 2, the size of the MXene sheets on the surface of the sonicated and non-sonicated MXene-based conductive cotton fabric fibers is comparable, whereas the non-sonicated MXene cotton fabric fibers have more bark-like defects not covered by MXene and are unevenly distributed, and thus are weaker in electrical conductivity than the sonicated MXene cotton fabric.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the MXene-based conductive cotton fabric comprises the following steps:
(1) Pretreating and modifying cotton embryo cloth in sequence to obtain modified cotton fabric;
(2) Sequentially carrying out dipping, ultrasonic treatment, rolling treatment and drying on the modified cotton fabric obtained in the step (1) to obtain a cotton fabric covered with MXene;
(3) Repeating the operation of the step (2) for 5-15 times to obtain the MXene-based conductive cotton fabric;
the modifier used in the modification treatment in the step (1) is an aqueous solution of gamma-aminopropyl triethoxysilane;
the impregnating solution used for the impregnation in the step (2) is a single-layer MXene dispersion solution.
2. The method according to claim 1, wherein the pretreatment in step (1) is performed by: soaking cotton embryo cloth in ethanol water solution for ultrasonic cleaning, and then drying.
3. The preparation method according to claim 2, wherein the volume ratio of ethanol to water in the aqueous solution of ethanol is (30-60): (100-150).
4. The method according to claim 1, wherein the volume ratio of γ -aminopropyl triethoxysilane to water in the aqueous solution of γ -aminopropyl triethoxysilane in step (1) is (5 to 10): (200-400).
5. The method according to claim 1, wherein the temperature of the modification treatment in the step (1) is 60 to 80 ℃ and the time of the modification treatment is 1 to 5 hours.
6. The method according to claim 1, wherein the power of the ultrasonic treatment in the step (2) is 450 to 550W, the time of the ultrasonic treatment is 50 to 90s, and the ultrasonic treatment is performed under ice bath conditions.
7. The method according to claim 1, wherein the concentration of the monolayer MXene dispersion in the step (2) is (2 to 5) mg/mL.
8. The method according to claim 1 or 7, wherein the method for preparing the single-layer MXene dispersion in step (2) comprises the steps of:
1) Will be front MAX phase Ti 3 AlC 2 Mixing with LiF hydrochloric acid solution for etching, and then sequentially carrying out centrifugation, acid washing, water washing, filter membrane filtration and drying treatment to obtain a multilayer MXene;
2) And (2) mixing the multi-layer MXene obtained in the step (1) with water, then carrying out gas washing treatment, and then sequentially carrying out ultrasonic dispersion and centrifugation to obtain a single-layer MXene dispersion liquid.
9. The method according to claim 8, wherein the ratio of the mass of LiF in the hydrochloric acid solution of LiF in step 1) to the volume of hydrochloric acid is (3-4) g: (40-50) mL.
10. The MXene-based conductive cotton fabric prepared by the preparation method of any one of claims 1 to 9.
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