CN113797761A - Method for regulating and controlling performance of graphene oxide-based composite membrane - Google Patents
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- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 7
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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
- B01D67/0079—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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
一种氧化石墨烯基复合膜性能的调控方法，包括：将聚合物材料纺制成丝，随后经冷压处理得到纳米纤维基膜；通过真空抽滤、涂敷方式将氧化石墨烯纳米片或氧化石墨烯纳米片/聚电解质的混合溶液沉积于静电纺丝纳米纤维基膜上抽滤成膜，随后在室温下放置，阴干，即得到氧化石墨烯基复合膜。本发明的方法以高通量静电纺丝纳米纤维为基膜，以氧化石墨烯纳米片为阻隔层，采用柔性长链聚电解质对其片层间距进行精细调控，以构筑高渗透性复合滤膜，解决了传统氧化石墨烯基复合滤膜存在的渗透性极低、稳定性差等问题。此种制备方法简单易行有效、对环境友好，能够实现对氧化石墨烯片层纳米材料阻隔层的有效调控，适用于规模化的低成本的生产复合纳滤膜。
A method for regulating the performance of a graphene oxide-based composite membrane, comprising: spinning a polymer material into silk, followed by cold pressing to obtain a nanofiber base membrane; The mixed solution of graphene oxide nanosheets/polyelectrolyte is deposited on the electrospinning nanofiber base membrane by suction filtration to form a membrane, and then placed at room temperature and dried in the shade to obtain a graphene oxide-based composite membrane. The method of the invention uses high-flux electrospinning nanofibers as base membranes, uses graphene oxide nanosheets as barrier layers, and uses flexible long-chain polyelectrolytes to finely control the interlayer spacing of the sheets, so as to construct a high-permeability composite filter membrane It solves the problems of extremely low permeability and poor stability of traditional graphene oxide-based composite membranes. The preparation method is simple, easy, effective, and environmentally friendly, can realize effective regulation of the graphene oxide sheet nanomaterial barrier layer, and is suitable for large-scale and low-cost production of composite nanofiltration membranes.
Description
Technical Field
The invention relates to preparation of a separation composite membrane, in particular to a method for regulating and controlling the performance of a graphene oxide-based composite membrane.
Background
In recent years, graphene oxide attracts much attention due to its advantages of high specific surface area, special two-dimensional nanostructure, and rich hydrophilic oxygen-containing groups (hydroxyl, carboxyl, etc.), and they are a class of soft materials with polymer, thin film, colloid, and amphiphilic properties, and are easy to form into films, convenient for mass production, and have a broad application prospect in the technical field of membrane separation. Graphene oxide is often used as a polymer membrane additive to construct water permeation channels and increase the hydrophilicity of the surface of the composite membrane. However, as a planar two-dimensional material, the sheets of the planar two-dimensional material are closely packed to form a dense graphene oxide film after being directly filtered and filtered into a film, so that the permeability is very poor. In addition, the interaction between the sheets is weak, resulting in poor stability in water.
Disclosure of Invention
The invention aims to provide a method for effectively regulating and controlling the interlayer spacing of graphene oxide nano materials, which aims to solve the problems of poor permeability, poor stability and low water treatment efficiency of the traditional graphene oxide composite membrane in the prior art.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for regulating and controlling the performance of a graphene oxide-based composite membrane comprises the following steps:
(1) preparing a nanofiber-based membrane: dissolving a proper amount of polymer in a solvent to prepare a uniform solution with the concentration of 1-50 wt%, preparing nano fibers by using an electrostatic spinning technology, and performing cold pressing treatment to obtain a nano fiber base film;
(2) preparing a graphene oxide functional barrier layer: ultrasonically dispersing a proper amount of graphene oxide nano sheets in a solvent to prepare a solution A with the concentration of 0.001-20 mg/mL; dissolving a proper amount of long-chain polyelectrolyte in a solvent to prepare a solution B with the mass fraction of 0.01-20 wt%; ultrasonically and uniformly mixing the prepared solution A and the prepared solution B according to a certain ratio (1:0-1:500) to form a mixed solution C; depositing the solution C on the surface of the nanofiber base membrane in the step (1) in a vacuum filtration or coating mode, and drying in the shade to obtain the graphene oxide-based composite filter membrane; and soaking the prepared composite filter membrane in deionized water for later use.
Further, the polymer material in step (1) includes, but is not limited to, one or more of polysulfone, polyethersulfone, polyvinyl alcohol, polyacrylonitrile, polyvinyl alcohol, polystyrene, polyvinylidene fluoride, and the like.
Further, the polyelectrolyte in the step (2) includes, but is not limited to, one or more of polyethyleneimine, chitosan, poly (allylamine hydrochloride), polyamide, polyvinylamine, polyvinylpyridine, polydimethyldiallylammonium chloride, polyvinylpyrrolidone, polycarboxymethyl cellulose, gelatin, polystyrene sulfonate, sodium alginate, polyacrylamide, polymethacrylic acid (salt), polyvinyl sulfonic acid (salt), polyvinyl phosphoric acid (salt), carboxymethyl cellulose (salt), polyphosphate, polysilicic acid, and the like.
Further, the solvent in steps (1) and (2) includes, but is not limited to, one or more of deionized water, aqueous acetic acid, N-dimethylformamide, hexane, N-dimethylacetamide, toluene, acetone, diethyl ether, and the like.
The invention also provides the graphene oxide-based composite filter membrane prepared by the method.
Compared with the prior art, the invention has the beneficial technical effects that:
according to the method, the long-chain flexible polymer electrolyte is used as a regulator to modify the graphene oxide nanosheet functional barrier layer, so that the method has good application potential in the aspect of efficient water treatment;
the method provided by the invention has the advantages that the polyelectrolyte is used for regulating and controlling the lamella spacing of the graphene oxide nanosheets, the stability of the functional layer of the nanosheets is improved, the permeability of the functional layer of the nanosheets is improved, the method is simple and effective, energy-saving and environment-friendly, and the fine regulation and control of the surface aperture of the functional barrier layer on the surface of the composite membrane can be realized;
the invention adopts the high-permeability porous nanofiber membrane as the base membrane and has an ultrathin nanosheet barrier layer, wherein the flexible polymer can effectively regulate and control the lamella spacing, and more water permeation channels are provided, so that the prepared composite membrane has high permeability as a whole.
Drawings
FIG. 1 is an SEM photograph of the surface morphology of the GO-PEI/PAN nanofiber-based composite membrane of example 1;
FIG. 2 is the GO: influence of mass ratio of PEI on separation effect of GO-PEI/PAN composite membrane.
FIG. 3 is the separation effect of GO-CTS/PAN composite membranes on different dyes in example 2.
Detailed Description
The present invention will be further illustrated with reference to the following examples.
Example 1
A preparation method of a high-flux graphene oxide-Polyethyleneimine (PEI)/polyacrylonitrile nanofiber-based composite filter membrane comprises the following steps:
1. dissolving polyacrylonitrile in an N, N-dimethylformamide solvent to prepare a 10 wt% solution, preparing nanofibers in an electrostatic spinning mode, and obtaining a PAN nanofiber base membrane after cold pressing;
2. dissolving PEI in deionized water to prepare a uniform solution with the mass fraction of 1%;
3. dispersing graphene oxide in water to prepare a solution of 0.05 mg/L;
4. preparing a mixed solution according to the mass ratio of GO to PEI, taking a proper amount of the mixed solution, depositing the mixed solution on the PAN nano-fiber in a vacuum filtration mode, and drying in the shade to form the GO-PEI/PAN nano-fiber composite filter membrane (figure 1).
As shown in figure 2, when the GO/PEI mass ratio is 1:0, 1:15 and 1:25 in sequence, the permeation flux of the composite filter membrane under 0.3MPa is 411.1, 173.8 and 89.2L/m respectively2h, the retention rates are 70.9%, 99.6% and 99.8% respectively. It can be found that when the mass ratio of GO to PEI is 1:15, the prepared GO-PEI/PAN nanofiber-based composite filter membrane has the best filtration performance, and the graphene oxide interlayer spacing is increased after PEI modification
The penetration flux is reduced by less than 30 percent after 24h test, and the antifouling paint has good antifouling performance.
Example 2
A preparation method of a high-flux Graphene Oxide (GO) -Chitosan (CTS)/Polyacrylonitrile (PAN) nanofiber-based composite filter membrane comprises the following steps:
1. dissolving polyacrylonitrile in an N, N-dimethylformamide solvent to prepare a 12 wt% solution, preparing nanofibers in an electrostatic spinning mode, and obtaining a PAN nanofiber base membrane after cold pressing;
2. dissolving chitosan in acetic acid water solution to prepare coating solution with the mass fraction of 1.0%;
3. dispersing graphene oxide in water to prepare a solution of 0.02 mg/L;
4. preparing a mixed solution according to the mass ratio of GO to CTS, taking a proper amount of the mixed solution, depositing the mixed solution on the PAN nano-fiber in a vacuum filtration mode, and drying in the shade to form the GO-CTS/PAN nano-fiber composite filter membrane.
As shown in fig. 3, the graphene oxide-chitosan/polyacrylonitrile nanofiber-based composite filter membrane was used for the filtration test of direct red 80 dye: the mass ratio of GO to CTS is 1:75, 1:100 and 0 when the mass ratio of GO to CTS is 1:125 in sequence.The permeation flux of the composite filter membrane under 3MPa is 112.9, 246.9 and 369.8L/m respectively2h, the retention rates are 99.0%, 98.2% and 99.3% respectively. It can be found that when the mass ratio of GO to CTS is 1:125, the prepared GO-CTS/PAN nanofiber-based composite filter membrane has the best filtration performance, and the graphene oxide interlayer spacing is increased after chitosan modification
And the permeation flux is still maintained at a higher level (141.2L/m) after 24h test2h) And the antifouling paint shows good antifouling performance.
For pure GO membrane, when the retention rate is more than 99%, the permeation flux is only 28.5L/m under 0.3MPa2h, the result shows that the method is really effective in regulating and controlling the graphene oxide functional barrier layer.
Example 3
A preparation method of a high-flux GO-polyacrylic acid (PAA)/polyether sulfone (PES) nanofiber-based composite filter membrane comprises the following steps:
1. dissolving polyether sulfone in an N, N-dimethylacetamide solvent to prepare a 26 wt% solution, preparing nanofibers through an electrostatic spinning mode, and obtaining a PES nanofiber base membrane after cold pressing;
2. dissolving PAA in deionized water to prepare a uniform solution with the mass fraction of 0.2%;
3. dispersing GO in water to prepare a 0.1mg/L solution;
4. preparing a mixed solution according to the GO/PAA mass ratio, taking a proper amount of the mixed solution, depositing the mixed solution on PES nano fibers in a vacuum filtration mode, and drying in the shade to form the GO-PAA/PES nano fiber composite filter membrane.
When the mass ratio of GO to PAA is 1:0.25, 1:0.5 and 1:0.75 in sequence, the permeation flux of the composite filter membrane under 0.1MPa is respectively 256.2, 271.3 and 275.9L/m2h, the retention rates are 86.5%, 98.9% and 96.3% respectively. It can be found that when the mass ratio of GO to PAA is 1:0.5, the prepared GO-PAA/PES nanofiber-based composite filter membrane has the best filtration performance, and the interlayer spacing of graphene oxide modified by PAA is increased after analysis
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114774951A (en) * | 2022-03-14 | 2022-07-22 | 东华大学 | Graphene-based bipolar membrane and preparation method and application thereof |
| CN114887498A (en) * | 2022-06-21 | 2022-08-12 | 青岛大学 | Graphene oxide/sodium alginate composite nanofiltration membrane with controllable water flux or rejection rate |
| CN115025635A (en) * | 2022-06-30 | 2022-09-09 | 常州大学 | Preparation method of bridge organic silicon/GO composite nanofiltration membrane |
| CN115121134A (en) * | 2022-07-04 | 2022-09-30 | 重庆工商大学 | Preparation method of novel MXene-based composite membrane |
| CN117621592A (en) * | 2023-12-28 | 2024-03-01 | 苏州羽燕特种材料科技有限公司 | Antistatic high-barrier TPU film laminated composite fabric and preparation method thereof |
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| CN114774951A (en) * | 2022-03-14 | 2022-07-22 | 东华大学 | Graphene-based bipolar membrane and preparation method and application thereof |
| CN114887498A (en) * | 2022-06-21 | 2022-08-12 | 青岛大学 | Graphene oxide/sodium alginate composite nanofiltration membrane with controllable water flux or rejection rate |
| CN114887498B (en) * | 2022-06-21 | 2023-09-22 | 青岛大学 | Graphene oxide/sodium alginate composite nanofiltration membrane with controllable water flux or rejection rate |
| CN115025635A (en) * | 2022-06-30 | 2022-09-09 | 常州大学 | Preparation method of bridge organic silicon/GO composite nanofiltration membrane |
| CN115025635B (en) * | 2022-06-30 | 2023-08-18 | 常州大学 | A preparation method of bridge organosilicon/GO composite nanofiltration membrane |
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Application publication date: 20211217 |