CN112011094A - Nano cellulose MXene gel and preparation method and application thereof - Google Patents
Nano cellulose MXene gel and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nano-cellulose MXene gel and a preparation method and application thereof, and belongs to the technical field of two-dimensional materials. Uniformly mixing a two-dimensional transition metal carbonitride aqueous dispersion and a carboxylated nanocellulose aqueous dispersion, freezing, and thawing to form hydrogel; freezing and drying the hydrogel to obtain aerogel; wherein the molecular formula of the two-dimensional transition metal carbonitride is Mn+1XnTs(ii) a Wherein M is a transition metal, X is carbon and/or nitrogen, TsIs a surface terminal group containing hydroxyl, fluorine, oxygen, hydrogen, alkyl, ammonium orCombinations thereof. The obtained hydrogel and aerogel material have good application in the fields of supercapacitors, lithium ion batteries, electromagnetic shielding and electrocatalysis.
Description
Technical Field
The invention belongs to the technical field of two-dimensional materials, and particularly relates to a two-dimensional transition metal carbonitride (MXene) and nanocellulose composite gel, and a preparation method and application thereof.
Background
The two-dimensional transition metal carbonitride (MXene) is a novel two-dimensional material obtained by removing an A atomic layer from a MAX phase of a layered ceramic material, has the thickness of only about 1nm, has excellent conductivity and water dispersibility, has excellent application prospects in the fields of supercapacitors, lithium ion batteries, conductive coatings, electromagnetic shielding, electrocatalysis, adsorption and the like, is called aqueous graphene, and is a two-dimensional material which is developed after the graphene and has the fastest variety.
The most widely used titanium-based metal carbide materials reported to date are those made of Ti, for example3AlC2Etch prepared Ti3C2TsMaterial and Ti2Ti prepared by AlC etching2CTs. The former is MXene material which is most widely researched and most applied at present, the conductivity of the MXene material can reach 15000S/cm, and the capacitance of the MXene material can reach 1000F/cm3Or above, the conductive coating has attracted much attention in the fields of super capacitors, lithium ion batteries, conductive coatings, electromagnetic shielding and the like. Most MXene tends to get a few layers of dispersion dispersed in water during preparation by etching and intercalation. In the application process, whether the electrode material, the conductive paint or the electromagnetic shielding material is used, the electrode material, the conductive paint or the electromagnetic shielding material needs to be dispersed in a solvent, and the electrode material, the conductive paint or the electromagnetic shielding material is most commonly dispersed in water.
However, their electrochemical performance is greatly reduced by the loss of available surface area and the increase of ionic diffusion resistance due to random stacking of MXene Nanoplates (NSs). Graphene faces the same problems, but its self-assembly into a 3D structure can effectively solve these problems.
Cellulose is a renewable, non-toxic and biodegradable natural polymer, and is an inexhaustible natural renewable resource. It can even replace fossil energy in many ways. Cellulose has been widely used in many industries, and especially hydrogels and aerogels prepared from cellulose have attracted more and more attention. The hydrogel has a three-dimensional network structure, and the dispersion medium is water inside the structure, and the water in the medium is removed and replaced by air, and meanwhile, the three-dimensional network structure of the hydrogel is not changed, so that the aerogel is obtained. In recent years, cellulose aerogels have been widely studied in the direction of transportation, oil-water separation, sewage treatment, sensors, and the like, because of their uniform three-dimensional network structure.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of two-dimensional transition metal carbonitride (MXene) nano cellulose hydrogel and aerogel, and the specific technical scheme is as follows:
uniformly mixing a two-dimensional transition metal carbonitride aqueous dispersion and a carboxylated nano cellulose aqueous dispersion, freezing, and thawing to form hydrogel; freezing and drying the hydrogel to obtain aerogel; wherein the molecular formula of the two-dimensional transition metal carbonitride is Mn+1XnTs(ii) a Wherein M is a transition metal, X is carbon and/or nitrogen, n represents the sum of carbon and/or nitrogen atoms, TsThe surface end group is one or the combination of more than two of hydroxyl, fluorine, oxygen, hydrogen, alkyl and ammonium. And the quaternized nanocellulose and the two-dimensional transition metal carbonitride dispersion liquid are mixed, so that agglomeration occurs, and the hydrogel cannot be obtained. In addition, the mixed solution of the carboxylated nanocellulose and the two-dimensional transition metal carbonitride, which is left at room temperature without freezing, cannot form a gel.
In one embodiment of the invention, the mass ratio of carboxylated nanocellulose to two-dimensional transition metal carbonitride is between 20:1 and 1: 20;
in one embodiment of the invention, the concentration of the aqueous dispersion of carboxylated nanocellulose is from 0.1 to 50mg/g and the concentration of the aqueous dispersion of two-dimensional transition metal carbonitride is from 0.1 to 60 mg/g.
In one embodiment of the invention, the freezing temperature is from-198 to-5 degrees; the freezing time is 30min-48 h.
In one embodiment of the present invention, the transition metal in the two-dimensional transition metal carbonitride is at least one of Ti, V, Cr, Sc, Zr, Nb, Mo, Hf, and Ta.
In one embodiment of the invention, the two-dimensional transition metal carbonitride is selected from Ti3C2Ts、Ti2CTs、V2CTs、Cr2CTs、Sc2CTs、Zr2CTs、Mo2CTs、Mo2TiC2Ts、Hf2CTs、Ta2CTs、Ti3CNTs、Nb2CTs、TiyNb2-yCTsOr VyNb2-yCTs(ii) a Wherein, 0<y<2。
The hydrogel and the aerogel prepared by the method have good application in the fields of super capacitors, lithium ion batteries, electromagnetic shielding, electrocatalysis and the like.
The invention has the beneficial effects that:
the method provided by the invention provides a simple and effective method for preparing MXene-nanocellulose hydrogel and aerogel, and the hydrogel can be obtained only by freezing and unfreezing the mixed dispersion liquid of the two substances. The aerogel is prepared after freeze-drying. Compared with MXene, the aerogel has larger specific surface area and better rate performance when being used as a supercapacitor electrode material. Can be applied to the fields of preparing super capacitors, lithium ion batteries, electromagnetic shielding and electrocatalysis, and has wide prospect.
Drawings
FIG. 1 shows XRD patterns of aerogels obtained in examples 1, 2 and 3.
FIG. 2 is a scanning electron micrograph of the aerogel obtained in example 2.
FIG. 3 is a cyclic voltammogram of the aerogel obtained in example 2.
FIG. 4 is a scanning electron micrograph of the aerogel obtained in example 3.
FIG. 5 is a cyclic voltammogram of the aerogel obtained in example 3.
Fig. 6 is a cyclic voltammogram of the MXene film obtained in comparative example 1.
Detailed Description
The technical solution of the present invention will be described in detail by specific examples.
Example 1
In-situ generation of HF vs Ti using HCl and LiF3AlC2And etching is carried out. 2g LiF are completely dissolved in 30mL of 9mol/L HCl solution, and then 1g Ti is slowly added under magnetic stirring3AlC2And reacting at 35 ℃ for 24 h. After the reaction is finished, the product is centrifugally washed by deionized water until the pH value is more than 6. The obtained precipitate is multilayer Ti3C2TxDispersing the mixture in 100mL of deoxygenated water, performing ice-water bath ultrasound for 0.5h under the protection of argon, and then performing ultrasonic treatment on the obtained dispersion liquid for 3500r min-1Is centrifuged for 1h at the rotating speed, and the stable black dispersion liquid at the upper layer is few-layer or single-layer Ti3C2TxThe formed colloid is dissolved. The concentration is adjusted to 5mg ml by diluting with water-1. Mixing with carboxylated nano-cellulose solution (concentration is 6mg ml) prepared by TEMPO oxidation method-1) Mixing the materials in a transparent sample bottle according to a certain mass ratio to obtain NFC-Ti3C2TxAnd magnetically stirring the mixed solution in a mass ratio of 2:1 for 0.5h, then freezing the mixed solution in a refrigerator at the freezing temperature of-20 ℃, taking out the mixed solution after freezing for 2h, and unfreezing the mixed solution at room temperature overnight. After thawing, the sample was found to be hydrogel-like, and the container glass was inverted and the hydrogel did not flow down. The mixed liquid which is not frozen and thawed is still in a liquid state after being placed at room temperature for three days, and no gel is formed.
And freezing the sample of which the gel is confirmed by using liquid nitrogen until the sample is completely frozen, and then putting the sample into a freeze dryer for drying for 48 hours to obtain the light MXene-nanocellulose composite aerogel. For convenience, the NFC is mixed with M-Ti3C2TxThe aerogel obtained when the mass ratio is 2:1 is named as NM-21, the XRD pattern of the aerogel is shown in figure 1(NM-21), and the XRD pattern of the nano-cellulose is shown in figure 1 (NC).
Example 2
Same as example 1, but the mixed solution is mixed with NFC and Ti3C2TxAdjusting the mass ratio to be 1:3, magnetically stirring for 0.5h, then placing the mixture in a refrigerator for freezing at the temperature of-20 ℃, taking out the mixture after freezing for 2h, and unfreezing at room temperature overnight. After thawing, the sample was found to be hydrogel-like, and the container glass was inverted and the hydrogel did not flow down. Freezing the sample with the gel confirmed by liquid nitrogen until the gel is completely frozen, putting the sample into a freeze dryer for drying for 48 hours to obtain the light MXene-nanocellulose composite aerogel, and naming the aerogel as NM-13, wherein the XRD pattern is shown in figure 1(NM-13), and the scanning electron microscope pattern is shown in figure 2. The aerogel was cut into disks for electrochemical testing, used as a counter electrode over a capacitive activated carbon membrane, Hg/Hg2SO4The electrode was used as a reference electrode, Celgard3501 was used as a separator, and the electrolyte was 3mol/L H2SO4Cyclic Voltammetry (CV) tests were performed for the assembled three-electrode Swagelok cells, with the CV curves shown in fig. 3. From the figure, it can be calculated that s is 5mV-1The specific capacitance at the smaller scanning rate of (2) is 132F g respectively-1When the scan rate is from 5mV s-1Increase to 500mV s-1When the specific capacitance is 95F g-And 72% at 5 mV/s. The multiplying power performance of the film is obviously better than that of the simple MXene film in the comparative example 1.
Example 3
Same as example 1, but the mixed solution is mixed with NFC and Ti3C2TxAdjusting the mass ratio to be 1:5, magnetically stirring for 0.5h, then placing the mixture in a refrigerator for freezing at the temperature of-20 ℃, taking out the mixture after freezing for 2h, and unfreezing at room temperature overnight. After thawing, the sample was found to be hydrogel-like, and the container glass was inverted and the hydrogel did not flow down. A sample solution for confirming the gelAnd (3) freezing by nitrogen, putting the obtained product into a freeze dryer for drying for 48 hours after complete freezing to obtain the light MXene-nanocellulose composite aerogel, and naming the aerogel as NM-15, wherein an XRD (X-ray diffraction) spectrum of the aerogel is shown in figure 1(NM-13), and a Scanning Electron Microscope (SEM) spectrum of the aerogel is shown in figure 4. The aerogel was cut into disks for electrochemical testing, used as a counter electrode over a capacitive activated carbon membrane, Hg/Hg2SO4The electrode was used as a reference electrode, Celgard3501 was used as a separator, and the electrolyte was 3mol/L H2SO4Cyclic Voltammetry (CV) tests were performed for the assembled three-electrode Swagelok cells, with the CV curves shown in fig. 5. From the figure, it can be calculated that s is 5mV-1188F g at a smaller scanning rate-1When the scan rate is from 5mV s-1Increase to 500mV s-1The specific capacitance is 125F g-And 66.5% at 5 mV/s. The multiplying power performance of the film is obviously better than that of the simple MXene film in the comparative example 1.
Comparative example 1
0.8g LiF was added to 10mL 9M HCl and stirred well, followed by 0.5g Ti3AlC2Reacting at room temperature for 24h, washing the product with deionized water until the pH is more than 5, and then adding 100g of deionized water; by hand shaking, Ti stably dispersed in water was obtained3C2Ts(ii) a Vacuum filtering the black uniform liquid on the upper layer, naturally drying, and separating from the filter membrane to obtain Ti3C2TsA film.
Adding the Ti3C2TsThe film is used as a working electrode, the active carbon film through capacitance is used as a counter electrode, Hg/Hg2SO4The electrode was used as a reference electrode, Celgard3501 was used as a separator, and the electrolyte was 3mol/L H2SO4. CV and CP tests were performed for the assembled three-electrode Swagelok cells, and the test results are shown in fig. 6. From the figure, it can be calculated that s is 5mV-1Is 291F g at a smaller scanning rate-1When the scan rate is from 5mV s-1Increase to 500mV s-1When the specific capacitance is 51F g-And only 17.5% at 5 mV/s.
Comparative example 2
In the same way as example 1, but the carboxylated nanocellulose is changed into the quaternized nanocellulose with the same concentration, the nanocellulose and MXene are mixed according to the mass ratio of 2:1,1:3 and 1:5, and after mixing, the MXene is agglomerated and forms a cluster which is obviously visible to the naked eye in water, so that the stable dispersion of the MXene dispersion liquid is broken by adding the nanocellulose, and the reason that the surface charge of the quaternized nanocellulose is positive and the surface charge of the MXene is negative is supposed to be that the electric double layer is broken, so that the colloid stability is reduced. Thus, hydrogels could not be formed using quaternized nanocellulose and MXene.
Claims (8)
1. A preparation method of nano-cellulose MXene gel is characterized in that a two-dimensional transition metal carbonitride aqueous dispersion and a carboxylated nano-cellulose aqueous dispersion are uniformly mixed, then are frozen and are unfrozen to form hydrogel; freezing and drying the hydrogel to obtain aerogel; wherein the molecular formula of the two-dimensional transition metal carbonitride is Mn+1XnTs(ii) a Wherein M is a transition metal, X is carbon and/or nitrogen, n represents the sum of carbon and/or nitrogen atoms, TsThe surface end group is one or the combination of more than two of hydroxyl, fluorine, oxygen, hydrogen, alkyl and ammonium.
2. The method for preparing the nano-cellulose MXene gel according to claim 1, wherein the mass ratio of the carboxylated nano-cellulose to the two-dimensional transition metal carbonitride is between 20:1 and 1: 20.
3. The method for preparing nano-cellulose MXene gel according to claim 1, wherein the concentration of the carboxylated nano-cellulose aqueous dispersion is 0.1-50mg/g, and the concentration of the two-dimensional transition metal carbonitride aqueous dispersion is 0.1-60 mg/g.
4. The method for preparing nano cellulose MXene gel according to claim 1, wherein the freezing temperature is-198 degree to-5 degree; the freezing time is 30min-48 h.
5. The method as claimed in claim 1, wherein the transition metal in the two-dimensional transition metal carbonitride is at least one of Ti, V, Cr, Sc, Zr, Nb, Mo, Hf, Ta.
6. The method for preparing nano-cellulose MXene gel according to claim 1, wherein the two-dimensional transition metal carbonitride is selected from Ti3C2Ts、Ti2CTs、V2CTs、Cr2CTs、Sc2CTs、Zr2CTs、Mo2CTs、Mo2TiC2Ts、Hf2CTs、Ta2CTs、Ti3CNTs、Nb2CTs、TiyNb2-yCTsOr VyNb2-yCTs(ii) a Wherein, 0<y<2。
7. A nano-cellulose MXene gel, characterized in that it is prepared by a method according to any one of claims 1 to 6.
8. Use of a nanocellulose MXene gel, characterized in that, the nanocellulose MXene gel is prepared by a preparation method of any one of claims 1-6, and the nanocellulose MXene gel can be applied to the fields of supercapacitors, lithium ion batteries, electromagnetic shielding or electrocatalysis.
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CN113024732A (en) * | 2021-02-05 | 2021-06-25 | 深圳大学 | Near-infrared light response N-isopropyl acrylamide-based hydrogel and preparation method and application thereof |
CN113185193A (en) * | 2021-04-07 | 2021-07-30 | 东南大学 | MXene composite fiber reinforced graphene aerogel wave-absorbing material and preparation method thereof |
CN113549386A (en) * | 2021-08-18 | 2021-10-26 | 中国科学院宁波材料技术与工程研究所 | Water-based anticorrosive paint applied to deep sea environment and preparation method and application thereof |
CN114588846A (en) * | 2022-02-28 | 2022-06-07 | 武汉理工大学 | Nano cellulose/Ti3C2TXComposite aerogel and preparation method and application thereof |
CN114797747A (en) * | 2022-05-06 | 2022-07-29 | 中国石油大学(华东) | Super-elastic and high-adsorbability MXene aerogel and preparation method thereof |
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CN112871135A (en) * | 2021-01-29 | 2021-06-01 | 北京林业大学 | Preparation method and application of graphene oxide and MXene co-doped cellulose-based carbon aerogel |
CN113024732A (en) * | 2021-02-05 | 2021-06-25 | 深圳大学 | Near-infrared light response N-isopropyl acrylamide-based hydrogel and preparation method and application thereof |
CN113024732B (en) * | 2021-02-05 | 2022-08-16 | 深圳大学 | Near-infrared light response N-isopropyl acrylamide-based hydrogel and preparation method and application thereof |
CN113185193A (en) * | 2021-04-07 | 2021-07-30 | 东南大学 | MXene composite fiber reinforced graphene aerogel wave-absorbing material and preparation method thereof |
CN113549386A (en) * | 2021-08-18 | 2021-10-26 | 中国科学院宁波材料技术与工程研究所 | Water-based anticorrosive paint applied to deep sea environment and preparation method and application thereof |
CN114588846A (en) * | 2022-02-28 | 2022-06-07 | 武汉理工大学 | Nano cellulose/Ti3C2TXComposite aerogel and preparation method and application thereof |
CN114797747A (en) * | 2022-05-06 | 2022-07-29 | 中国石油大学(华东) | Super-elastic and high-adsorbability MXene aerogel and preparation method thereof |
CN114797747B (en) * | 2022-05-06 | 2023-09-05 | 中国石油大学(华东) | Super-elastic and high-adsorptivity MXene aerogel and preparation method thereof |
CN115216056A (en) * | 2022-08-16 | 2022-10-21 | 山东大学 | Hydrogel material with bionic pore structure and preparation method and application thereof |
CN115216056B (en) * | 2022-08-16 | 2023-10-03 | 山东大学 | Hydrogel material with bionic pore structure and preparation method and application thereof |
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