CN112844065A - MXene composite film preparation method and MXene composite film - Google Patents
MXene composite film preparation method and MXene composite film Download PDFInfo
- Publication number
- CN112844065A CN112844065A CN202110056912.0A CN202110056912A CN112844065A CN 112844065 A CN112844065 A CN 112844065A CN 202110056912 A CN202110056912 A CN 202110056912A CN 112844065 A CN112844065 A CN 112844065A
- Authority
- CN
- China
- Prior art keywords
- mxene
- composite membrane
- solution
- mxene composite
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Analytical Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to the technical field of membrane materials, and particularly discloses an MXene composite membrane preparation method and an MXene composite membrane, wherein the method comprises the steps of respectively adding MXene powder and HNTs powder into a beaker, and carrying out ultrasonic dispersion at the temperature of 20-30 ℃ to respectively obtain a first solution and a second solution; mixing the first solution and the second solution, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a mixed solution; adding a PDA + tris-HCl mixed reagent with a pH value of 8-9 into the mixed solution for ultrasonic dispersion, and after the ultrasonic dispersion is finished, performing magnetic stirring on the mixed solution uniformly to obtain a target solution; and carrying out vacuum filtration on the target solution to an organic polymer film to obtain the MXene composite film. The MXene and the HNTs are blended and modified according to a certain proportion to increase the interlayer spacing of the MXene composite membrane, namely the pore diameter of the limber of the MXene composite membrane is enlarged, so that the water permeability of the composite membrane is stronger, and a good water delivery channel is provided.
Description
Technical Field
The invention relates to the technical field of membrane materials, in particular to a preparation method of an MXene composite membrane and the MXene composite membrane.
Background
Industrial wastewater refers to wastewater and waste liquid generated in industrial production process, and its pollutants are various and complex in composition (such as oil stain, dye, heavy metal and microorganism, etc.), and if they are not effectively treated before being discharged, they will pose a great threat to the surrounding ecological environment and human health. The membrane separation technology has the characteristics of high separation efficiency, environmental friendliness and the like, is widely applied to the fields of industrial wastewater treatment and the like at present, and has the reputation of 'water treatment technology in the 21 st century'. The membrane material is the key of the membrane separation technology and is a core component for the industrialization of the membrane technology. The traditional membrane material has poor pollution resistance, and the relationship between permeation flux and rejection rate is mutually restricted.
However, the existing membrane material has the problem of small interlayer spacing, and the stacking structure of the membrane material prolongs the liquid permeation pore canal, thereby finally severely limiting the permeation flux of the membrane material to oil-water droplets with large particle size.
Therefore, how to provide a membrane material capable of improving the oil-water separation capability becomes a technical problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of an MXene composite membrane, which aims to solve the problems that the liquid permeation pore canal is lengthened due to the small interlayer spacing and the stacking structure of the existing membrane material, and the permeation flux of the membrane material to oil-water droplets with large particle sizes is finally severely limited.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, a method for preparing an MXene composite membrane is provided, which comprises the following steps:
respectively adding MXene powder and HNTs powder into a beaker, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to respectively obtain a first solution and a second solution;
mixing the first solution and the second solution, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a mixed solution;
adding a PDA + tris-HCl mixed reagent with a pH value of 8-9 into the mixed solution for ultrasonic dispersion, and after the ultrasonic dispersion is finished, performing magnetic stirring on the mixed solution uniformly to obtain a target solution;
and carrying out vacuum filtration on the target solution to an organic polymer film to obtain the MXene composite film.
Further, the dosage of MXene powder is 1-3mg, the dosage of HNTs powder is 0-6mg, and the dosage of PDA is 0-300 mg.
Further, the dosage of MXene powder is 2mg, the dosage of HNTs powder is 2mg, and the dosage of PDA is 200 mg.
Further, the method further comprises:
preparing multiple MXene composite films by respectively taking MXene powder, HNTs powder and PDA with different formula proportions, respectively calculating preset index values of each MXene composite film, and selecting the formula proportion corresponding to the MXene composite films with the preset index values falling within a preset threshold range as an optimal proportion.
Further, the preset index value is the water flux of the MXene composite membrane, and the calculation process of the water flux is as follows:
wherein J represents the pure water flux (L.m) of the membrane-2·h-1) (ii) a V represents the volume (L) of pure water permeating the membrane, A is the effective area (square meter) of the MXene composite membrane, and t is the permeation time (h).
Further, the preset index value is the rejection rate of the MXene composite membrane, and the calculation process of the rejection rate is as follows:
wherein R is the rejection, CpConcentration of oil-water mixture in the separated liquid after permeating the MXene composite membrane, CfThe concentration of the oil-water mixture in the liquid to be separated after the MXene composite membrane permeates.
Further, the organic polymer film is a CA film.
Further, the pore size of the CA membrane is 0.22 um.
Further, the MXene powder preparation step comprises:
dispersing MAX phase powder in a LiF + HCl mixed reagent for etching reaction to obtain a first mixed solution, and stirring the first mixed solution uniformly at the temperature of 20-30 ℃ to obtain a second mixed solution;
centrifugally washing the second mixed solution by using deionized water until the ph value of the supernatant of the second mixed solution is 5-7, and obtaining a precipitate of the second mixed solution;
shaking the precipitate for 5-15 minutes, and carrying out centrifugal treatment to obtain MXene homogeneous phase solution;
and (3) drying the upper suspension of the MXene homogeneous phase solution in a vacuum drying box at 40 ℃ to obtain MXene powder.
Further, the MAX phase is Ti3AlC 2.
Further, the rotational speed of the deionized water centrifugal washing is 3000-4000rpm, and the precipitate is centrifuged for 1-2h at 3000-4000 rpm.
The invention also provides an MXene composite membrane prepared by the MXene composite membrane preparation method.
The invention has the beneficial effects that:
the method for preparing the MXene composite membrane and the MXene composite membrane comprises the steps of respectively adding MXene powder and HNTs powder into a beaker, and carrying out ultrasonic dispersion at the temperature of 20-30 ℃ to respectively obtain a first solution and a second solution; mixing the first solution and the second solution, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a mixed solution; adding a PDA + tris-HCl mixed reagent with a pH value of 8-9 into the mixed solution for ultrasonic dispersion, and after the ultrasonic dispersion is finished, performing magnetic stirring on the mixed solution uniformly to obtain a target solution; and carrying out vacuum filtration on the target solution to an organic polymer film to obtain the MXene composite film. The MXene and the HNTs are blended and modified according to a certain proportion to increase the interlayer spacing of the MXene composite membrane, namely the pore diameter of the limber of the MXene composite membrane is enlarged, so that the water permeability of the composite membrane is stronger, and a good water delivery channel is provided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing an MXene composite membrane according to an embodiment of the present invention;
FIG. 2 is a diagram illustrating the adhesion effect of MXene composite membrane on HNTs and MXene of PDA tested in this invention;
FIG. 3 is a diagram showing another result of MXene composite membrane testing the adhesion effect of PDA on HNTs and MXene in the example of the present invention.
Detailed Description
The numerical values set forth in the examples of the present invention are approximations, not necessarily values. All values within the error range may be included without limiting to the specific values disclosed in the embodiments of the present invention, where the error or experimental conditions allow.
The numerical ranges disclosed in the examples of the present invention are intended to indicate the relative amounts of the components in the mixture and the ranges of temperatures or other parameters recited in the other method examples.
In one aspect, the present invention provides a method for preparing an MXene composite film, as shown in fig. 1, the method includes the following steps:
s1: respectively adding MXene powder and HNTs powder into a beaker, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to respectively obtain a first solution and a second solution;
s2: mixing the first solution and the second solution, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a mixed solution;
s3: adding a PDA + tris-HCl mixed reagent with a pH value of 8-9 into the mixed solution for ultrasonic dispersion, and after the ultrasonic dispersion is finished, performing magnetic stirring on the mixed solution uniformly to obtain a target solution;
s4: and carrying out vacuum filtration on the target solution to an organic polymer film to obtain the MXene composite film.
It should be explained that MXene is a new type of two-dimensional transition metal carbide or carbonitride, typically prepared by selective removal of a atomic layer in the MAX phase by chemical etching or the like. MXene has a chemical formula represented by Mn +1XnTx (wherein M is an early transition metal element, X represents carbon or nitrogen, and T is a surface-attached active group-OH, -F, etc.). Compared with graphene-based materials, MXene not only has the characteristics of high specific surface area, high conductivity and the like, but also has adjustable and controllable interlayer spacing and components. The functional groups such as-OH, -O and the like rich on the surface endow MXene with more excellent reactivity and hydrophilicity, so that MXene can be well dispersed in an aqueous solution.
HNTs (halloysite) is a natural silicate clay mineral with its interior and exterior composed of alumina octahedra and silica tetrahedra, respectively, and the spatial mismatch between the interior and exterior walls causes the natural curling of the bilayers into hollow tubular nanostructures. The HNTs has a structure similar to that of the carbon nano tube, and both the HNTs have a hollow tubular structure with openings at two ends, the inner diameter and the outer diameter of the tube are respectively 10-30 nm and 50-200 nm, the length of the tube is different from dozens of nanometers to hundreds of nanometers, but the HNTs has wide sources, is low in price and easy to obtain, and is beneficial to practical application. HNTs have higher length-diameter ratio and 10.7-39% hollow tube wall space, and can provide a high-efficiency diffusion channel for water molecules. In addition, a large number of positively charged Al-OH groups exist on the inner surfaces of HNTs, so that the HNTs have good hydrophilicity; the Si-O-Si structure and the tubular structure with low chemical activity on the outer surface ensure that HNTs have weaker interaction and are easy to uniformly and stably disperse in a polymer matrix.
Wherein the preparation method of MXene powder comprises the following steps:
dispersing MAX phase powder in a LiF + HCl mixed reagent for etching reaction to obtain a first mixed solution, and stirring the first mixed solution uniformly at the temperature of 20-30 ℃ to obtain a second mixed solution. Among them, the MAX phase is preferably Ti3AlC 2. Compared with the common etching method in the prior art, in which HF solvent etching is adopted, the defects that the MXene material is not compact in stacking structure and is easy to fall off can be overcome.
Centrifuging and washing the second mixed solution at the rotation speed of 3000-4000rpm, preferably 3500rpm, by using deionized water until the ph value of the supernatant of the second mixed solution is 5-7, preferably 6, and obtaining a precipitate of the second mixed solution at the moment;
the precipitate is shaken for 5-15 minutes, preferably 10 minutes, and centrifuged at 3000-4000rpm for 1-2 hours to obtain MXene homogeneous solution, preferably at 3500rpm for 1 hour.
And (3) drying the upper suspension of the MXene homogeneous phase solution in a vacuum drying box at 40 ℃ to obtain MXene powder.
In a specific embodiment, MXene powder and HNTs (halloysite) powder are respectively added into a 250ml beaker, ultrasonic dispersion is carried out at the temperature of 25 ℃ for 30 minutes to respectively obtain a first solution and a second solution, the first solution and the second solution are mixed and subjected to ultrasonic dispersion at the temperature of 25 ℃ for 30 minutes to obtain a mixed solution, a PDA + tris-HCl mixed reagent with a pH value of 8.5 is added into the mixed solution to carry out ultrasonic dispersion for 30 minutes, after the ultrasonic dispersion is finished, the mixed solution is magnetically stirred for 24 hours to obtain a target solution, the target solution is subjected to vacuum filtration to obtain a CA membrane (cellulose acetate membrane) with a pore diameter of 0.22 micron, or an organic polymer membrane material such as polyvinylidene fluoride (PVDF) membrane, polyether sulfone (PES) and Polysulfone (PSF) is used as a supporting layer to obtain the MXene composite membrane.
The MXene composite membrane prepared based on the preparation method takes CA as a substrate, and MXene and HNTs are blended and modified according to a certain proportion to increase the interlayer spacing of the MXene composite membrane, namely the pore diameter of a limber hole of the MXene composite membrane is enlarged, so that the water permeability of the composite membrane is stronger, and a good water delivery channel is provided. And the inner diameter and the outer diameter of the HNTs are respectively 10-30 nm and 50-200 nm, and the length is different from dozens of nanometers to hundreds of nanometers, so that the MXene composite membrane can be prepared by selecting HNTs with different apertures according to actual conditions.
In addition, a large number of oxygen-containing functional groups on the HNTs can improve the hydrophilic performance of the composite membrane. The subsequent addition of PDA (polydopamine) can prevent MXene from being oxidized, and the PDA has the adhesion property of firmly adhering HNTs and MXene together, so that the water conveying channel is not easy to damage. In addition, as with HNTs, the large number of oxygen-containing functional groups of PDA can provide significant hydrophilicity to the composite membrane, thereby enhancing the anti-fouling properties of the composite membrane.
To verify the adhesion effect of PDA to HNTs and MXene, swelling properties of the unmodified MXene pure film and the MXnen composite film are shown in fig. 2 and 3, and it can be seen that the films all fall off after immersing the unmodified MXene pure film in deionized water at pH 12 for 7 days. In contrast, the MXnen composite membrane does not fall off not only after being soaked in deionized water at pH 3 and pH 7 for 7 days, but also after being soaked in deionized water at pH 12 for 7 days. The adhesion of PDA proved to greatly improve the mechanical stability of the composite membrane.
And then, screening the formula proportion with the best oil-water separation effect of the MXene composite membrane as the optimal proportion to prepare the MXene composite membrane by observing the preset index values of the MXene composite membrane prepared by different formula proportions. The specific operation process is as follows:
preparing multiple MXene composite films from MXene powder, HNTs powder and PDA with different formula proportions, respectively calculating preset index values of each MXene composite film, and selecting the formula proportion corresponding to the MXene composite film with the preset index value within a preset threshold range as an optimal proportion.
Presetting an index value as the water flux of the MXene composite membrane, wherein the calculation process of the water flux is as follows:
wherein J represents the pure water flux (L.m) of the membrane-2·h-1) (ii) a V represents the volume (L) of pure water permeating the membrane, A is the effective area (square meter) of the MXene composite membrane, and t is the permeation time (h).
In another embodiment, the preset index value may also be a rejection rate of the MXene composite membrane, and the rejection rate is calculated by:
wherein R is the rejection, CpConcentration of oil-water mixture in the separated liquid after permeating the MXene composite membrane, CfThe concentration of the oil-water mixture in the liquid to be separated after the MXene composite membrane permeates.
The performances of the MXene composite membrane can be reflected by testing the water flux and the retention rate corresponding to multiple portions of MXene composite membrane prepared from MXene powder, HNTs powder and PDA with different formula proportions, and the optimal formula proportion for preparing the MXene composite membrane can be determined.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Embodiments of the present invention will now be described in detail with reference to examples M1-M7, but it will be understood by those skilled in the art that the following examples are illustrative of the present invention only and should not be taken as limiting the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
MXene composite membranes of examples M1-M7 were prepared according to the contents of the components in Table 1 below in parts by weight.
TABLE 1
From the above experimental results, it can be seen that the optimum formulation ratio is M6 (i.e. the separation layer is composed of 2mg MXene +2mg HNTs +200mg PDA), and the flux of pure MXene membrane is only 401.7 + -50 L.m.under the pressure of 0.1MPa-2·h-1The pure water flux of the modified composite membrane can reach 5036.2 +/-484.7 L.m-2·h-1(i.e. the preset threshold range), in addition, the retention rate of the modified film to the oil-water emulsion reaches 99 +/-0.1% (i.e. the preset threshold range). Therefore, the scheme of the invention improves the water flux and the rejection rate of the membrane, and constructs a novel high-performance two-dimensional MXene oil-water separation membrane which has stable structure, high permeability and high selectivity and excellent comprehensive performances such as pollution resistance and the like. Provides a certain guidance for developing novel membrane materials, can be widely applied to solving the problem of industrial water pollution, accords with the concept of green development, and has important theoretical value and practical significance in implementation.
In order to further verify that the MXene composite membrane prepared by the preparation method has excellent water pollution treatment performance, the MXene composite membrane can be verified by testing the interlayer spacing of the MXene composite membrane.
In the present invention, the interlayer spacing algorithm is calculated by X-ray diffraction (XRD) and theory:
where d is the interlayer spacing, n is 1, λ is 0.154nm, and θ is obtained by the characteristic peak angle in origin.
As can be seen from the calculation of the interlayer spacings corresponding to the above-mentioned embodiments, the interlayer spacing of M6 is 17.7A, which is in accordance with the optimum interlayer spacing rangeTherefore, the MXene composite membrane prepared by the formula ratio corresponding to M6 has the best effect in wastewater treatment.
The invention also provides an MXene composite membrane prepared by the MXene composite membrane preparation method.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (12)
1. A preparation method of an MXene composite membrane is characterized by comprising the following steps:
respectively adding MXene powder and HNTs powder into a beaker, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to respectively obtain a first solution and a second solution;
mixing the first solution and the second solution, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a mixed solution;
adding a PDA + tris-HCl mixed reagent with a pH value of 8-9 into the mixed solution for ultrasonic dispersion, and after the ultrasonic dispersion is finished, performing magnetic stirring on the mixed solution uniformly to obtain a target solution;
and carrying out vacuum filtration on the target solution to an organic polymer film to obtain the MXene composite film.
2. The method for preparing the MXene composite membrane according to claim 1, wherein the MXene powder is used in an amount of 1-3mg, the HNTs powder is used in an amount of 0-6mg, and the PDA is used in an amount of 0-300 mg.
3. The method for preparing the MXene composite membrane according to claim 2, wherein the MXene powder is 2mg, the HNTs powder is 2mg, and the PDA is 200 mg.
4. The method of preparing the MXene composite film of claim 1, further comprising:
preparing multiple MXene composite films by respectively taking MXene powder, HNTs powder and PDA with different formula proportions, respectively calculating preset index values of each MXene composite film, and selecting the formula proportion corresponding to the MXene composite films with the preset index values falling within a preset threshold range as an optimal proportion.
5. The method for preparing the MXene composite membrane according to claim 4, wherein the preset index value is a water flux of the MXene composite membrane, and the water flux is calculated by the following steps:
wherein J represents the pure water flux (L.m) of the membrane-2·h-1) (ii) a V represents the volume (L) of pure water permeating the membrane, A is the effective area (square meter) of the MXene composite membrane, and t is the permeation time (h).
6. The method for preparing the MXene composite membrane according to claim 4, wherein the preset index value is a rejection rate of the MXene composite membrane, and the rejection rate is calculated by the following steps:
wherein R is the rejection, CpConcentration of oil-water mixture in the separated liquid after permeating the MXene composite membrane, CfThe concentration of the oil-water mixture in the liquid to be separated after the MXene composite membrane permeates.
7. The method for preparing the MXene composite film of claim 1, wherein the organic polymer film is a CA film.
8. The method for preparing the MXene composite membrane according to claim 7, wherein the CA membrane has a pore size of 0.22 um.
9. The method for preparing the MXene composite membrane according to claim 1, wherein the MXene powder is prepared by the steps of:
dispersing MAX phase powder in a LiF + HCl mixed reagent for etching reaction to obtain a first mixed solution, and stirring the first mixed solution uniformly at the temperature of 20-30 ℃ to obtain a second mixed solution;
centrifugally washing the second mixed solution by using deionized water until the ph value of the supernatant of the second mixed solution is 5-7, and obtaining a precipitate of the second mixed solution;
shaking the precipitate for 5-15 minutes, and carrying out centrifugal treatment to obtain MXene homogeneous phase solution;
and (3) drying the upper suspension of the MXene homogeneous phase solution in a vacuum drying box at 40 ℃ to obtain MXene powder.
10. The method of making MXene of claim 9, wherein the MAX phase is Ti3AlC 2.
11. The method for preparing MXene of claim 10, wherein the deionized water centrifugal washing rotation speed is 3000-4000rpm, and the precipitate is centrifuged at 3000-4000rpm for 1-2 h.
12. An MXene composite membrane prepared by the MXene composite membrane preparation method of any one of claims 1-11.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110056912.0A CN112844065B (en) | 2021-01-15 | 2021-01-15 | MXene composite film preparation method and MXene composite film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110056912.0A CN112844065B (en) | 2021-01-15 | 2021-01-15 | MXene composite film preparation method and MXene composite film |
Publications (2)
Publication Number | Publication Date |
---|---|
CN112844065A true CN112844065A (en) | 2021-05-28 |
CN112844065B CN112844065B (en) | 2023-03-14 |
Family
ID=76007005
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110056912.0A Active CN112844065B (en) | 2021-01-15 | 2021-01-15 | MXene composite film preparation method and MXene composite film |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112844065B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113416572A (en) * | 2021-06-17 | 2021-09-21 | 宁夏神瑞工贸有限责任公司 | Separation process and method for energy-saving environment-friendly stable light hydrocarbon processing |
CN114558458A (en) * | 2021-12-27 | 2022-05-31 | 长安大学 | Preparation method of HNTs/oleylamine composite membrane |
Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005089642A (en) * | 2003-09-18 | 2005-04-07 | Nippon Zeon Co Ltd | Film, oriented film, laminate and method for producing film |
CN107138048A (en) * | 2017-05-23 | 2017-09-08 | 安徽大学 | A kind of preparation method of the oily seperation film of High-performance graphite oxide alkene/halloysite nanotubes Compound Water |
CN107715700A (en) * | 2017-11-24 | 2018-02-23 | 中国科学院烟台海岸带研究所 | A kind of high-salt wastewater processing corrosion resistant anti-soil film and its preparation method and application |
CN108499588A (en) * | 2018-03-02 | 2018-09-07 | 东华大学 | A kind of g-C3N4The preparation method of/MXene composite materials |
CN108993165A (en) * | 2018-08-21 | 2018-12-14 | 郑州大学 | A kind of layered inorganic material organic solvent nanofiltration composite membrane and preparation method thereof |
CN109482071A (en) * | 2018-11-16 | 2019-03-19 | 江苏大学 | A kind of preparation method and its usage of PVDF/GO@PDA@HNTs composite membrane |
CN109553103A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A kind of two dimension self-crosslinking MXene film and preparation method thereof |
CN109569317A (en) * | 2018-12-12 | 2019-04-05 | 浙江工业大学 | A kind of preparation method of MXene nanofiltration membrane |
CN110124529A (en) * | 2019-05-28 | 2019-08-16 | 北京理工大学 | A kind of preparation method and application of graphene oxide/MXene composite membrane |
WO2020058481A1 (en) * | 2018-09-21 | 2020-03-26 | Danmarks Tekniske Universitet | A protein-based water insoluble and bendable polymer with ionic conductivity |
CN110975655A (en) * | 2019-11-22 | 2020-04-10 | 成都理工大学 | Novel RGO/MXene composite membrane and preparation method thereof |
US20200254396A1 (en) * | 2020-04-03 | 2020-08-13 | Qatar University | Precise Fabrication of Activated-Hydrophilic-Hydrophobic MXenes-based Multidimensional Nanosystems for Efficient and Prompt Water Purification from Petroleum Wastes and Desalination Process under Ambient Conditions |
CN111905574A (en) * | 2020-07-14 | 2020-11-10 | 广东工业大学 | MXene attapulgite composite film and preparation method thereof |
-
2021
- 2021-01-15 CN CN202110056912.0A patent/CN112844065B/en active Active
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005089642A (en) * | 2003-09-18 | 2005-04-07 | Nippon Zeon Co Ltd | Film, oriented film, laminate and method for producing film |
CN107138048A (en) * | 2017-05-23 | 2017-09-08 | 安徽大学 | A kind of preparation method of the oily seperation film of High-performance graphite oxide alkene/halloysite nanotubes Compound Water |
CN107715700A (en) * | 2017-11-24 | 2018-02-23 | 中国科学院烟台海岸带研究所 | A kind of high-salt wastewater processing corrosion resistant anti-soil film and its preparation method and application |
CN108499588A (en) * | 2018-03-02 | 2018-09-07 | 东华大学 | A kind of g-C3N4The preparation method of/MXene composite materials |
CN108993165A (en) * | 2018-08-21 | 2018-12-14 | 郑州大学 | A kind of layered inorganic material organic solvent nanofiltration composite membrane and preparation method thereof |
WO2020058481A1 (en) * | 2018-09-21 | 2020-03-26 | Danmarks Tekniske Universitet | A protein-based water insoluble and bendable polymer with ionic conductivity |
CN109482071A (en) * | 2018-11-16 | 2019-03-19 | 江苏大学 | A kind of preparation method and its usage of PVDF/GO@PDA@HNTs composite membrane |
CN109569317A (en) * | 2018-12-12 | 2019-04-05 | 浙江工业大学 | A kind of preparation method of MXene nanofiltration membrane |
CN109553103A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A kind of two dimension self-crosslinking MXene film and preparation method thereof |
CN110124529A (en) * | 2019-05-28 | 2019-08-16 | 北京理工大学 | A kind of preparation method and application of graphene oxide/MXene composite membrane |
CN110975655A (en) * | 2019-11-22 | 2020-04-10 | 成都理工大学 | Novel RGO/MXene composite membrane and preparation method thereof |
US20200254396A1 (en) * | 2020-04-03 | 2020-08-13 | Qatar University | Precise Fabrication of Activated-Hydrophilic-Hydrophobic MXenes-based Multidimensional Nanosystems for Efficient and Prompt Water Purification from Petroleum Wastes and Desalination Process under Ambient Conditions |
CN111905574A (en) * | 2020-07-14 | 2020-11-10 | 广东工业大学 | MXene attapulgite composite film and preparation method thereof |
Non-Patent Citations (7)
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113416572A (en) * | 2021-06-17 | 2021-09-21 | 宁夏神瑞工贸有限责任公司 | Separation process and method for energy-saving environment-friendly stable light hydrocarbon processing |
CN114558458A (en) * | 2021-12-27 | 2022-05-31 | 长安大学 | Preparation method of HNTs/oleylamine composite membrane |
Also Published As
Publication number | Publication date |
---|---|
CN112844065B (en) | 2023-03-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110975655B (en) | Novel RGO/MXene composite membrane and preparation method thereof | |
Junaidi et al. | Recent development of graphene oxide-based membranes for oil–water separation: A review | |
Khosla et al. | Emergence of MXene and MXene–polymer hybrid membranes as future‐environmental remediation strategies | |
CN112844065B (en) | MXene composite film preparation method and MXene composite film | |
CN101700473B (en) | Self-assembly method of inorganic nano particle hybridization organic membrane | |
Yang et al. | Recent advances in graphene oxide membranes for nanofiltration | |
Yang et al. | Novel hydrophilic PVDF ultrafiltration membranes based on a ZrO 2–multiwalled carbon nanotube hybrid for oil/water separation | |
Shao et al. | Enhancing interfacial adhesion of MXene nanofiltration membranes via pillaring carbon nanotubes for pressure and solvent stable molecular sieving | |
CN102068925B (en) | Preparation method of polyaniline nano composite film | |
CN102824856B (en) | Preparation method for generating inorganic nanoparticle hybrid membrane in situ by using self-assembly technology | |
CN110038450B (en) | Preparation method of super-hydrophilic carbon nanotube nano porous membrane | |
CN102674337A (en) | Self-extension graphene and preparation method thereof | |
CN112354378B (en) | Layered MoS2Nano graphene oxide membrane reduced by blending nanosheets and preparation method thereof | |
CN103657456A (en) | Preparation method of ethanol-permselective POSS (polyhedral oligomeric silsesquioxanes)/silicone rubber composite membrane | |
Ma et al. | 2D lamellar membrane with MXene hetero-intercalated small sized graphene oxide for harsh environmental wastewater treatment | |
CN108993165B (en) | Layered inorganic material organic solvent nanofiltration composite membrane and preparation method thereof | |
CN110280147A (en) | A kind of swelling resistance two-dimensional layer film, preparation and application that inter-layer passages size is controllable | |
CN112090300A (en) | Preparation method, product and application of hydrophilized zirconium-based MOF (Metal organic framework) doped PVDF (polyvinylidene fluoride) membrane | |
CN107051208B (en) | Doping Kynoar mixed-matrix ultrafiltration membrane and its preparation is blended in three-dimensional structure nano-complex | |
CN112588115B (en) | Fusiform MXene-carbon nanotube two-dimensional film and preparation method and application thereof | |
CN107081068A (en) | Infiltrating and vaporizing membrane and preparation method thereof | |
Zhang et al. | Preparation of sepiolite modified MXene composite membrane for oil/water separation | |
Chen et al. | Formation of Titania/Silica Hybrid Nanowires Containing Linear Mesocage Arrays by Evaporation‐Induced Block‐Copolymer Self‐Assembly and Atomic Layer Deposition | |
CN107675362A (en) | A kind of Kynoar/polysulfonamides composite nano fiber net and preparation method thereof | |
CN110449039B (en) | Graphene/graphene oxide-based separation membrane and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |