CN114405295A - High-flux graphene oxide hollow fiber composite nanofiltration membrane and preparation method thereof - Google Patents
High-flux graphene oxide hollow fiber composite nanofiltration membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-flux graphene oxide hollow fiber composite nanofiltration membrane and a preparation method thereof. The nano-fibers are embedded between the porous graphene oxide layers, the nano-pores in the surfaces of the porous graphene oxide layers provide additional transmission channels, the embedded nano-fibers can control the distance between the porous graphene oxide layers to form the nano-channels through which fluid can rapidly pass, and after the nano-channels are compounded with the porous structure of the graphene oxide, the molecular transmission path can be effectively shortened, so that the flux of the composite membrane can be improved, and the high selectivity of the composite membrane on water and dye can be maintained. The high-flux graphene oxide hollow fiber composite nanofiltration membrane has a good separation effect on dyes in water, is high in rejection rate, and has high water flux.
Description
Technical Field
The invention belongs to the field of separation membranes, and relates to a high-flux graphene oxide hollow fiber composite nanofiltration membrane and a preparation method thereof.
Background
In recent years, the textile industry in China develops rapidly, a large amount of printing and dyeing wastewater is inevitably generated, and serious environmental pollution and resource waste are caused, so that the problem of pollution of dye wastewater is urgently solved. Compared with the traditional separation technology such as rectification and molecular sieve adsorption, the membrane separation process has the advantages of operation at normal temperature, no phase change, small equipment volume, high efficiency, energy conservation, no pollution in the production process and the like.
Graphene oxide, one of the main derivatives of graphene, is a two-dimensional nanomaterial with a monoatomic layer thickness, whose lateral dimensions are up to tens of microns. The graphene oxide layers contain rich hydrophilic oxygen-containing functional groups, stable graphene oxide dispersion liquid can be formed, and the graphene oxide layer self-assembled film has the potential of large-scale application. The graphene oxide membrane can be divided into a flat membrane and a hollow fiber membrane according to the configuration, and compared with the flat membrane, the hollow fiber membrane has larger membrane area filled in a unit volume separator, and is more suitable for industrial production. Although the graphene oxide membrane has higher dye separation efficiency, the large-scale application of the graphene oxide membrane is limited due to small water flux, and the low permeation flux is a key technical problem to be solved by the graphene oxide membrane. The flux of the graphene oxide film can be increased in a limited way by intercalation of the nano particles and the nano wires, but the intercalation amount is low, and the flux of the composite film is increased slightly; the intercalation amount is increased, the flux of the composite membrane is greatly increased, but the retention rate is greatly reduced, and the requirement of high flux and high selectivity in practical application cannot be met.
The porous graphene oxide is a graphene oxide nanosheet material with nanoscale holes, the porous graphene oxide nanosheet contains some random or ordered carbon atom vacancies, and the porous characteristic enables the graphene nanosheet layer to form an additional water channel, so that the membrane flux can be remarkably improved without losing selectivity. For example, the chinese patent with the patent application number of 202110183596.3 discloses a preparation method of a porous graphene oxide nanofiltration membrane, which realizes in-plane pore-forming of graphene oxide nanosheets by chemically etching the graphene oxide nanosheets with concentrated sulfuric acid under the action of ultrasonication force. The porous graphene oxide nanofiltration membrane prepared by vacuum-assisted self-assembly has the advantages that the pure water flux is obviously improved, and the dye retention rate is slightly reduced. Furthermore, the interlayer distance can be enlarged by embedding the one-dimensional nano material between the porous graphene oxide layers, and the surface property of the porous graphene oxide film can be optimized through hybridization cooperation, so that the water flux of the composite film can be greatly improved. The nano fiber is a one-dimensional linear structure with a large length-diameter ratio, and some nano fibers have rich oxygen-containing functional groups on the surface, have excellent hydrophilicity and simultaneously have better chemical stability. The hydroxyapatite, the titanium dioxide and the polyaniline nanofiber which are low in synthesis cost and environmentally friendly are the best choice for the material embedded between the porous graphene oxide layers.
Disclosure of Invention
The invention provides a high-flux graphene oxide hollow fiber composite nanofiltration membrane and a preparation method thereof.
The technical scheme of the invention is as follows:
a high-flux graphene oxide hollow fiber composite nanofiltration membrane comprises a ceramic or polymer hollow fiber support body and a porous graphene oxide separation layer which is covered on the surface of the hollow fiber support body and is embedded with nanofibers.
In the technical scheme, the nano-fiber is one of hydroxyapatite nano-fiber, titanium dioxide nano-fiber and polyaniline nano-fiber; the diameter of the nano fiber is 50-200nm, and the length of the nano fiber is 1-100 mu m; the pore diameter of the porous graphene oxide is 2-50 nm; the mass ratio of the nano fibers to the porous graphene oxide in the separation layer is 1: 10-10: 1; the thickness of the separation layer is 10-900 nm.
The preparation method of the separation membrane comprises the following steps:
step 1, mixing the graphene oxide dispersion liquid with a 30% hydrogen peroxide solution, heating and reacting for a period of time, centrifuging to remove agglomerated particles, and diluting in deionized water to a specified concentration to obtain a porous graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid in the step 1 is 2-10 mg/mL; the volume ratio of the 30% hydrogen peroxide solution to the graphene oxide dispersion is 1: 20-1: 5. in the step 1, the heating temperature is 50-120 ℃, and the heating time is 2-6 h.
The concentration of the porous graphene oxide dispersion liquid in the step 1 is 0.2-200 mug/mL.
Step 2, adding the nano fibers into deionized water, stirring and ultrasonically dispersing to prepare nano fiber dispersion liquid, uniformly mixing the nano fiber dispersion liquid with the porous graphene oxide dispersion liquid in the step 1 to prepare a mixed solution with a certain mass ratio of nano fibers to porous graphene oxide; the concentration of the nanofiber dispersion liquid in the step 2 is 0.2-200 mug/mL. In the step 2, the mass ratio of the nano fibers to the porous graphene oxide is 1: 10-10: 1.
and 3, immersing the hollow fiber support body in the mixed solution obtained in the step 2, depositing a solute on the surface of the hollow fiber substrate through vacuum suction, and performing vacuum drying to obtain the porous graphene oxide hollow fiber composite nanofiltration membrane embedded with the nanofibers. And the vacuum filtration time in the step 3 is 10-100 min. In the step 3, the vacuum drying temperature is 20-50 ℃, and the drying time is 2-24 h.
According to the invention, the nano-fibers are embedded between the porous graphene oxide layers, the nano-pores in the surfaces of the porous graphene oxide layers provide additional transmission channels, the embedded nano-fibers can control the distance between the porous graphene oxide layers to form the nano-channels through which fluid can rapidly pass, and after the nano-fibers are compounded with the porous structure of the graphene oxide, the molecular transmission path can be effectively shortened, so that the flux of the composite membrane can be improved, and the high selectivity of the composite membrane on water and dye can be maintained. The high-flux graphene oxide hollow fiber composite nanofiltration membrane has a good separation effect on dyes in water, is high in rejection rate, and has high water flux.
Drawings
Fig. 1 is a cross-sectional scanning electron microscope photograph of the titanium dioxide nanofiber/porous graphene oxide hollow fiber composite nanofiltration membrane prepared in example 1.
Fig. 2 is a transmission electron microscope photograph of the porous graphene oxide nanosheet prepared in example 3.
Detailed Description
Comparative example 1
(1) Adding the graphene oxide material into deionized water to prepare graphene oxide dispersion liquid with the concentration of 0.2 mu g/mL. (2) And (2) carrying out vacuum filtration on the dispersion liquid obtained in the step (1) for 50min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support body, and carrying out vacuum drying at 20 ℃ for 2h to obtain the graphene oxide hollow fiber membrane.
Comparative example 2
(1) Adding the graphene oxide material into deionized water to prepare a graphene oxide dispersion liquid with the concentration of 20 mug/mL.
(2) Adding the titanium dioxide nano-fiber material into deionized water to prepare titanium dioxide nano-fiber dispersion liquid with the concentration of 20 mug/mL.
(3) Mixing the graphene oxide dispersion liquid in the step (1) and the titanium dioxide nanofiber dispersion liquid in the step (2) according to a mass ratio of 1: 1, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 50min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 50 ℃ for 24h to obtain the graphene oxide hollow fiber composite membrane.
Example 1
(1) Mixing 2mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 20: 1, mixing, heating at 50 ℃ for 2h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and re-dispersing the porous graphene oxide in deionized water to prepare a porous graphene oxide dispersion liquid with the concentration of 0.2 mu g/mL.
(2) Adding the titanium dioxide nano-fiber material into deionized water to prepare titanium dioxide nano-fiber dispersion liquid with the concentration of 0.2 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the titanium dioxide nanofiber dispersion liquid in the step (2) according to a mass ratio of 10: 1, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 10min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 20 ℃ for 2h to obtain the porous graphene oxide hollow fiber composite membrane.
Example 2
(1) Mixing 5mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 10: 1, mixing, heating at 80 ℃ for 4h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and dispersing in deionized water again to prepare porous graphene oxide dispersion liquid with the concentration of 20 mu g/mL.
(2) Adding the titanium dioxide nano-fiber material into deionized water to prepare titanium dioxide nano-fiber dispersion liquid with the concentration of 20 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the titanium dioxide nanofiber dispersion liquid in the step (2) according to a mass ratio of 1: 1, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 50min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 40 ℃ for 10h to obtain the porous graphene oxide hollow fiber composite membrane.
Example 3
(1) Mixing 10mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 5: 1, mixing, heating at 120 ℃ for 6h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and dispersing in deionized water again to prepare porous graphene oxide dispersion liquid with the concentration of 200 mu g/mL.
(2) Adding the titanium dioxide nano-fiber material into deionized water to prepare titanium dioxide nano-fiber dispersion liquid with the concentration of 200 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the titanium dioxide nanofiber dispersion liquid in the step (2) according to a mass ratio of 1: 10, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 100min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 50 ℃ for 24h to obtain the porous graphene oxide hollow fiber composite membrane.
The nanofiltration membranes prepared in comparative examples 1-2 and examples 1-3 were subjected to performance tests for pure water flux, dye rejection and permeation flux. Namely, at 25 ℃ and at a flow rate of 150L/h and an operating pressure of 0.2MPa, pure water, a 20mg/L rhodamine B (RhB) solution and a 20mg/L Evans Blue (EB) solution were used for the tests, and the results are shown in the following table:
example 4
(1) Mixing 2mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 20: 1, mixing, heating at 50 ℃ for 2h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and re-dispersing the porous graphene oxide in deionized water to prepare a porous graphene oxide dispersion liquid with the concentration of 0.2 mu g/mL.
(2) Adding the polyaniline nano-fiber material into deionized water to prepare polyaniline nano-fiber dispersion liquid with the concentration of 0.2 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the polyaniline nanofiber dispersion liquid in the step (2) according to a mass ratio of 10: 1, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 100min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 20 ℃ for 2h to obtain the porous graphene oxide hollow fiber composite membrane.
Example 5
(1) Mixing 10mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 5: 1, mixing, heating at 120 ℃ for 6h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and dispersing in deionized water again to prepare porous graphene oxide dispersion liquid with the concentration of 200 mu g/mL.
(2) Adding the polyaniline nano-fiber material into deionized water to prepare polyaniline nano-fiber dispersion liquid with the concentration of 200 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the polyaniline nanofiber dispersion liquid in the step (2) according to a mass ratio of 1: 10, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 10min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 50 ℃ for 24h to obtain the porous graphene oxide hollow fiber composite membrane.
Example 6
(1) Mixing 2mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 20: 1, mixing, heating at 50 ℃ for 2h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and re-dispersing the porous graphene oxide in deionized water to prepare a porous graphene oxide dispersion liquid with the concentration of 0.2 mu g/mL.
(2) Adding the hydroxyapatite nanofiber material into deionized water to prepare hydroxyapatite nanofiber dispersion liquid with the concentration of 0.2 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the hydroxyapatite nanofiber dispersion liquid in the step (2) according to a mass ratio of 10: 1, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 100min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 20 ℃ for 2h to obtain the porous graphene oxide hollow fiber composite membrane.
Example 7
(1) Mixing 10mg/mL of graphene oxide dispersion liquid with 30% of hydrogen peroxide solution according to a volume ratio of 5: 1, mixing, heating at 120 ℃ for 6h, centrifuging to remove agglomerated particles, freeze-drying the residual solution to obtain porous graphene oxide, and dispersing in deionized water again to prepare porous graphene oxide dispersion liquid with the concentration of 200 mu g/mL.
(2) Adding the hydroxyapatite nanofiber material into deionized water to prepare hydroxyapatite nanofiber dispersion liquid with the concentration of 200 mug/mL.
(3) Mixing the porous graphene oxide dispersion liquid in the step (1) and the hydroxyapatite nanofiber dispersion liquid in the step (2) according to a mass ratio of 1: 10, preparing a mixed solution.
(4) And (4) carrying out vacuum filtration on the dispersion liquid obtained in the step (3) for 10min, depositing a separation layer with the thickness of 10-900nm on a polyvinylidene fluoride hollow fiber support, and carrying out vacuum drying at 50 ℃ for 24h to obtain the porous graphene oxide hollow fiber composite membrane.
High retention rate and high water flux.
Claims (3)
1. The utility model provides a high flux oxidation graphite alkene hollow fiber composite nanofiltration membrane, includes ceramic or polymer hollow fiber supporter, its characterized in that: the porous graphene oxide separation layer is covered on the surface of the hollow fiber support body and is embedded with the nano fibers;
the nano-fiber is one of hydroxyapatite nano-fiber, titanium dioxide nano-fiber and polyaniline nano-fiber, the diameter is 50-200nm, and the length is 1-100 μm;
the pore diameter of the porous graphene oxide is 2-50 nm;
in the porous graphene oxide separation layer embedded with the nano fibers, the mass ratio of the nano fibers to the porous graphene oxide is 1: 10-10: 1; the thickness of the separation layer is 10-900 nm.
2. The preparation method of the high-flux graphene oxide hollow fiber composite nanofiltration membrane as claimed in claim 1, is characterized in that: comprises the following steps of (a) carrying out,
step 1: ultrasonically dispersing graphene oxide in a hydrogen peroxide solution, heating for reaction, centrifuging to remove agglomerated particles, and diluting in deionized water to a specified concentration to obtain a porous graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 2-10 mg/mL; the mass ratio of the hydrogen peroxide to the graphene oxide is 1: 20-1: 5; the heating reaction temperature is 50-120 ℃, and the heating time is 2-6 h; the concentration of the porous graphene oxide dispersion liquid is 0.2-200 mug/mL;
step 2, adding the nano fibers into deionized water, stirring and ultrasonically dispersing to prepare nano fiber dispersion liquid, and uniformly mixing the nano fiber dispersion liquid and the porous graphene oxide dispersion liquid in the step 1 to prepare a mixed solution of the nano fibers and the porous graphene oxide in a mass ratio; the concentration of the nanofiber dispersion liquid in the step 2 is 0.2-200 mug/mL; the mass ratio of the nano fibers to the porous graphene oxide is 1: 10-10: 1;
and step 3: and (3) immersing the hollow fiber support body in the mixed solution obtained in the step (2), depositing a solute on the surface of the hollow fiber substrate through vacuum suction, and performing vacuum drying to obtain the porous graphene oxide hollow fiber composite nanofiltration membrane embedded with the nanofibers.
3. The preparation method of the high-flux graphene oxide hollow fiber composite nanofiltration membrane according to claim 2, wherein the preparation method comprises the following steps: and in the step 3, the suction filtration time is 10-100min, the vacuum drying temperature is 20-50 ℃, and the vacuum drying time is 2-24 h.
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