CN113522059A - Folded graphene oxide film and preparation method thereof - Google Patents
Folded graphene oxide film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a wrinkled graphene oxide film and a preparation method thereof, and belongs to the technical field of new materials. The preparation method of the wrinkled graphene oxide film comprises the following steps: uniformly dispersing graphene oxide in a first organic solvent to obtain a graphene oxide dispersion liquid; pouring the graphene oxide dispersion liquid onto a support body with holes, and performing suction filtration to obtain a graphene oxide film adhered to the support body with holes; then removing the first organic solvent in the graphene oxide film; and standing the graphene oxide film without the first organic solvent in a second organic solvent, and finally removing the second organic solvent to obtain the wrinkled graphene oxide film. The folded graphene oxide membrane obtained by the preparation method is stable in structure, has excellent nanofiltration separation performance, and can be used in related fields such as water purification.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a wrinkled graphene oxide film and a preparation method thereof.
Background
In recent years, membrane separation technology has attracted attention because of the advantages of no phase change, low energy consumption, environmental friendliness and the like in the separation process. The two-dimensional material represented by graphene oxide is an ideal material for constructing a high-performance separation membrane due to the unique layered structure and adjustable physicochemical properties. The graphene oxide film shows excellent molecular transmission characteristics and has wide application prospects in various fields such as environment, resources, energy and the like.
However, the parallel arrangement of the interlayer channels in the graphene oxide membrane usually results in a narrow and tortuous molecular transmission path, so that the graphene oxide membrane has high mass transfer resistance and unsatisfactory separation performance. At present, many research reports adopt various methods such as physical intercalation, chemical modification and the like to focus on widening the channel size of the graphene oxide membrane or shortening the channel length of the graphene oxide membrane so as to realize the efficient separation of the graphene oxide membrane. However, these methods often require additional materials, complicated steps, delicate operations, and even precise instruments, and it is difficult to satisfy the requirements of simple process and reasonable investment in industrial production.
The spontaneously formed fold structure in the graphene oxide membrane can be used as an additional molecular rapid mass transfer channel. Therefore, it is necessary to develop an effective method for obtaining a wrinkled graphene oxide film having a regular ordered two-dimensional structure to achieve high performance of the graphene oxide film.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a folded graphene oxide membrane with a regular ordered two-dimensional structure and excellent nanofiltration performance and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a method of preparing a wrinkled graphene oxide film, comprising the steps of:
(1) uniformly dispersing graphene oxide in a first organic solvent to obtain a graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto a support body with holes, and performing suction filtration to obtain a graphene oxide film adhered to the support body with holes;
(3) removing the first organic solvent from the graphene oxide film of step (2);
(4) standing the graphene oxide film without the first organic solvent in the step (3) in a second organic solvent, and then removing the second organic solvent to obtain the wrinkled graphene oxide film.
According to the technical scheme, the proper first organic solvent and the proper second organic solvent are selected, and the proper mode is adopted to respectively remove the first organic solvent and the proper second organic solvent, so that the micro-wrinkle structure of the graphene oxide film can be reasonably regulated and controlled, and the wrinkled graphene oxide film with a regular ordered two-dimensional structure is formed. The process of removing the first organic solvent induces a graphene oxide film micro-scale folded structure, and the process of standing in the second organic solvent and removing the second organic solvent induces a graphene oxide film nano-scale folded structure. The wrinkled graphene oxide film obtained by the technical scheme of the invention has abundant wrinkles on the basis of a regular and ordered two-dimensional structure, wherein a narrow area in the wrinkled structure can play a role in screening to prevent large-size molecules from passing through; a wide area in the microcosmic fold structure of the graphene oxide film can provide a mass transfer space and promote the transfer of small-sized molecules; and the integral structure is stable, the nanofiltration separation performance is excellent, and the application prospect in the related fields of water purification and the like is good.
As a preferred embodiment of the method for producing a wrinkled graphene oxide film according to the present invention, in the step (1), the graphene oxide is a monodisperse graphene oxide nanosheet. The monodisperse graphene oxide nanosheet has a very high surface-to-volume ratio, and can be orderly stacked under the assistance of a solvent to form a regular two-dimensional layered membrane structure.
As a preferred embodiment of the method for preparing the wrinkled graphene oxide membrane, in the step (1), the first organic solvent is dimethyl sulfoxide (DMSO), N-methylformamide (NMF), N-Dimethylformamide (DMF), or N-methyl-2-pyrrolidone (NMP). The graphene oxide has good dispersibility in the solvent, is not easy to generate local agglomeration, and is beneficial to forming a film on a support body with holes by suction filtration in the follow-up process.
In a preferred embodiment of the method for preparing a wrinkled graphene oxide film according to the present invention, in the step (1), the graphene oxide is uniformly dispersed in the first organic solvent at a ratio of 0.005 to 0.1mg of the graphene oxide per milliliter of the volume of the first organic solvent. Too low of the above ratio may result in a decrease in the film preparation efficiency, and too high may result in a decrease in the dispersibility of the graphene oxide nanoplatelets in the solvent.
As a preferred embodiment of the preparation method of the wrinkled graphene oxide film, in the step (1), stirring and ultrasound are adopted as uniform dispersion modes, and more preferably, the stirring time is 10-60 min, the ultrasound power is 100-700W, and the ultrasound time is 5-30 min. Proper stirring and ultrasound are beneficial to uniform dispersion of the graphene oxide nanosheets in the solvent, and the excessively high ultrasonic power and the excessively long ultrasonic time can cause the undersize of the graphene oxide nanosheets, so that the structure and the performance of the graphene oxide film are influenced.
As a preferred embodiment of the preparation method of the wrinkled graphene oxide film, in the step (2), the suction filtration is pressure filtration or vacuum filtration, wherein the pressure of the pressure filtration is 0.1-0.6 MPa. Too low a pressure during pressure filtration leads to low membrane preparation efficiency, and too high a pressure leads to compression of the membrane channel structure.
In a preferred embodiment of the method for producing a wrinkled graphene oxide film according to the present invention, in the step (2), the porous support is made of polyacrylonitrile, polycarbonate, nylon, mixed cellulose ester, zirconia, alumina, zinc oxide, silicon oxide, or titanium oxide. The support material with the holes can provide enough mechanical strength for the graphene oxide film formed in the suction filtration film forming process.
As a preferred embodiment of the method for preparing the wrinkled graphene oxide membrane, in the step (2), the structure type of the porous support is a single-tube type, a multi-channel tube type, a hollow fiber type, a sheet type or a flat plate type.
In a preferred embodiment of the method for producing a wrinkled graphene oxide film according to the present invention, in the step (2), the average pore diameter of pores in the porous support is 50 to 1000 nm. The average pore diameter of the pores in the porous support is too small, so that extra mass transfer resistance is brought, the membrane separation efficiency is reduced, and the nano sheets are too large to fall into the pore channels of the porous support, so that a membrane cannot be formed.
In a preferred embodiment of the method for preparing the wrinkled graphene oxide film, in the step (3), the first organic solvent is removed by evaporation, wherein the evaporation temperature is 60-100 ℃ and the evaporation time is 4-12 h. The solvent evaporation treatment can vaporize the solvent remained in the graphene oxide film after the filtration film forming step to generate local steam bubbles, and the stress of the graphene oxide film layer is insufficiently released at the interface of the bubbles/liquid solvent/solid graphene oxide film layer due to the existence of surface tension, so that a micron-scale folded structure of the graphene oxide film is induced to be formed.
In a preferred embodiment of the method for preparing the wrinkled graphene oxide film, in the step (4), the standing time is 4-12 hours, and the second organic solvent is methanol, ethanol, butanol, ethyl acetate or n-hexane. The graphene oxide film can be shrunk by standing in the second organic solvent, because the graphene oxide has a self-avoiding tendency in the second organic solvent, namely the intermolecular interaction between the graphene oxide and the second organic solvent is weakened and is smaller than the threshold value of the intramolecular interaction of the graphene oxide, so that the graphene oxide nanosheet is promoted to be converted from a flat unfolded state to an aggregated collapsed state, a nano-scale folded structure of the graphene oxide sheet layer is induced to be formed, and the interlayer stacking structure of the graphene oxide film is not changed.
In the step (4), the second organic solvent is removed by vacuum drying, the vacuum drying temperature is 25-60 ℃, and the vacuum drying time is 12-36 hours. And removing the second organic solvent in the vacuum drying process to form a wrinkled graphene oxide film, wherein the low vacuum drying temperature can cause low film preparation efficiency, and the high vacuum drying temperature can cause partial reduction or removal of oxygen groups in the graphene oxide film to destroy the film structure.
In addition, the invention also provides a folded graphene oxide film prepared by the method.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is simple and easy to implement, does not need any modifier, cross-linking agent, intercalation agent or other additional materials, can recycle all the used organic solvents, and is energy-saving and environment-friendly. The wrinkled graphene oxide membrane obtained by the technical scheme of the invention has abundant wrinkles on a regular and ordered two-dimensional structure, has a stable structure and excellent nanofiltration separation performance, and has good application prospects in related fields such as water purification and the like.
Drawings
FIG. 1 is a scanning electron microscope photograph of a wrinkled graphene oxide film prepared in example 1;
FIG. 2 is a scanning electron microscope photograph of the wrinkled graphene oxide film prepared in example 2;
fig. 3 is a scanning electron microscope photograph of the wrinkled graphene oxide film prepared in example 3.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
According to the corrugated graphene oxide film disclosed by the embodiment of the invention, DMSO (dimethyl sulfoxide) is used as a first organic solvent, butanol is used as a second organic solvent to induce the preparation of the corrugated graphene oxide film:
(1) dispersing 5mg of graphene oxide nanosheets in 100mL of DMSO, stirring for 30 minutes, and performing 500W ultrasonic treatment for 10 minutes to obtain uniformly dispersed graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto a nylon flat plate type porous support body with the average pore diameter of 220nm, and performing vacuum filtration to obtain a graphene oxide film adhered to the porous support body;
(3) evaporating the graphene oxide film in the step (2), setting the evaporation temperature to be 100 ℃ and the evaporation time to be 4 h;
(4) standing the graphene oxide membrane without the DMSO in the step (3) in butanol for 4h, then carrying out vacuum drying treatment on the standing graphene oxide membrane, setting the vacuum drying temperature to be 45 ℃, and carrying out vacuum drying for 18h to obtain the DMSO/butanol induced wrinkling graphene oxide membrane, wherein the porosity is 5.25%.
Fig. 1 is a scanning electron microscope photograph of the wrinkled graphene oxide film prepared in example 1. As can be seen from fig. 1, the DMSO/butanol induced wrinkled graphene oxide film exhibited a rich wrinkled structure.
Example 2
According to the wrinkled graphene oxide film disclosed by the embodiment of the invention, NMF is used as a first organic solvent, and ethyl acetate is used as a second organic solvent to induce the preparation of the wrinkled graphene oxide film:
(1) dispersing 0.5mg of graphene oxide nanosheets in 100mL of NMF, stirring for 10 minutes, and carrying out 100W ultrasonic treatment for 30 minutes to obtain uniformly dispersed graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto an alumina single-tube type porous support body with the average pore diameter of 50nm, and performing pressure suction filtration to obtain a graphene oxide film adhered to the porous support body;
(3) evaporating the graphene oxide film in the step (2), setting the evaporation temperature to be 80 ℃ and the evaporation time to be 6 h;
(4) standing the graphene oxide film without the NMF in the step (3) in ethyl acetate for 8 hours, and then carrying out vacuum drying treatment on the graphene oxide film after standing, setting the vacuum drying temperature to be 25 ℃, and the vacuum drying time to be 36 hours to obtain the NMF/ethyl acetate induced wrinkled graphene oxide film, wherein the porosity is 9.55%.
Fig. 2 is a scanning electron microscope photograph of the wrinkled graphene oxide film prepared in example 2. As can be seen from fig. 2, the NMF/ethyl acetate induced wrinkled graphene oxide film exhibited a rich wrinkled structure.
Example 3
According to the wrinkled graphene oxide film disclosed by the embodiment of the invention, DMF (dimethyl formamide) is used as a first organic solvent, and n-hexane is used as a second organic solvent to induce the preparation of the wrinkled graphene oxide film:
(1) dispersing 10mg of graphene oxide nanosheets in 100mL of DMF, stirring for 60 minutes, and carrying out 700W ultrasonic treatment for 5 minutes to obtain uniformly dispersed graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto a mixed cellulose ester flat plate type porous support with the average pore diameter of 1000nm, and performing vacuum filtration to obtain a graphene oxide film adhered to the porous support;
(3) evaporating the graphene oxide film in the step (2), setting the evaporation temperature to be 60 ℃ and the evaporation time to be 12 h;
(4) and (3) standing the graphene oxide membrane without the DMF in the step (3) in n-hexane for 12h, then carrying out vacuum drying treatment on the standing graphene oxide membrane, setting the vacuum drying temperature to be 60 ℃, and carrying out vacuum drying for 12h to obtain the DMF/n-hexane induced wrinkled graphene oxide membrane, wherein the porosity is 20.30%.
Fig. 3 is a scanning electron microscope photograph of the wrinkled graphene oxide film prepared in example 3. As can be seen from fig. 3, the DMF/n-hexane induced wrinkled graphene oxide film exhibited a rich wrinkled structure.
Comparative example 1
Comparative example 1 a graphene oxide film was prepared by removing a first organic solvent through direct heat treatment on the basis of example 1 without using a second organic solvent treatment, and was prepared as follows:
(1) dispersing 5mg of graphene oxide nanosheets in 100mL of DMSO, stirring for 30 minutes, and performing 500W ultrasonic treatment for 10 minutes to obtain uniformly dispersed graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto a nylon flat plate type porous support body with the average pore diameter of 220nm, and performing vacuum filtration to obtain a graphene oxide film adhered to the porous support body;
(3) carrying out vacuum drying treatment on the graphene oxide film in the step (2), setting the vacuum drying temperature to be 45 ℃, and carrying out vacuum drying for 18 h; the comparative graphene oxide film was obtained, with a porosity of 3.66%.
The graphene oxide membranes obtained in the examples and comparative examples were subjected to nanofiltration separation performance test under the condition that the feed solution was 200ppm of rhodamine B dye solution, and the test results are shown in table 1:
as can be seen from table 1, the water permeability of the wrinkled graphene oxide film obtained in the present invention is significantly improved in the nanofiltration performance test compared to the graphene oxide film obtained in comparative example 1, in both example 1 and comparative example 1, DMSO is used as the first organic solvent, and other treatment parameters are the same, and compared to the two, the water permeability of the DMSO/butanol induced wrinkled graphene oxide film in example 1 is increased by 5.60 times compared to the water permeability of the DMSO-induced graphene oxide film in comparative example 1; meanwhile, the embodiment of the invention has higher dye retention rate. Therefore, the folded graphene oxide membrane prepared by the method can provide an additional molecular rapid mass transfer channel and has obviously more excellent nanofiltration separation performance.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of a wrinkled graphene oxide film is characterized by comprising the following steps:
(1) uniformly dispersing graphene oxide in a first organic solvent to obtain a graphene oxide dispersion liquid;
(2) pouring the graphene oxide dispersion liquid obtained in the step (1) onto a support body with holes, and performing suction filtration to obtain a graphene oxide film adhered to the support body with holes;
(3) removing the first organic solvent from the graphene oxide film of step (2);
(4) standing the graphene oxide film without the first organic solvent in the step (3) in a second organic solvent, and then removing the second organic solvent to obtain the wrinkled graphene oxide film.
2. The method for preparing a wrinkled graphene oxide film according to claim 1, wherein in the step (1), the graphene oxide is uniformly dispersed in the first organic solvent according to a ratio of 0.005-0.1 mg of the graphene oxide per milliliter of the volume of the first organic solvent.
3. The method for preparing a wrinkled graphene oxide membrane according to claim 1, wherein in the step (1), the first organic solvent is dimethyl sulfoxide, N-methylformamide, N-dimethylformamide or N-methyl-2-pyrrolidone.
4. The method for preparing a wrinkled graphene oxide film according to claim 1, wherein in the step (2), the average pore diameter of pores in the porous support is 50 to 1000 nm.
5. The method for preparing the wrinkled graphene oxide film according to claim 1, wherein in the step (3), the first organic solvent is removed by evaporation, wherein the evaporation temperature is 60-100 ℃ and the evaporation time is 4-12 h.
6. The method for preparing the wrinkled graphene oxide film according to claim 1, wherein in the step (4), the standing time is 4-12 h.
7. The method for preparing the wrinkled graphene oxide film according to claim 1, wherein in the step (4), the second organic solvent is methanol, ethanol, butanol, ethyl acetate or n-hexane.
8. The method for preparing the wrinkled graphene oxide film according to claim 1, wherein in the step (4), the second organic solvent is removed by vacuum drying, the vacuum drying temperature is 25-60 ℃, and the vacuum drying time is 12-36 h.
9. A wrinkled graphene oxide film, which is prepared by the method for preparing the wrinkled graphene oxide film according to any one of claims 1-8.
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