CN114507383A - Preparation method of esterified cellulose loaded MXene high-toughness film - Google Patents
Preparation method of esterified cellulose loaded MXene high-toughness film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 39
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- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims abstract description 9
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- 235000013312 flour Nutrition 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 19
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 abstract description 4
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
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- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- -1 hydrogen ions Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 239000011229 interlayer Substances 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Manufacturing & Machinery (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Manufacture Of Macromolecular Shaped Articles (AREA)
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Abstract
The invention discloses a preparation method of an esterified cellulose loaded MXene high-toughness film, which comprises the following steps: 1. proportionally mixing LiF, HCl and Ti3AlC2Mixing, stirring in a water bath, and separating and washing to obtain MXene suspension; 2. soaking poplar powder in NaOH, heating and stirring, separating to obtain treated poplar powder, mixing choline chloride and oxalic acid according to a molar ratio to obtain a mixture, mixing the treated poplar powder and the mixture according to a mass ratio, heating and stirring until viscous liquid is formed, and adding water to obtain a mixed solution; 3. adding sodium chlorite and acetic acid into the mixed solution according to a certain proportion, heating and stirring the mixed solution to be milk white, filtering and washing the mixed solution to obtain esterified cellulose, and preparing the esterified cellulose into slurry; 4.MXene suspension is filtered and dried to prepare suspension F, the suspension F is added into the slurry to obtain suspension G, the suspension G is subjected to dispersion treatment to obtain an esterified cellulose loaded MXene resin matrix, and the esterified cellulose loaded MXene resin matrix is prepared into a film.
Description
Technical Field
The invention relates to preparation of a cellulose film, in particular to a preparation method of an esterified cellulose loaded MXene high-toughness film.
Background
The technology for extracting cellulose from natural biomass raw materials has been widely researched and applied, the application potential of the cellulose film is explored and developed, and the improvement of the use performance of the cellulose film is still a task worth exploring. The processing waste poplar wood flour is one of effective renewable resources, has great development potential and can be used for manufacturing sustainable polymers. The DES cosolvent composed of choline chloride and oxalic acid can dissolve lignin and hemicellulose, so that cellulose coated by the choline chloride and the oxalic acid leaks out, and due to protonation of hydrogen ions in the DES cosolvent, hydroxyl groups of partial cellulose chain segments can be esterified, and hydrogen bond binding sites among cellulose molecules are improved. The esterified cellulose subjected to uniform dispersion treatment is intertwined and crosslinked, has more negative charges and has good stability.
The invention patent of application No. 202011106596.5 discloses a preparation method of a micronized cellulose/MXene composite film, and mainly aims to solve the problems that the mechanical property and the capacitance of the existing MXene composite film are poor, and the conductivity of the MXene cellulose composite film is in a linear reduction trend along with the increase of nano-cellulose. By making MFC @ Ti3C2After Tx microgel, MFC @ Ti is added3C2The Tx micro-gel is subjected to vacuum filtration through a mixed cellulose membrane with the aperture of 0.22 mu m, and then is dried at room temperature to obtain an independently supported microfibrillated cellulose/MXene composite membrane. The invention patent with the application number of CN201910896661.X discloses a preparation method of oxidized esterified cellulose applied to microcapsules, which comprises the steps of firstly, uniformly mixing cellulose with an oxidant and an esterifying agent, and putting the mixture into a microwave reactor for pre-reaction for 5min to activate the cellulose and oxidize the esterifying agent. Taking out and placing in a flask, reacting for a certain time at a certain temperature to obtain oxygenEsterifying cellulose; preparing microcapsules by using the obtained oxidized esterified cellulose as an object and utilizing a solvent evaporation method; and then carrying out suction filtration, washing the product with distilled water, and carrying out vacuum drying to finally obtain the cellulose ester microcapsule.
However, the film prepared by the above method does not have high wear resistance, flexibility and foldability, and excellent electrical and thermal conductivity and biodegradability, and the preparation process is complicated, and has no good economic benefit.
Disclosure of Invention
The invention aims to provide a preparation method of an esterified cellulose loaded MXene high-toughness film, which not only simplifies the preparation process, but also ensures that the prepared ENCF @ MXene film has good wear resistance, water stability and biodegradability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an esterified cellulose loaded MXene high-toughness film comprises the following steps:
step 1, mixing LiF with 36% HCl solution at a ratio (1.02.0 g) to 40mL (1.02.0 g), and slowly adding Ti3AlC2Obtaining a solution A, then placing the solution A under a water bath condition and continuously stirring, finally performing centrifugal separation, and washing with deionized water to obtain an MXene suspension B;
and 4, firstly, carrying out vacuum filtration on the MXene suspension B, drying, adding distilled water with a corresponding volume to prepare a suspension F with the concentration of 56 mg/mL, then adding the suspension F into the esterified cellulose slurry according to the volume ratio of 1: 34 to obtain a suspension G, carrying out ultrasonic dispersion treatment on the suspension G to obtain an esterified cellulose loaded MXene resin matrix, and finally preparing the esterified cellulose loaded MXene resin matrix into the ENCF @ MXene film.
Further, the temperature of the water bath in the step 1 is 45 ℃, and the stirring time is 24 hours.
Further, the pH value of MXene suspension B obtained in the step 1 is 67.
Further, the step 1 adopts a centrifuge with the rotating speed of 35004000 r/min for centrifugal separation.
Further, the concentration of the NaOH solution in the step 2 is 80100 mg/mL.
Further, in the step 2, the poplar powder is soaked in the NaOH solution at the heating temperature of 100 ℃ and the stirring time is 68 hours.
Further, the heating temperature of the mixture C of the processed poplar powder and the mixture C in the step 2 is 100120 ℃, and the stirring time is 3-5 hours.
Further, the heating temperature of the step 3 is 100 ℃, and the stirring time is 34 hours.
Further, in the step 4, the esterified cellulose loaded MXene resin matrix is prepared into the ENCF @ MXene film by adopting a suction filtration method, a casting method, a mould pressing method or a hot pressing method.
The invention has the following beneficial effects:
(1) according to the invention, the wood structure of poplar wood powder is firstly deconstructed by sodium hydroxide under the conditions of heating and stirring, lignin attached to cellulose and hemicellulose is partially dissolved and coated, then the simple heating, dissolving, filtering and cleaning treatment is carried out, unnecessary impurity removal steps are not needed, the preparation and processing technology is greatly simplified, the impurities are removed by simply adopting two-step dissolving and chlorine process bleaching, an ENCF @ MXene resin matrix can be obtained by adding MXene suspension into esterified cellulose pulp and then carrying out ultrasonic dispersion treatment, and finally the ENCF @ MXene film is prepared by adopting the existing film forming technology, so that the ENCF @ MXene film has very high economic benefit.
(2) The ENCF @ MXene film has good mechanical property due to the crosslinking and interlocking among cellulose micro/nano fibers through hydrogen bonds and van der Waals force action (the interaction between hydroxyl and carbonyl groups of esterified cellulose) and the formed reinforcing effect that the sheet layer MXene is uniformly dispersed among film laminated structures. Based on the self-reinforced compact layered structure of the ENCF @ MXene film, the slippage effect of MXene in the friction process enables the ENCF @ MXene film to have high surface strength and wear resistance. In addition, the surface of the ENCF @ MXene film has a compact cross-linked structure, water molecules are difficult to destroy the cross-linked structure formed by intertwining the micro-fibers and the nano-fibers, and the ENCF @ MXene film is not destructured even if being soaked in water for more than 3 months, so that the ENCF @ MXene film has good water stability.
(3) The raw material adopted by the invention is wood processing waste poplar powder, which is one of the most typical biomass green natural materials, and has the characteristics of wide source, large reserve and environmental protection; and the used solvent is green, environment-friendly and pollution-free, so that the ENCF @ MXene film can be degraded by microorganisms in a natural environment and converted into humus, can also be recovered, can be repeatedly used after being crushed, effectively realizes high-value utilization of waste wood, is environment-friendly and has sustainability.
Drawings
FIG. 1: a schematic diagram of a structure simulation of the ENCF @ MXene film prepared in example 1;
FIG. 2: SEM image of layered MXene prepared in example 1;
FIG. 3: the infrared spectra of the ENCF and ENCF @ MXene films prepared in example 1;
FIG. 4: plot of coefficient of friction for the ENCF @ MXene films prepared in example 2 under different conditions;
FIG. 5: a topography of dry friction wear scar of the ENCF @ MXene film prepared in example 2 under a light mirror;
FIG. 6: the heat dissipation and temperature reduction curve of the ENCF @ MXene film prepared in example 3;
FIG. 7: a graph showing flexibility and foldability of the ENCF @ MXene film prepared in example 3;
FIG. 8: stress strain profile of the ENCF @ MXene film prepared in example 3.
Detailed Description
The following examples are given to illustrate the present invention in further detail, but are not intended to limit the scope of the present invention.
Example 1
A preparation method of an esterified cellulose loaded MXene high-toughness film comprises the following steps:
step 1, uniformly mixing 1g of LiF and 40mL of HCl aqueous solution with the mass fraction of 36%, and then slowly adding 1.5g of Ti3AlC2Obtaining a solution A, then placing the solution A under the condition of water bath at 45 ℃ and continuously stirring for 24 hours, finally carrying out centrifugal separation by adopting a centrifugal machine with the rotating speed of 3500r/min, and washing by using deionized water to obtain MXene suspension B with the pH value of 6;
and 4, filtering and drying the MXene suspension B in vacuum, adding distilled water to prepare a suspension F with the concentration of 5mg/mL, adding the suspension F into the esterified cellulose slurry according to the volume ratio of 1: 3 to obtain a suspension G, performing ultrasonic dispersion treatment on the suspension G for 30min to obtain an esterified cellulose loaded MXene resin matrix, and finally preparing the esterified cellulose loaded MXene resin matrix ENCF @ MXene by adopting a suction filtration method.
Example 2
A preparation method of an esterified cellulose loaded MXene high-toughness film comprises the following steps:
step 1, uniformly mixing 1g of LiF and 40mL of HCl aqueous solution with the mass fraction of 36%, and then slowly adding 1g of Ti3AlC2Obtaining a solution A, then placing the solution A in a water bath condition of 45 ℃ and continuously stirring for 24 hours, finally adopting a centrifuge with the rotating speed of 4000r/min to carry out centrifugal separation, and washing with deionized water to obtain an MXene suspension B with the pH value of 7;
and step 4, carrying out vacuum filtration on the MXene suspension B, drying, adding distilled water to prepare a suspension F with the concentration of 6mg/mL, adding the suspension F into the esterified cellulose pulp according to the volume ratio of 1: 3.5 to obtain a suspension G, carrying out ultrasonic dispersion treatment on the suspension G for 40min to obtain an esterified cellulose loaded MXene resin matrix, and finally carrying out suction filtration on the esterified cellulose loaded MXene resin matrix ENCF @ MXene to obtain the thin film.
Example 3
A preparation method of an esterified cellulose loaded MXene high-toughness film comprises the following steps:
step 1, uniformly mixing 2g of LiF and 40mL of HCl aqueous solution with the mass fraction of 36%, and then slowly adding 2g of Ti3AlC2Obtaining a solution A, then placing the solution A in a water bath condition of 45 ℃ and continuously stirring for 24 hours, and finally adopting the rotating speed ofCentrifuging by a 4000r/min centrifugal machine, and washing by deionized water to obtain MXene suspension B with the pH value of 6;
and 4, filtering and drying the MXene suspension B in vacuum, adding distilled water to prepare a suspension F with the concentration of 6mg/mL, adding the suspension F into the esterified cellulose slurry according to the volume ratio of 1: 4 to obtain a suspension G, performing ultrasonic dispersion treatment on the suspension G for 50min to obtain an esterified cellulose loaded MXene resin matrix, and finally preparing the esterified cellulose loaded MXene resin matrix ENCF @ MXene by adopting a suction filtration method.
Example 4
A preparation method of an esterified cellulose loaded MXene high-toughness film comprises the following steps:
step 1, uniformly mixing 4g of LiF and 80mL of HCl aqueous solution with the mass fraction of 36%, and then slowly adding 4g of Ti3AlC2Obtaining a solution A, then placing the solution A in a water bath condition at 45 ℃, continuously stirring for 24 hours, and finally centrifuging and separating by adopting a centrifuge with the rotation speed of 3500r/min, and washing by using deionized water to obtain an MXene suspension B with the pH value of 7;
and 4, filtering and drying the MXene suspension B in vacuum, adding distilled water to prepare a suspension F with the concentration of 5mg/mL, adding the suspension F into the esterified cellulose slurry according to the volume ratio of 1: 3 to obtain a suspension G, performing ultrasonic dispersion treatment on the suspension G for 60min to obtain an esterified cellulose loaded MXene resin matrix, and finally preparing the esterified cellulose loaded MXene resin matrix ENCF @ MXene by adopting a suction filtration method.
FIG. 1 is a structural simulation diagram of the ENCF @ MXene film prepared in example 1, wherein the uniformly dispersed esterified cellulose is intertwined and crosslinked, and the MXene is uniformly dispersed in a crosslinked network structure of the cellulose, and the adhesion strength of the sheet layer MXene on the esterified cellulose skeleton can be increased by suction filtration and film formation.
Fig. 2 is an SEM image of MXene prepared in example 1, and it is evident that MXene etched by this method has a layered structure similar to an accordion, and under the urging of energy, the carriers can move rapidly in the interlayer structure, which is helpful for the transfer of heat energy and imparts thermal conductivity to the insulating cellulose film.
FIG. 3 is an infrared spectrum of the ENCF and ENCF @ MXene films prepared in example 1, showing similar diffraction peaks in the infrared spectrum of the ENCF @ MXene compared to the esterified cellulose ENCF film, and a decrease in the diffraction intensity indicating that the MXene is dispersed and loaded into the cellulose backbone, thereby limiting the depth of detection of the infrared light.
FIG. 4 is a graph of the friction coefficient of the ENCF @ MXene film prepared in example 2 under different loads, wherein the friction coefficient under dry friction condition is very close to that under PAO lubricating oil dripping condition, which shows that MXene plays a key role in enhancing the mechanical property and surface property.
FIG. 5 is a graph of the wear scar topography under a light mirror for the ENCF @ MXene film prepared from example 2, which has a relatively flat surface, strong mechanical strength, and low wear rate.
FIG. 6 is a graph of the heat dissipation and temperature reduction of the ENCF @ MXene film prepared in example 3, compared with the esterified cellulose ENCF film, the ENCF @ MXene film has metal conductivity of transition metal carbide and excellent thermal conductivity due to the fact that MXene in the ENCF @ MXene film is loaded on a cellulose skeleton and hydroxyl groups or terminal oxygen are arranged on the surface of MXene material.
FIG. 7 is a graph showing the flexibility and foldability of the ENCF @ MXene film prepared in example 3, and it can be seen that the ENCF @ MXene film has excellent flexibility and does not break or break even when folded in half.
FIG. 8 is a stress-strain plot of the ENCF @ MXene film prepared in example 3 of the present invention having a higher tensile stress at break than the esterified cellulose ENCF film.
Claims (9)
1. A preparation method of an esterified cellulose loaded MXene high-toughness film is characterized by comprising the following steps:
step 1, mixing LiF with 36% by mass of HCl in water at a ratio (1.02.0 g) to 40mL (1.02.0 g), and slowly adding Ti3AlC2Obtaining a solution A, then placing the solution A under a water bath condition and continuously stirring, finally performing centrifugal separation, and washing with deionized water to obtain an MXene suspension B;
step 2, soaking the poplar wood flour in NaOH solution, heating and stirring, performing centrifugal separation to obtain treated poplar wood flour, mixing choline chloride and oxalic acid according to a mass ratio of 7: 613 to obtain a mixture C, mixing the treated poplar wood flour with the mixture C according to a mass ratio of 1: 1520, heating and stirring until viscous liquid D is formed, and finally performing centrifugal separation according to a volume ratio of 1: (10-15) adding deionized water into the viscous liquid D to obtain a mixed solution E;
step 3, adding sodium chlorite and acetic acid into the mixed solution E according to the ratio of (23 g) to 1mL to 100mL, heating and stirring until the solution becomes milky white, filtering and washing to obtain esterified cellulose, and then adding the esterified cellulose into distilled water to prepare esterified cellulose slurry with the concentration of 2025 mg/mL;
and step 4, carrying out vacuum filtration on the MXene suspension B, drying, adding distilled water with a corresponding volume to prepare a suspension F with the concentration of 56 mg/mL, adding the suspension F into the esterified cellulose pulp according to a volume ratio of 1: 34 to obtain a suspension G, carrying out ultrasonic dispersion treatment on the suspension G to obtain an esterified cellulose loaded MXene resin matrix, and finally preparing the esterified cellulose loaded MXene resin matrix into the ENCF @ MXene film.
2. The method for preparing the esterified cellulose loaded MXene high-toughness film according to claim 1, wherein the water bath temperature in step 1 is 45 ℃ and the stirring time is 24 hours.
3. The method for preparing the MXene high-toughness film loaded with the esterified cellulose according to claim 1, wherein the pH value of the MXene suspension B obtained in the step 1 is 67.
4. The method for preparing the esterified cellulose loaded MXene high-toughness film according to claim 1, wherein the step 1 is performed by centrifugation with a centrifuge rotating at 35004000 r/min.
5. The method for preparing the esterified cellulose loaded MXene high-toughness film according to claim 1, wherein the concentration of the NaOH solution in the step 2 is 80100 mg/mL.
6. The method for preparing the esterified cellulose loaded MXene high-toughness film according to claim 1, wherein the heating temperature for soaking poplar wood flour in NaOH solution in the step 2 is 100 ℃, and the stirring time is 68 hours.
7. The method for preparing the esterified cellulose loaded MXene high-toughness film according to claim 1, wherein the heating temperature of the mixture of the processed poplar wood flour and the mixture C in the step 2 is 100120 ℃, and the stirring time is 3-5 hours.
8. The method for preparing the esterified cellulose loaded MXene high toughness film according to claim 1, wherein the heating temperature in step 3 is 100 ℃ and the stirring time is 34 hours.
9. The method for preparing the esterified cellulose loaded MXene high toughness film according to claim 1, wherein step 4 is to form the esterified cellulose loaded MXene resin matrix into the ENCF @ MXene film by suction filtration, casting, molding or hot pressing.
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| CN202210285882.5A CN114507383B (en) | 2022-03-23 | 2022-03-23 | Preparation method of esterified cellulose loaded MXene high-toughness film |
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| CN114958466A (en) * | 2022-06-21 | 2022-08-30 | 陕西科技大学 | lignocellulose-MXene/polytetrafluoroethylene wax limited self-lubricating material and preparation method thereof |
| CN115041027A (en) * | 2022-06-13 | 2022-09-13 | 成都理工大学 | Dual-regulation two-dimensional MXene composite membrane and preparation method thereof |
| CN116515146A (en) * | 2023-05-06 | 2023-08-01 | 陕西科技大学 | Multifunctional film material with cellulose/graphene-Mxene hybrid interweaving structure and preparation method thereof |
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| CN114958466A (en) * | 2022-06-21 | 2022-08-30 | 陕西科技大学 | lignocellulose-MXene/polytetrafluoroethylene wax limited self-lubricating material and preparation method thereof |
| CN114958466B (en) * | 2022-06-21 | 2023-02-17 | 陕西科技大学 | lignocellulose-MXene/polytetrafluoroethylene wax limited self-lubricating material and preparation method thereof |
| CN116515146A (en) * | 2023-05-06 | 2023-08-01 | 陕西科技大学 | Multifunctional film material with cellulose/graphene-Mxene hybrid interweaving structure and preparation method thereof |
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