CN113604898B - Hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets and preparation method and application thereof - Google Patents
Hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets and preparation method and application thereof Download PDFInfo
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
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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
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/364—Membrane distillation
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4318—Fluorine series
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention belongs to the technical field of membrane materials, and particularly discloses a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets, and a preparation method and application thereof. The fluorinated graphite particles are used for replacing common graphite particles, and the modified Hummers method is used for preparing the high-fluorinated graphene oxide nanosheet material, so that the strong-hydrophobicity two-dimensional carbon nanomaterial can be directly obtained, and the problems of preparation cost and environmental pollution caused by reduction treatment of graphene oxide are avoided. The graphite fluoride particles exhibit high hydrophobicity and excellent chemical stability due to the inclusion of certain C-F bonds. The fluorinated graphene oxide nano sheet has a unique two-dimensional sheet structure, and meanwhile, the fluorine group endows the fluorinated graphene oxide nano sheet with high hydrophobicity, can be used as an additive material for preparing a super-hydrophobic nanofiber membrane material, is applied to the field of membrane distillation, and provides a novel membrane preparation process for membrane distillation industrialization.
Description
Technical Field
The invention belongs to the technical field of membrane materials, and particularly relates to a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets, and a preparation method and application thereof.
Background
In recent years, two-dimensional carbon nanomaterials including graphene oxide, reduced graphene oxide and graphene as additive materials are widely applied to the field of preparation of novel film materials. The two-dimensional carbon nanomaterial can significantly increase the conductivity of the polymer electrospinning solution, thereby promoting the generation of more uniform nanofiber filaments. Compared with graphene oxide, the graphene nanomaterial has strong hydrophobicity, but the current excessively high preparation cost greatly limits the large-scale application of the graphene nanomaterial. The graphene oxide nanomaterial is subjected to subsequent reduction treatment, so that functional groups on the surface of the graphene oxide can be removed to a certain extent, and the corresponding nanomaterial is called reduced graphene oxide. The hydrophobicity of the reduced graphene oxide nanoplatelets is enhanced due to the increase of the proportion of the non-oxidized regions. In terms of hydrophilicity and hydrophobicity, the reduced graphene oxide nanomaterial is interposed between graphene oxide and graphene. The hydrophobicity of the reduced graphite oxide nano-sheet is directly related to the reduction degree, and currently, strong reducing agents such as hydrazine hydrate, dimethylhydrazine, sodium borohydride and hydroiodic acid are mostly adopted to prepare the reduced graphite oxide nano-sheet, and high temperature and other harsh conditions are generally required, and meanwhile, the adopted reducing agents can cause potential secondary pollution to the environment.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the primary object of the invention is to provide a preparation method of a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanoplatelets.
The invention further aims to provide the hydrophobic electrospun nanofiber membrane based on the fluorinated graphene oxide nanosheets, which is prepared by the method.
It is still another object of the present invention to provide the use of the above-described hydrophobic electrospun nanofiber membranes based on fluorinated graphene oxide nanoplatelets in the field of membrane distillation.
The aim of the invention is achieved by the following scheme:
a preparation method of a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets comprises the following steps:
(1) Dispersing carbon fluoride in concentrated sulfuric acid/concentrated phosphoric acid solution, stirring, adding potassium permanganate after stirring, and continuously stirring to obtain a mixed solution; adding the obtained mixed solution into ice water, then adding hydrogen peroxide, standing, and collecting solid at the top of the liquid level to obtain the highly fluorinated graphene oxide nano-sheet;
(2) And ultrasonically dispersing the obtained high-fluorinated graphene oxide nano-sheets in a dimethylformamide solvent, dissolving polyvinylidene fluoride polymer in a dimethylformamide/acetone mixed solvent, mixing the two solutions to obtain a uniformly dispersed solution serving as an electrospinning polymer solution, and carrying out electrospinning to obtain the hydrophobic electrospinning nanofiber membrane based on the fluorinated graphene oxide nano-sheets.
The mass volume ratio of the fluorocarbon to the concentrated sulfuric acid/concentrated phosphoric acid solution in the step (1) is 1 g-50 mL:1g to 200mL, preferably 1g:100mL.
The volume ratio of the concentrated sulfuric acid to the concentrated phosphoric acid in the concentrated sulfuric acid/concentrated phosphoric acid solution in the step (1) is 6:1-12:1, preferably 9:1.
The mass ratio of the potassium permanganate to the fluorocarbon in the step (1) is 6-12: 2, preferably 9:2.
The volume mass ratio of the hydrogen peroxide to the fluorocarbon in the step (1) is 8-15 mL:4g; preferably 10mL:4g.
The temperature of the stirring for the first time in the step (1) is 40-60 ℃, and the stirring time is 2-6 h; the temperature of the second stirring is 80-90 ℃, and the stirring time is 6-24 h.
The concentration of the highly fluorinated graphene oxide nanoplatelets in the electrospun polymer solution in the step (2) is 1 to 10wt%, preferably 2 to 6wt%, and most preferably 4wt%.
The concentration of the polyvinylidene fluoride polymer in the electrospun polymer solution in the step (2) is 8-15 wt%, preferably 12wt%.
The concentration of dimethylformamide in the electrospun polymer solution in the step (2) is 40 to 48wt%, preferably 41 to 44.0wt%, and the concentration of acetone is 40 to 48wt%, preferably 41 to 44.0wt%.
The hydrophobic electrospun nanofiber membrane based on the fluorinated graphene oxide nanosheets is prepared by the method.
The application of a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanosheets in the field of membrane distillation.
Compared with the prior art, the invention has the following advantages:
the fluorinated graphite particles are used for replacing common graphite particles, and the modified Hummers method is used for preparing the highly fluorinated graphene oxide (Fluorinated graphene oxide, FGO) nanosheet material, so that the highly hydrophobic two-dimensional carbon nanomaterial can be directly obtained, and the problems of preparation cost and environmental pollution caused by reduction treatment of the graphene oxide are avoided. The graphite fluoride particles exhibit high hydrophobicity and excellent chemical stability due to the inclusion of certain C-F bonds. The fluorinated graphene oxide nano sheet has a unique two-dimensional sheet structure, and meanwhile, the fluorine group endows the fluorinated graphene oxide nano sheet with high hydrophobicity, can be used as an additive material for preparing a super-hydrophobic nanofiber membrane material, is applied to the field of membrane distillation, and provides a novel membrane preparation process for membrane distillation industrialization.
Drawings
FIG. 1 is a graph of nanofiber dimensions of a nanofiber membrane under different fluorinated graphene oxide nanoplatelet doping conditions; wherein (a) is FGO ENMs-1; (b) is FGO ENMs-2; (c) is FGO ENMs-4; (d) FGO ENMs-6.
FIG. 2 is a graph of membrane distillation permeate flux and rejection rate of nanofiber membranes under different fluorinated graphene oxide nanoplatelet doping conditions.
FIG. 3 is a steady-state analysis of the optimal membrane material.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available as usual unless otherwise specified.
Example 1
(1) 4g of fluorocarbon (60% of fluorination) was dispersed in 400mL of a concentrated sulfuric acid/concentrated phosphoric acid (volume ratio: 9:1) solution, stirred at 50℃for 4 hours, and then 18g of potassium permanganate powder was slowly added thereto, followed by stirring at 90℃overnight. The mixed solution was poured into ice water, and 10mL of hydrogen peroxide (30%) was added. After sufficient standing for stratification, brown solids at the top of the liquid surface were collected. Centrifugation was carried out at 6000rpm for 1 hour, and the residual impurities were removed by washing with 30wt% hydrochloric acid and absolute ethanol.
(2) 2wt% of the prepared highly fluorinated graphene oxide nanosheet material (FGO) is ultrasonically dispersed in a dimethylformamide solvent, and a certain amount of polyvinylidene fluoride polymer is dissolved in a dimethylformamide/acetone mixed solvent. The two solutions were mixed and stirred to form a uniform dispersion solution as an electrospinning polymer solution, and the nanofiber membrane was obtained by electrospinning (electrospinning parameters are shown in table 2). The specific proportioning parameters are shown in table 1:
TABLE 1 electrospinning solution formulation
TABLE 2 electrospinning parameters
Example 2
Referring to example 1, the addition amount of the highly fluorinated graphene oxide nanoplatelets in step (2) was changed to 1wt%, and the amounts of dimethylformamide and acetone were 43.5%.
Example 3
Referring to example 1, the addition amount of the highly fluorinated graphene oxide nanoplatelets in step (2) was changed to 4wt%, and the amounts of dimethylformamide and acetone were 42%.
Example 4
Referring to example 1, the addition amount of the highly fluorinated graphene oxide nanoplatelets in step (2) was changed to 6wt%, and the amounts of dimethylformamide and acetone were 41%.
The FGO addition amounts of the prepared electrospun nanofiber membranes were 1wt%, 2wt%, 4wt% and 6wt%, respectively, and were expressed as FGO ENMs-1, FGO ENMs-2, FGO ENMs-4 and FGO ENMs-6, respectively. The original polyvinylidene fluoride nanofiber membrane served as the control membrane PVDF ENMs.
Application examples
(1) Characterization of film materials
The nanofiber diameter distribution of the prepared nanofiber membrane was measured from a scanning electron microscope Image using Image J software. After determining the ratio of the pixel to the actual distance, the diameter of at least one hundred nanofibers is measured manually, ensuring that no repeated measurement of any same nanofibers occurs during the measurement. And calculating the statistical result by Gaussian fitting to obtain the diameter distribution and average diameter of the nanofibers of the nanofiber membrane.
(2) Membrane distillation performance test of membrane material
The membrane distillation performance of the prepared electrospun nanofiber membrane was evaluated by a laboratory-scale air gap membrane distillation test platform. In the device, forThe effective membrane area for mass transfer was 2.32cm 2 The air gap thickness was 4mm. NaCl at a concentration of 3.5wt% was placed as simulated seawater in a round bottom flask immersed in an oil bath to maintain the desired 70 ℃. The temperature of the condensate was maintained at 10 ℃. Stainless steel plates are used as condensing plates for condensing water vapor. The cross flow rate of the feed liquid and condensate was maintained at 10L/h by peristaltic pumps. The air gap membrane distillation system was started for 30 minutes before measurement so that there was enough time for the system to reach steady state, and then membrane performance was measured for different electrospun nanofiber membranes. The salt concentration was determined by means of a conductivity meter (INESA Scientific Instrument co., ltd. Ddsj-308F). Each film sample was tested three times and averaged.
The osmotic flux was calculated as follows:
J＝m/(A×t)
wherein J (L/m) 2 h) Is the permeate flux, m (kg) is the weight of distilled water, A (m 2 ) Is the membrane area and t (h) represents the duration of the operation.
The desalination rate is calculated according to the following equation:
SR＝(C f -C p )/C f ×100
wherein SR (%) represents the salt rejection, C f (g/L) and C p (g/L) represents the salt concentration of the feed solution and permeate water, respectively.
(3) Long term stability performance determination of membranes
The best membranes were chosen for long-term run experiments to verify their performance stability.
As can be seen from fig. 1, addition of FGO results in smaller nanofibers.
As can be seen from fig. 2, the addition of FGO increases the water flux and rejection of the electrospun nanofiber membrane.
From fig. 3, it can be seen that polyvinylidene fluoride electrospun nanofiber membranes with FGO content of 4wt% have strong stability in long-term membrane distillation operation.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the hydrophobic electrospun nanofiber membrane based on the fluorinated graphene oxide nanosheets is characterized by comprising the following steps of:
(1) Dispersing carbon fluoride in concentrated sulfuric acid/concentrated phosphoric acid solution, stirring, adding potassium permanganate after stirring, and continuously stirring to obtain a mixed solution; adding the obtained mixed solution into ice water, then adding hydrogen peroxide, standing, and collecting solid at the top of the liquid level to obtain the highly fluorinated graphene oxide nano-sheet;
(2) Ultrasonically dispersing the obtained high-fluorinated graphene oxide nano-sheets in a dimethylformamide solvent, dissolving polyvinylidene fluoride polymer in a dimethylformamide/acetone mixed solvent, mixing the two solutions to obtain uniformly dispersed solution serving as an electrospinning polymer solution, and carrying out electrospinning to obtain hydrophobic electrospinning based on the fluorinated graphene oxide nano-sheets;
and (2) the concentration of the highly fluorinated graphene oxide nano-sheets in the electrospinning polymer solution is 1-10wt%.
2. The method according to claim 1, characterized in that: and (2) the concentration of the high fluorinated graphene oxide nano-sheets in the electrospinning polymer solution is 2-6wt%.
3. The method according to claim 1, characterized in that: the mass volume ratio of the fluorocarbon to the concentrated sulfuric acid/concentrated phosphoric acid solution in the step (1) is 1g:50 mL-1 g:200mL.
4. The method according to claim 1, characterized in that:
the mass ratio of the potassium permanganate to the fluorocarbon in the step (1) is 6-12: 2; the volume mass ratio of the hydrogen peroxide to the fluorocarbon in the step (1) is 8-15 mL:4g.
5. The method according to claim 1, characterized in that: and (2) the concentration of the polyvinylidene fluoride polymer in the electrospinning polymer solution is 8-15 wt%.
6. The method according to claim 1, characterized in that: the concentration of dimethylformamide in the electrospinning polymer solution in the step (2) is 40-48wt%; the concentration of the acetone is 40-48wt%.
7. The method according to claim 1, characterized in that: the temperature of the stirring for the first time in the step (1) is 40-60 ℃, and the stirring time is 2-6 h; the temperature of the second stirring is 80-90 ℃, and the stirring time is 6-24 h.
8. A hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanoplatelets prepared by the method of any one of claims 1-7.
9. Use of a hydrophobic electrospun nanofiber membrane based on fluorinated graphene oxide nanoplatelets according to claim 8 in the field of membrane distillation.
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