CN113198332A - MXene-nanofiber composite membrane and preparation method and application thereof - Google Patents
MXene-nanofiber composite membrane and preparation method and application thereof Download PDFInfo
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- CN113198332A CN113198332A CN202110377127.5A CN202110377127A CN113198332A CN 113198332 A CN113198332 A CN 113198332A CN 202110377127 A CN202110377127 A CN 202110377127A CN 113198332 A CN113198332 A CN 113198332A
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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
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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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
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/365—Coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
- B01D2325/028—Microfluidic pore structures
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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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
Abstract
The invention discloses an MXene-nanofiber composite membrane and a preparation method and application thereof. The MXene-nanofiber composite membrane comprises a porous base membrane and an MXene-nanofiber layer which are laminated, wherein the MXene-nanofiber layer comprises MXene nanosheets and nanofibers. The preparation method of the MXene-nanofiber composite membrane comprises the following steps: 1) preparing nano-fiber sol; 2) preparing MXene liquid crystal phase; 3) preparing MXene-nanofiber mixed sol; 4) and (3) coating the MXene-nanofiber mixed sol on a porous base membrane by a blade, and drying. The MXene-nanofiber composite membrane has ultrahigh water flux and organic solvent flux, higher selectivity, good mechanical property and stability, high reusability times, simple preparation method, low energy consumption, low cost and wide applicability.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to an MXene-nanofiber composite membrane and a preparation method and application thereof.
Background
With the rapid development of industry and cities, the water consumption of the world increases year by year, the phenomenon of water pollution also increases, and the scarcity of fresh water resources becomes a serious problem. Membrane separation technology has been a technology that can address environmental and energy challenges in the past few decades, with membrane material being the core of membrane separation technology.
The nanofiltration membrane separation technology has the advantages of low energy consumption, high safety, small occupied area, cleanness, high efficiency and the like, and is highly valued by various countries in recent decades. The selection and design of the nanofiltration membrane material should be combined with the application system and the separation principle thereof, and the qualified nanofiltration membrane material should have the following characteristics: good film forming property, excellent film separation performance, good stain resistance and antibacterial property, and good mechanical and chemical stability.
The organic nanofiltration membrane is a common nanofiltration membrane material and is widely applied, but the following problems are generally existed: 1) the chemical stability in organic solvents is poor; 2) lower flux, it is difficult to effectively improve the efficiency of the solvent treatment process; 3) it is difficult to overcome the trade-off effect (flux-selectivity is not compatible). In conclusion, the further application of the existing organic nanofiltration membrane is seriously hindered by the problems.
Therefore, there is a need to develop a separation membrane having high porosity, continuous uniform nano-scale channels, and good chemical and mechanical structural stability.
Disclosure of Invention
The invention aims to provide an MXene-nanofiber composite membrane and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the MXene-nanofiber composite membrane comprises a porous base membrane and an MXene-nanofiber layer which are laminated, wherein the MXene-nanofiber layer comprises MXene nanosheets and nanofibers.
Preferably, the porous base membrane is one of a nylon organic filter membrane, a mixed cellulose ester membrane, a polypropylene membrane and a polyether sulfone membrane.
Further preferably, the porous base membrane is a nylon organic filter membrane.
Preferably, the pore diameter of the porous base membrane is 100nm to 500 nm.
Preferably, the mass ratio of the MXene nanosheets to the nanofibers is 1: 0.01-1: 500.
More preferably, the mass ratio of the MXene nanosheets to the nanofibers is 1: 50-1: 300.
Preferably, the MXene nanosheets are Ti3C2-MXene nanosheet, Ti2C-MXene nanosheet, Ti4N3-MXene nanosheet, Ta4C3-at least one of MXene nanoplatelets.
More preferably, the MXene nanosheets are Ti3C2Tx-MXene nanoplatelets.
Preferably, the lateral dimension of the MXene nano-sheet is 1-10 μm.
Preferably, the nanofiber is at least one of aramid fiber, silk fiber, nanocellulose and cotton fiber.
Preferably, the nanofibers have a length of 1 to 500 μm and a diameter of 1 to 100 nm.
The preparation method of the MXene-nanofiber composite membrane comprises the following steps:
1) dispersing the crude fiber and alkali in an organic solvent, and stirring for reaction to obtain nanofiber sol;
2) dispersing MXene nanosheets in an organic solvent, and performing ultrasonic treatment to obtain an MXene liquid crystal phase;
3) adding the nano-fiber sol into an MXene liquid crystal phase, and stirring to obtain an MXene-nano-fiber mixed sol;
4) and (3) blade-coating the MXene-nanofiber mixed sol on a porous base membrane, and drying to obtain the MXene-nanofiber composite membrane.
Preferably, the alkali in step 1) is at least one of KOH, NaOH and LiOH.
Preferably, the amount of the alkali used in the step 1) is 100-150% of the mass of the crude fiber.
Preferably, the organic solvent in step 1) is at least one of dimethyl sulfoxide (DMSO), Dimethylformamide (DMF), and N-methylpyrrolidone (NMP).
Preferably, the stirring reaction in the step 1) is carried out at room temperature (15-25 ℃), the stirring speed is 100-5000 rpm, and the stirring time is 1-10 days.
Preferably, the power of the ultrasound in the step 2) is 5W-40W, the frequency is 50Hz, and the ultrasound time is 5 min-20 min.
Preferably, the stirring speed of the stirring in the step 3) is 100rpm to 4000rpm, and the stirring time is 1h to 8 h.
Preferably, the height of the scraper used in the step 4) is 50 μm to 600 μm.
Preferably, the drying in step 4) is one of natural drying, forced air drying, vacuum drying and drying agent drying.
Further preferably, the drying in the step 4) is vacuum drying, the drying temperature is 40-100 ℃, and the drying time is 12-72 h.
The invention has the beneficial effects that: the MXene-nanofiber composite membrane has ultrahigh water flux and organic solvent flux, higher selectivity, good mechanical property and stability, high reusability times, simple preparation method, low energy consumption, low cost and wide applicability.
Specifically, the method comprises the following steps:
1) by compounding MXene and the nano-fiber, the composite material has the advantages of high separation performance, good stability, good mechanical performance, strong pollution resistance and high reutilization frequency;
2) when the MXene-nanofiber composite membrane is used for treating ions of about 3nm, the MXene-nanofiber composite membrane has high water flux, ultrahigh selectivity and high separation efficiency, and has a good application prospect in a nanofiltration membrane;
3) the MXene-nanofiber composite membrane is prepared by a blade coating method, is simple in method and strong in applicability, can be prepared in a large scale, and is suitable for industrial production.
Drawings
Fig. 1 is an SEM image of the MXene-nanofiber composite membrane of example 1.
Fig. 2 is a digital photograph of the MXene-nanofiber composite film of example 1.
FIG. 3 is a diagram showing the results of testing the water flux and the methanol flux of MXene-nanofiber composite membranes with different MXene contents under a positive pressure of 3 bar.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
an MXene-nanofiber composite membrane is prepared by the following steps:
1) dispersing 2g of crude aramid fiber and 2g of KOH in 80mL of dimethyl sulfoxide, stirring at room temperature for 3 days at the stirring speed of 500rpm to obtain nanofiber sol (the length of the nanofiber is 1-200 mu m, and the diameter is 1-20 nm);
2) 10mL of Ti with a concentration of 2.7mg/mL3C2TxAdding 50mL of deionized water into a solution of the-MXene nanosheet (the transverse dimension of the nanosheet is 9 μm), centrifuging at 3000rpm for 80min, pouring out the supernatant, adding 60mL of dimethyl sulfoxide, centrifuging at 3000rpm for 80min, pouring out the supernatant, repeating the centrifuging operation for 3 times respectively, and adding Ti3C2TxAdding the MXene nanosheets into 2mL of dimethyl sulfoxide, and carrying out ultrasonic treatment with ultrasonic power of 40W, frequency of 50Hz and ultrasonic time of 10min to obtain MXene liquid crystal phases;
3) adding 5mL of nano-fiber sol into MXene liquid crystal phase, stirring for 3h at the stirring speed of 300rpm to obtain MXene-nano-fiber mixed sol;
4) vacuumizing the MXene-nanofiber mixed sol to remove bubbles, then scraping and coating the MXene-nanofiber mixed sol on a nylon organic filter membrane with the aperture of 100nm by using a scraper with the height of 200 mu m, and performing vacuum drying for 24 hours at the temperature of 60 ℃ to obtain the MXene-nanofiber composite membrane.
And (3) performance testing:
1) a Scanning Electron Microscope (SEM) image of the MXene-nanofiber composite film prepared in this example is shown in fig. 1 (in the figure, a is a surface, and b is a cross section), and a digital photograph is shown in fig. 2.
As can be seen from fig. 1: the thickness of the MXene-nanofiber composite membrane prepared in the embodiment is about 1 μm, the surface of the membrane presents an interwoven fiber shape, and a large number of pore channels can be used for solvent molecule transmission.
As can be seen from fig. 2: the composite membrane prepared by the embodiment has smooth and uniform surface and no obvious defect.
2) Treatment of dyes in organic solvents: the MXene-nanofiber composite membrane prepared in this example was placed in a membrane separation unit, and a 10mg/mL concentration of Evans blue (particle size 3nm) methanol solution was added to the feed side.
The test finds that: the MXene-nanofiber composite membrane prepared in the embodiment has the retention rate of 99% of Evans blue with the particle size of 3nm and the methanol flux of 550L/(m)2H.bar); the MXene-nanofiber composite membrane prepared by the embodiment can be stably stored in methanol for 1 month and can be repeatedly used for more than 10 times.
3) Referring to the preparation method of the embodiment, by adjusting the mass fraction (0-60%) of the MXene nanosheets in the MXene-nanofiber mixed sol, the MXene-nanofiber composite membranes with different MXene nanosheet contents are prepared, and then the water flux of the MXene-nanofiber composite membranes with different MXene nanosheet contents under a positive pressure of 3bar and the methanol flux of the evans blue methanol solution with a concentration of 10mg/L under a positive pressure of 3bar are tested, and the test results are shown in fig. 3 (a in the figure is water flux, and b is methanol flux).
As can be seen from fig. 3: when the mass fraction of the MXene nanosheets is 30%, the water flux and the methanol flux reach the maximum values, and the methanol flux is lower than the water flux.
Example 2:
an MXene-nanofiber composite membrane is prepared by the following steps:
1) dispersing 4g of crude aramid fiber and 6g of KOH in 120mL of dimethyl sulfoxide, stirring at room temperature for 5 days at the stirring speed of 400rpm to obtain nanofiber sol (the length of the nanofiber is 1-400 microns, and the diameter is 1-50 nm);
2) 20mL of Ti with a concentration of 2mg/mL2CTx-MXene nanosheet (nano)Transverse dimension of rice flake is 6 μm) solution is added with 40mL deionized water, then centrifuged at 5000rpm for 50min, the supernatant is poured off, 60mL dimethyl sulfoxide is added, then centrifuged at 5000rpm for 50min, the supernatant is poured off, the centrifugation operations are repeated for 3 times, and then Ti is added3C2TxAdding the MXene nanosheets into 5mL of dimethyl sulfoxide, and performing ultrasonic treatment with ultrasonic power of 40W, frequency of 50Hz and ultrasonic time of 20min to obtain MXene liquid crystal phase;
3) adding 10mL of nano-fiber sol into the MXene liquid crystal phase, stirring for 5h at the stirring speed of 500rpm to obtain MXene-nano-fiber mixed sol;
4) vacuumizing the MXene-nanofiber mixed sol to remove bubbles, then scraping and coating the MXene-nanofiber mixed sol on a nylon organic filter membrane with the aperture of 100nm by using a scraper with the height of 300 mu m, and carrying out vacuum drying at 80 ℃ for 36 hours to obtain the MXene-nanofiber composite membrane.
And (3) performance testing:
treatment of dyes in organic solvents: the MXene-nanofiber composite membrane prepared in this example was placed in a membrane separation unit, and an aqueous solution of TMPyP (particle size 2nm) having a concentration of 10mg/mL was added to the feed side.
The test finds that: the retention rate of the MXene-nanofiber composite membrane on TMPyP with the particle size of 2nm prepared in the embodiment is 92%, and the water flux is 900L/(m)2H.bar); the MXene-nanofiber composite membrane prepared by the embodiment can be stably stored in water for 2 months and can be repeatedly utilized for more than 10 times.
Example 3:
an MXene-nanofiber composite membrane is prepared by the following steps:
1) dispersing 10g of crude silk fiber and 10g of KOH in 250mL of dimethyl sulfoxide, stirring for 7 days at room temperature and the stirring speed of 500rpm to obtain nanofiber sol (the length of the nanofiber is 1-500 mu m, and the diameter is 1-100 nm);
2) 40mL of Ti at a concentration of 1mg/mL2CTxAdding 20mL of deionized water into a solution of the-MXene nanosheets (the transverse dimension of the nanosheets is 2 μm), centrifuging at 7000rpm for 40min, pouring out the supernatant, adding 60mL of dimethyl sulfoxide, centrifuging at 7000rpm for 40min, pouring out the supernatant, and repeatingRepeating the above centrifugation 3 times, and adding Ti3C2TxAdding the MXene nanosheets into 10mL of dimethyl sulfoxide, and carrying out ultrasonic treatment with ultrasonic power of 40W, frequency of 50Hz and ultrasonic time of 15min to obtain MXene liquid crystal phases;
3) adding 20mL of nano-fiber sol into MXene liquid crystal phase, stirring for 7h at the stirring speed of 200rpm to obtain MXene-nano-fiber mixed sol;
4) vacuumizing the MXene-nanofiber mixed sol to remove bubbles, then scraping and coating the MXene-nanofiber mixed sol on a nylon organic filter membrane with the aperture of 100nm by using a scraper with the height of 500 mu m, and performing vacuum drying at 60 ℃ for 72 hours to obtain the MXene-nanofiber composite membrane.
And (3) performance testing:
treatment of dyes in organic solvents: the MXene-nanofiber composite membrane prepared in this example was placed in a membrane separation device, and an aqueous solution of methylene blue (particle size 1.4nm) having a concentration of 20mg/mL was added to the feed side.
The test finds that: the retention rate of the MXene-nanofiber composite membrane on methylene blue with the particle size of 1.4nm prepared in the embodiment is 95%, and the water flux is 800L/(m)2H.bar); the MXene-nanofiber composite membrane prepared in the embodiment can stably exist in water for 1 and a half month, and can be repeatedly utilized for more than 15 times.
Comparative example 1:
commercial ultrafiltration mixed cellulose ester membranes.
Fixing the ultrafiltration mixed cellulose ester membrane in a water treatment device, treating TMPyP (particle size 2nm) aqueous solution with concentration of 10mg/L, wherein the water flux is 15L/(m)2H.bar) retention of 85% for TMPyP.
Comparative example 2:
commercial ultrafiltration polycarbonate membranes.
Fixing the ultrafiltration polycarbonate membrane in a water treatment device, treating TMPyP (particle size of 2nm) aqueous solution with concentration of 10mg/L, wherein the water flux is 20L/(m)2H.bar) retention of 60% for TMPyP.
Comparative example 3:
commercial ultrafiltration polyethersulfone membranes.
Fixing the ultrafiltration polyethersulfone membrane in a water treatment device, treating a TMPyP (particle size of 2nm) aqueous solution with the concentration of 10mg/L, wherein the water flux is 12L/(m)2H.bar) retention of 80% for TMPyP.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. An MXene-nanofiber composite membrane, characterized in that: the MXene-nanofiber composite membrane comprises a porous base membrane and an MXene-nanofiber layer which are laminated and attached; the MXene-nanofiber layer comprises MXene nanosheets and nanofibers.
2. The MXene-nanofiber composite membrane of claim 1, wherein: the porous base membrane is one of a nylon organic filter membrane, a mixed cellulose ester membrane, a polypropylene membrane and a polyether sulfone membrane.
3. The MXene-nanofiber composite membrane according to claim 1 or 2, characterized in that: the aperture of the porous base membrane is 100 nm-500 nm.
4. The MXene-nanofiber composite membrane of claim 1, wherein: the mass ratio of the MXene nanosheets to the nanofibers is 1: 0.01-1: 500.
5. The MXene-nanofiber composite membrane according to any one of claims 1, 2 and 4, characterized in that: the MXene nano-sheet is Ti3C2-MXene nanosheet, Ti2C-MXene nanosheet, Ti4N3-MXene nanosheet, Ta4C3-at least one of MXene nanoplatelets.
6. The MXene-nanofiber composite membrane according to any one of claims 1, 2 and 4, characterized in that: the lateral dimension of the MXene nano-sheet is 1-10 μm.
7. The MXene-nanofiber composite membrane of claim 1, wherein: the nano-fiber is at least one of aramid fiber, silk fiber, nano-cellulose and cotton fiber.
8. The MXene-nanofiber composite membrane according to any one of claims 1, 2, 4 and 7, wherein: the length of the nano fiber is 1-500 mu m, and the diameter is 1-100 nm.
9. The preparation method of the MXene-nanofiber composite membrane of any one of claims 1 to 8, characterized by comprising the steps of:
1) dispersing the crude fiber and alkali in an organic solvent, and stirring for reaction to obtain nanofiber sol;
2) dispersing MXene nanosheets in an organic solvent, and performing ultrasonic treatment to obtain an MXene liquid crystal phase;
3) adding the nano-fiber sol into an MXene liquid crystal phase, and stirring to obtain an MXene-nano-fiber mixed sol;
4) and (3) blade-coating the MXene-nanofiber mixed sol on a porous base membrane, and drying to obtain the MXene-nanofiber composite membrane.
10. The use of the MXene-nanofiber composite membrane of any one of claims 1 to 8 as a nanofiltration membrane.
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| CN113750827A (en) * | 2021-08-10 | 2021-12-07 | 华南理工大学 | Nanofiber-polydopamine composite membrane and preparation method and application thereof |
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