CN112844065B - MXene composite film preparation method and MXene composite film - Google Patents
MXene composite film preparation method and MXene composite film Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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- B01D71/025—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- 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
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- 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
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 adding MXene powder and HNTs powder into a beaker respectively, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a first solution and a second solution respectively; 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 obtain the MXene composite membrane. 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 in 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 realize 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:
adding MXene powder and HNTs powder into a beaker respectively, and performing ultrasonic dispersion at the temperature of 20-30 ℃ to obtain a first solution and a second solution respectively;
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;
carrying out vacuum filtration on the target solution to an organic polymer film to obtain an MXene composite film;
the dosage of the MXene powder is 2mg, the dosage of the HNTs powder is 2-5mg, and the dosage of the PDA is 20-200mg.
Further, the dosage of MXene powder is 2mg, the dosage of HNTs powder is 2mg, and the dosage of PDA is 80mg.
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 a rejection rate of the MXene composite membrane, and the rejection rate is calculated by the following steps:
wherein R is the rejection, C p Concentration of oil-water mixture in the separated liquid after permeating the MXene composite membrane, C f The 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 0.22um.
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 Ti3AlC2.
Further, the centrifugal washing rotating speed of the deionized water 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 obtain the MXene composite membrane. 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 or technical solutions of the present invention, the drawings used in the embodiments or technical solutions of 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, which is shown in fig. 1 and 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 obtain the MXene composite membrane.
It should be noted 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 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 between 10 nm and 30nm and between 50 nm and 200nm, and the length of the tube is different from dozens of to hundreds of nanometers. HNTs have higher length-diameter ratio and 10.7-39% of 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 Ti3AlC2. 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 by using deionized water at the rotating speed of 3000-4000rpm, preferably 3500rpm, 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 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 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 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 organic polymer membrane materials such as polyvinylidene fluoride (PVDF) membrane, polyether sulfone (PES) and Polysulfone (PSF) are 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 so as 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 between 10-30 nm and 50-200 nm, and the lengths are different from dozens 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 PDA (poly dopamine) is added later to prevent the MXene from being oxidized, and the PDA has the adhesion property to firmly adhere the HNTs and the MXene together, so that a 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 effect of PDA on HNTs adhesion to MXene, swelling properties of unmodified MXene pure film and MXnen composite film are shown in fig. 2 and 3, and it can be seen that the films all fall off after immersion of 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 of pH =3 and pH =7 for 7 days, but also after being soaked in deionized water of 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 retention rate, C p Concentration of oil-water mixture in the separated liquid after permeating the MXene composite membrane, C f The 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 be described in detail below with reference to examples M1-M7, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present 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 films of examples M1 to 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, the optimum formulation ratio is M6 (i.e. the separation layer is composed of 2mg MXene +2mg HNTs +80mg PDA), and the flux of pure MXene membrane is only 401.7 + -50 L.m driven by 0.1MPa pressure -2 ·h -1 The pure water flux of the modified composite membrane can reach 5036.2 +/-484.7 L.m -2 ·h -1 (namely the preset threshold range), in addition, the retention rate of the modified film to the oil-water emulsion reaches 99 +/-0.1% (namely 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 of the invention has excellent performance of treating water pollution, the MXene composite membrane can be verified by testing the interlayer spacing of the MXene composite membrane in the invention.
In the invention, the interlayer spacing algorithm is calculated by X-ray diffraction (XRD) and theory:
As can be seen from the calculation of the interlayer spacings corresponding to the above embodiments, the interlayer spacing of M6 is 17.7A, which meets the optimum interlayer spacing range
Therefore, the MXene composite membrane prepared by the formula proportion 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 (11)
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 the 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;
carrying out vacuum filtration on the target solution to an organic polymer film to obtain an MXene composite film;
the dosage of the MXene powder is 2mg, the dosage of the HNTs powder is 2-5mg, and the dosage of the PDA is 20-200mg.
2. The method for preparing the MXene composite membrane according to claim 1, wherein the MXene powder is 2mg, the HNTs powder is 2mg, and the PDA is 80mg.
3. 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.
4. The method for preparing the MXene composite membrane of claim 3, wherein the predetermined index value is a water flux of the MXene composite membrane calculated by:
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 represents the effective area (m) of the MXene composite membrane 2 ) And t is the penetration time (h).
5. The method for preparing the MXene composite membrane according to claim 3, 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, C p Concentration of oil-water mixture in the separated liquid after the MXene composite membrane is permeated, C f Is the concentration of the oil-water mixture in the liquid to be separated before the MXene composite membrane permeates.
6. The method for preparing the MXene composite film of claim 1, wherein the organic polymer film is a CA film.
7. The method for preparing the MXene composite membrane according to claim 6, wherein the CA membrane has a pore size of 0.22um.
8. 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 into a LiF + HCl mixed reagent for an 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.
9. The method for preparing the MXene composite membrane of claim 8, wherein the MAX phase is Ti 3 AlC 2 。
10. The method for preparing the MXene composite membrane according to claim 9, wherein the deionized water centrifugal washing rotation speed is 3000-4000rpm, and the precipitate is centrifuged at 3000-4000rpm for 1-2h.
11. An MXene composite film produced by the method for producing an MXene composite film according to any one of claims 1 to 10.
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