CN113457464A - MXene film preparation method based on co-intercalation accurate interlayer spacing regulation - Google Patents
MXene film preparation method based on co-intercalation accurate interlayer spacing regulation Download PDFInfo
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- B01D67/0039—Inorganic membrane manufacture
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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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- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The invention discloses an MXene membrane preparation method based on co-intercalation accurate control of interlayer spacing, which takes single-layer or few-layer MXene nanosheet solution as a raw material, sodium hydroxide as an intercalating agent, succinic acid as a cross-linking agent and a Nylon membrane (Nylon 6) as a base membrane; the method comprises the steps of firstly, ultrasonically dispersing an MXene nanosheet solution with a certain volume and concentration uniformly, then, carrying out vacuum filtration on the MXene nanosheet solution to a Polydopamine (PDA) -coated Nylon6 base material (PDA/Nylon 6) to obtain an MXene film, then, soaking the MXene film in a mixed solution of 0.1-1.0 mol/L sodium hydroxide and 0.1-1.0 mol/L succinic acid for 0.5-1 h, and finally, heating the MXene film in a vacuum oven at 70-80 ℃ for 1-2 h to obtain the MXene film based on co-intercalation accurate interlayer spacing regulation. The preparation method is simple, the interlayer spacing of the obtained MXene membrane is about 6A, the MXene membrane has the characteristics of enlarged nano channel and swelling resistance, has higher rejection rate and stability, can be used in the fields of seawater desalination, hard water softening, sewage purification, gas separation and the like, and has good application potential.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to an MXene membrane preparation method based on co-intercalation accurate interlayer spacing regulation.
Background
. The separation is a big household of energy consumption and pollution in all chemical processes. Compared with the traditional energy-intensive separation method, the method comprises the following steps: rectification, evaporation, low-temperature pressure swing adsorption separation and the like, and the membrane separation has the advantages of high efficiency, energy conservation, low carbon, no phase change in the separation process, continuous operation, no chemical change and low operation temperature, and is one of the most potential means for replacing the traditional separation means. A membrane is a material that selectively functions as a separator, allowing certain substances to pass through, while blocking other substances. A film is a functionalized material of a particular structure, as defined by the film definition. The membranes are classified into organic membranes, inorganic membranes, and hybrid membranes according to materials. The research and development of membrane materials are always the most important direction in the research direction of membranes, and new materials can assist the research of membrane separation every time. The maturity of new material synthesis methods and processes also provides more solutions to the toggle problem arising from membrane development.
The appearance of sheet material films was initiated with the study of graphene in the field of membrane separation. Such material membranes are mainly sheet structures formed by stacking two-dimensional materials in a certain manner, and the two-dimensional channels formed between sheets can provide rapid transmission channels and precise size screening. At present, the membrane is prepared by pumping and filtering a solution with a certain concentration on an organic or inorganic substrate mainly by adopting a vacuum-assisted pumping and filtering mode, and a similar membrane structure can be obtained by methods such as spin coating, solution pouring and the like. Compared with the traditional organic film, the film is theoretically formed by stacking the sheets with the atomic-level thickness, so that the thickness can be controlled, the size of a two-dimensional channel formed between the layers is more uniform, and the stricter size screening characteristic can be displayed.
MXene is a new two-dimensional transition metal carbon/nitride discovered in recent years. Due to the fact that the two-dimensional film formed by stacking MXene nanosheet units is provided with a regular controllable transmission channel, rich surface functional groups and hydrophilic properties, transmission of water and an organic solvent can be achieved, and meanwhile molecules of different sizes can be effectively screened. Therefore, in the field of membrane separation, the MXene membrane shows excellent performances in aspects of gas separation, ion screening, dye interception and the like. However, as the interlayer spacing of MXene is nano-scale, the water molecule permeation channel is small, and the flux of the constructed membrane is low. In addition, the anti-swelling problem of the MXene film in the water treatment field is also faced. Researches show that by intercalation or surface modification of MXene, the permeation flux of the membrane can be remarkably improved, the higher retention rate can be maintained, and the MXene membrane has the multifunctional characteristics of swelling resistance, pollution resistance, bacteria resistance and the like.
Currently, studies on accurate control of the interlayer spacing of an MXene film based on co-intercalation are few.
Chinese patent application No. CN201811534886.2 entitled "two-dimensional self-crosslinking MXene membrane and preparation method thereof" discloses a method for self-crosslinking MXene membrane by regulating temperature, and the interlayer spacing of the prepared two-dimensional self-crosslinking MXene membrane in solution can be kept below the size of small-size hydrated ions, and has stable and effective interlayer channels. The method is simple and easy to operate, and is resistant to swelling, but the prepared membrane does not have expanded flux.
Chinese patent application No. CN202110073161.3 entitled MXene membrane preparation method based on ethylenediamine crosslinking regulation of interlamellar spacing discloses a method for regulating the interlamellar spacing of MXene by using ethylenediamine crosslinking. The method can effectively enlarge the interlayer spacing of the nanosheets and improve the swelling resistance of the film, but cannot accurately regulate the interlayer spacing of the MXene film.
Therefore, the development of an MXene film which has high retention rate, can accurately control the interlamellar spacing and is resistant to swelling is necessary.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the MXene membrane preparation method based on co-intercalation precise interlayer spacing regulation, which has the advantages of simple method, high water flux, good rejection rate and swelling resistance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
taking a single-layer or few-layer MXene nanosheet solution as a raw material, sodium hydroxide as an intercalating agent, succinic acid as a crosslinking agent, and a Nylon membrane (Nylon 6) as a base membrane; the method comprises the steps of firstly, ultrasonically dispersing an MXene nanosheet solution with a certain concentration uniformly, then, carrying out vacuum filtration on the MXene nanosheet solution to a PDA/Nylon6 substrate to obtain an MXene film, then, soaking the MXene film in a mixed solution of sodium hydroxide with the concentration of 0.1-1.0 mol/L and succinic acid with the concentration of 0.1-1.0 mol/L for 0.5-1 h, and finally, heating the MXene film in a vacuum oven at the temperature of 70-80 ℃ for 1-2 h to obtain the MXene film based on co-intercalation accurate interlayer spacing regulation.
The method specifically comprises the following steps:
1) carrying out ice bath on MXene nanosheet solution with the volume of 100-200 ml and the concentration of 0.01-0.02 mg/ml in an argon atmosphere, and carrying out ultrasonic treatment at 160-250W for 10-30 min.
2) Soaking the Nylon6 substrate into 1-2 g/L dopamine aqueous solution, and then processing in an oscillator at room temperature for 12-24 h to obtain the PDA/Nylon6 substrate.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene film obtained in the step 3) in a mixed solution of sodium hydroxide with the concentration of 0.1-1.0 mol/L and succinic acid with the concentration of 0.1-1.0 mol/L for 0.5-1 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.085 to-0.1 Mpa and the temperature of 70 to 80 ℃ for 1 to 2 hours to obtain the MXene film based on the co-intercalation layer accurate regulation and control of interlayer spacing.
Wherein: the volume of the MXene nanosheet solution in the step 1) is 100-200 ml, and the concentration is 0.01-0.02 mg/ml. When the volume of the MXene nanosheet solution is less than 100ml and the concentration is less than 0.01mg/ml, the amount of MXene nanosheets is small, namely the loading amount of the MXene nanosheets on the membrane is small, so that the thickness of the membrane is small, and the mechanical performance and the rejection rate of the membrane are reduced.
When the volume of the MXene nanosheet solution is more than 200ml and the concentration is more than 0.02mg/ml, the amount of MXene nanosheets is large, namely the capacity of the MXene nanosheets on the membrane is large, so that the pumping filtration is slow, more time and energy are consumed, the thickness of the membrane is large, the transmission path of water molecules among the membranes is lengthened, and the water flux is reduced.
Carrying out 160-250W ultrasonic treatment for 10-30 min in the step 1). When the ultrasonic power is less than 160W, the oscillation is not violent enough to uniformly mix the MXene nanosheet solution, and further the membrane stacking of the suction filtration is not uniform. When the ultrasonic power is more than 250W, the oscillation is too violent, so that MXene nanosheets are shattered, the lamella is not complete enough, and the retention rate is reduced. When the ultrasonic time is less than 10min, the ultrasonic time is too short, and the MXene nanosheet solution cannot be completely and uniformly distributed, so that the membrane subjected to suction filtration has large defects. When the ultrasonic time is longer than 30min, the MXene nanosheet layer is damaged due to the overlong ultrasonic time, the retention rate is reduced, and the overlong ultrasonic time is uneconomical.
The dopamine aqueous solution with the concentration of 1-2 g/L in the step 2). When the concentration is less than 1g/L, the dopamine amount is less, and a hydrophilic polydopamine layer (PDA) is not easy to deposit on the surface of the nylon support body, so that the interaction force between the support body and the functional layer is reduced, and the functional layer cannot be ensured to have good adhesion on the support body. When the concentration is more than 2g/L, the dopamine amount is excessive, so that a plurality of hydrophilic polydopamine layers are deposited on the surface of the nylon support, channels are blocked, and the water flux is reduced.
Treating in the oscillator at room temperature for 12-24 h in the step 2). When the oscillation time is less than 12 hours, the oscillation time is too short, a hydrophilic poly dopamine layer (PDA) cannot be completely deposited on the surface of the nylon support body, so that the interaction force between the support body and the functional layer is insufficient, the adhesion force is insufficient, and the film defect is easily generated. When the oscillation time is longer than 24 hours, the oscillation time is too long, and the energy consumption is large, which is not economical.
Soaking the mixture in the step 4) in a mixed solution of sodium hydroxide with the concentration of 0.1-1.0 mol/L and succinic acid with the concentration of 0.1-1.0 mol/L for 0.5-1 h. When the concentration of sodium hydroxide and succinic acid is less than 0.1mol/L, sodium ions are not enough to completely open the interlayer channel, and the succinic acid crosslinking reaction is not complete, so that the stability of the interlayer channel is not favorably controlled. When the concentration of sodium hydroxide and succinic acid is more than 1.0mol/L, excessive ions and crosslinking agents can be enriched in the membrane, so that the interlayer channel is blocked, and the water flux is reduced. When the soaking time is less than 0.5h, sodium ions cannot be completely inserted into the nanosheet layer of the membrane, and succinic acid cannot be completely reacted with hydroxyl on the nanosheet layer. When the soaking time is more than 1h, the excessive ions and the crosslinking agent can block the channels between the membranes, and the water flux is reduced.
And (5) heating for 1-2 h in a vacuum oven with the vacuum degree of-0.085 to-0.1 Mpa and the temperature of 70-80 ℃. When the vacuum degree is higher than-0.085 Mpa, the air level in the oven is completely exhausted, so that MXene film is oxidized, and the film performance is reduced. When the vacuum degree is lower than-0.1 MPa, the energy consumption is high and the method is not economical. When the temperature is lower than 70 ℃, the temperature of the crosslinking reaction is lower, so that the crosslinking is incomplete, the film spacing cannot be well regulated and controlled, and the swelling resistance cannot be greatly improved. When the temperature is higher than 80 ℃, the temperature of the crosslinking reaction is higher, so that the nanosheet structure is changed, self-crosslinking is carried out, the interlayer spacing is reduced, and the water flux is reduced. When the crosslinking time is less than 1h, the crosslinking time is short, and the succinic acid and the nanosheet layer are not stable enough and are easy to fall off. When the crosslinking time is more than 2 hours, the crosslinking time is long, increasing energy consumption, and being uneconomical.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method disclosed by the invention is simple to operate, easy to operate and control, low in energy consumption, low in production cost and high in economic feasibility.
2. The MXene film prepared by the method has the accurately controllable interlamellar spacing and swelling resistance.
3. The MXene membrane prepared by the method has the characteristics of high hydrophilicity, stable structure and the like, and has higher water flux and interception rate.
Detailed Description
The present invention will be described in further detail with reference to specific examples, wherein the raw materials used are common commercial products unless otherwise specified.
Example 1:
preparing an MXene film based on co-intercalation accurate control interlayer spacing by adopting the following steps of:
1) MXene nanosheet solution with volume of 100ml and concentration of 0.02mg/ml is subjected to ice bath under argon atmosphere and ultrasonic treatment at 160W for 20 min.
2) Soaking the Nylon6 base material into dopamine aqueous solution with the concentration of 1g/L, and then processing the base material in a vibrator for 24 hours at room temperature to obtain the PDA/Nylon6 base material.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene membrane obtained in the step 3) in a mixed solution of sodium hydroxide and succinic acid with the concentration of 0.1mol/L and 0.2mol/L for 1 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.1 Mpa and the temperature of 80 ℃ for 1h to obtain the MXene film based on the accurate interlayer spacing regulation of the co-intercalation.
Example 2:
preparing an MXene film based on co-intercalation accurate control interlayer spacing by adopting the following steps of:
1) 200ml of MXene nanosheet solution with the concentration of 0.01mg/ml is subjected to ice bath under the argon atmosphere, and ultrasonic treatment is carried out for 10min at 200W.
2) Soaking the Nylon6 substrate into dopamine aqueous solution with the concentration of 1.2g/L, and then processing the substrate in a vibrator for 20 hours at room temperature to obtain the PDA/Nylon6 substrate.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene membrane obtained in the step 3) in a mixed solution of sodium hydroxide and succinic acid, wherein the concentrations of the sodium hydroxide and the succinic acid are respectively 0.5mol/L and 0.7mol/L for 0.9 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.09 Mpa and the temperature of 75 ℃ for 1.5h to obtain the MXene film based on the co-intercalation accurate interlayer spacing regulation.
Example 3:
preparing an MXene film based on co-intercalation accurate control interlayer spacing by adopting the following steps of:
1) MXene nanosheet solution with volume of 150ml and concentration of 0.01mg/ml is subjected to ice bath under argon atmosphere, and ultrasonic treatment is carried out at 200W for 15 min.
2) Soaking the Nylon6 substrate into dopamine aqueous solution with the concentration of 1.5g/L, and then processing the substrate in a vibrator for 15 hours at room temperature to obtain the PDA/Nylon6 substrate.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene membrane obtained in the step 3) in a mixed solution of sodium hydroxide and succinic acid with the concentration of 0.8mol/L and 1mol/L respectively for 0.8 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.085 Mpa and the temperature of 70 ℃ for 2h to obtain the MXene film based on the co-intercalation accurate interlayer spacing regulation.
Example 4:
preparing an MXene film based on co-intercalation accurate control interlayer spacing by adopting the following steps of:
1) MXene nanosheet solution with volume of 150ml and concentration of 0.02mg/ml is subjected to ice bath under argon atmosphere and ultrasonic treatment at 180W for 30 min.
2) Soaking the Nylon6 base material into dopamine aqueous solution with the concentration of 2g/L, and then processing the base material in a vibrator for 12 hours at room temperature to obtain the PDA/Nylon6 base material.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene membrane obtained in the step 3) in a mixed solution of sodium hydroxide and succinic acid with the concentration of 1mol/L and 0.5mol/L for 0.5 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.09 Mpa and the temperature of 80 ℃ for 1.5h to obtain the MXene film based on the co-intercalation accurate interlayer spacing regulation.
Example 5:
preparing an MXene film based on co-intercalation accurate control interlayer spacing by adopting the following steps of:
1) MXene nanosheet solution with volume of 100ml and concentration of 0.015mg/ml is subjected to ice bath under argon atmosphere and ultrasonic treatment at 250W for 10 min.
2) Soaking the Nylon6 substrate into dopamine aqueous solution with the concentration of 1.8g/L, and then processing the substrate in a vibrator for 20 hours at room temperature to obtain the PDA/Nylon6 substrate.
3) And (3) carrying out vacuum filtration on the MXene nanosheet solution subjected to ultrasonic treatment in the step 1) to the PDA/Nylon6 base material obtained in the step 2) to obtain the MXene film.
4) Soaking the MXene membrane obtained in the step 3) in a mixed solution of sodium hydroxide and succinic acid with the concentration of 0.9mol/L and 0.6mol/L for 1 h.
5) Heating the MXene film soaked in the step 3) in a vacuum oven with the vacuum degree of-0.1 Mpa and the temperature of 75 ℃ for 2h to obtain the MXene film based on the accurate interlayer spacing regulation of the co-intercalation.
The MXene membranes prepared in examples 1-5 and based on co-intercalation precise control of interlamellar spacing were tested for lithium ion rejection rate and water flux by applying 1bar pressure with 3.5mol/L LiCl solution as raw material solution under a dead-end filtration device self-made in a laboratory. The data are detailed in table 1.
TABLE 1 Performance testing of MXene films based on co-intercalation precise control of interlayer spacing
| Product(s) | Retention (%) | Water flux (LMH) |
| Example 1 | 92.4 | 5.3 |
| Example 2 | 92.7 | 5.5 |
| Example 3 | 91.2 | 6.2 |
| Example 4 | 94.3 | 5.1 |
| Example 5 | 93.8 | 5.8 |
As can be seen from the above table 1, the MXene membrane of the invention based on co-intercalation precise control of interlamellar spacing has higher water flux and rejection rate. The preparation method effectively improves the performance of the MXene film.
Finally, it should be noted that the above-mentioned examples of the present invention are only examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (5)
1. The method for preparing the MXene membrane based on the co-intercalation precise control of the interlayer spacing is characterized by comprising the steps of ultrasonically dispersing MXene nanosheet solution with a certain volume and concentration uniformly, carrying out vacuum suction filtration on the MXene nanosheet solution to obtain the MXene membrane on a PDA/Nylon6 base material, soaking the MXene membrane in a mixed solution of sodium hydroxide with the concentration of 0.1-1.0 mol/L and succinic acid with the concentration of 0.1-1.0 mol/L for 0.5-1 h, and finally heating the MXene membrane in a vacuum oven at 70-80 ℃ for 1-2 h to obtain the MXene membrane based on the co-intercalation precise control of the interlayer spacing.
2. The method for preparing the MXene membrane based on co-intercalation precise control of interlayer distance according to claim 1, wherein the volume of MXene nanosheet solution is 100-200 ml, and the concentration is 0.01-0.02 mg/ml.
3. The method for preparing the MXene film based on the co-intercalation precise control of the interlayer distance according to claim 1, wherein the ultrasonic dispersion condition is ice bath under argon atmosphere and ultrasonic sound at 160-250W for 10-30 min.
4. The method for preparing the MXene membrane based on co-intercalation precise control of interlayer distance according to claim 1, wherein the PDA coated PES substrate is obtained by immersing Nylon6 substrate in 1-2 g/L dopamine aqueous solution, and then treating in a shaker at room temperature for 12-24 h.
5. The method for preparing the MXene film based on the co-intercalation precise control of interlayer distance according to claim 1, wherein the vacuum degree of the vacuum oven is-0.085 to-0.1 MPa.
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| CN114038689A (en) * | 2021-11-16 | 2022-02-11 | 盐城工学院 | Ti3Preparation method of CNTx film |
| CN114452837A (en) * | 2022-03-02 | 2022-05-10 | 重庆工商大学 | MXene two-dimensional thin film defect repairing method |
| CN114713050A (en) * | 2022-04-29 | 2022-07-08 | 重庆工商大学 | Preparation method of photosensitive MXene composite film |
| CN114713050B (en) * | 2022-04-29 | 2023-01-17 | 重庆工商大学 | Preparation method of photosensitive MXene composite film |
| CN115121134A (en) * | 2022-07-04 | 2022-09-30 | 重庆工商大学 | Preparation method of novel MXene-based composite membrane |
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