CN114592197B - Two-dimensional g-C 3 N 4 Nanosheet film, electrochemical preparation method thereof and application of nanosheet film in ion separation - Google Patents
Two-dimensional g-C 3 N 4 Nanosheet film, electrochemical preparation method thereof and application of nanosheet film in ion separation Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000926 separation method Methods 0.000 title claims description 22
- 239000002064 nanoplatelet Substances 0.000 claims abstract description 37
- 239000012528 membrane Substances 0.000 claims abstract description 36
- 150000002500 ions Chemical class 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 16
- 239000012498 ultrapure water Substances 0.000 claims abstract description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001652 electrophoretic deposition Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- 238000000502 dialysis Methods 0.000 claims abstract description 9
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 150000008040 ionic compounds Chemical class 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 31
- 238000000034 method Methods 0.000 description 10
- 239000012466 permeate Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 8
- 230000008859 change Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 3
- 229920005597 polymer membrane Polymers 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
-
- 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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
-
- 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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
-
- 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
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention discloses a two-dimensional g-C 3 N 4 A nano sheet membrane and an electrochemical preparation method thereof. The preparation method comprises the following steps: (1) Melamine, sodium hydroxide and water are mixed according to the mass volume ratio of (1-3) g: (0.5-1) g: (50-100) mL, and uniformly mixing to obtain electrolyte; the platinum sheet is used as an electrode, a direct current power supply with the voltage of 3-10V is electrified to react for 1-3 h, and the reacted electrolyte is subjected to centrifugal and dialysis treatment to obtain g-C 3 N 4 A nanoplatelet solution; (2) Fixing the treated porous substrate in the middle of U-shaped groove, inserting carbon plates as electrodes at two ends, adding g-C at one side of U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nano-sheet solution, electrifying to perform electrophoretic deposition, taking out the substrate after the deposition is completed, performing drying treatment,obtaining two-dimensional g-C 3 N 4 A nanoplatelet film. The two-dimensional g-C 3 N 4 The nano sheet film has higher interception effect on ions.
Description
Technical Field
The invention belongs to the technical field of ion separation membranes, and particularly relates to a two-dimensional g-C 3 N 4 The nanometer sheet film, its electrochemical preparation process and application in ion separation.
Background
With the overgrowth of population, the acceleration of industrialization progress, water pollution problem is becoming serious, and how to obtain clean water becomes a critical problem. Almost 97% of the water on earth is brackish water and seawater, and desalination of seawater and brackish water has become an important alternative source of clean water. Compared with the traditional desalting technology, the membrane separation technology has received a great deal of attention because of the advantages of small occupied area, low cost, convenient operation and the like.
In the membrane separation process, the most central problem is the development of membrane materials. At present, polymer membranes and ceramic membranes are used at most, but the polymer membranes have the problems of easy pollution, low flux and the like, and the ceramic membranes have the defects of high cost and the like, so that the application of the polymer membranes is greatly limited. Therefore, an ideal film with both ease of preparation of the organic film and thermal stability of the ceramic film would meet the needs of industrial applications.
In recent years, two-dimensional materials have appeared in the field of human vision and are used in the field of membrane separation, with the most representative two-dimensional membrane being a graphene oxide membrane. However, graphene oxide films are unstable in aqueous solutions and tend to swell. There is an urgent need to develop another two-dimensional material film for water treatment process. While two-dimensional graphite phase carbon nitride (g-C) 3 N 4 ) Compared with the graphene oxide film, the nano sheet film is simpler to prepare and higher in stability, and has industrial application potential in the separation field.
In general, the properties of two-dimensional nanoplatelet films are related to the quality of the nanoplatelets on the one hand and to the method of preparation of the film on the other hand. The quality of the nanoplatelets determines the stability of the membrane, while the method of preparation of the membrane determines to a large extent the integrity of the membrane, thus affecting its separation performance. Currently, g-C 3 N 4 NanoplateletsThe preparation is generally carried out by thermal polymerization to give bulk g-C 3 N 4 Stripping to obtain g-C 3 N 4 The nano-sheet, however, the process involves more steps and requires high temperature and other conditions, which easily results in g-C 3 N 4 The structure of the nano-sheet is destroyed; two-dimensional g-C 3 N 4 The preparation of the nano sheet membrane is generally to stack the nano sheets into a membrane by a suction filtration mode, but the process has longer time and low efficiency. Thus, if a high quality g-C can be produced by a simple method 3 N 4 Nanoplatelets and two-dimensional g-C 3 N 4 The nano sheet film has great significance to the development of industry when the nano sheet film has excellent separation performance.
Disclosure of Invention
To solve the disadvantages and shortcomings of the prior art, a primary object of the present invention is to provide a two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet membrane has the advantages of simple process, low energy consumption, less required raw materials, low cost, high repeatability and wide applicability, and is suitable for industrial production.
The second object of the present invention is to provide a two-dimensional g-C prepared by the above-mentioned preparation method 3 N 4 The nano sheet film has higher interception effect on ions.
A third object of the present invention is to provide a two-dimensional g-C 3 N 4 The application of the nano sheet membrane is particularly applied to the field of ion separation.
The primary purpose of the invention is realized by the following technical scheme:
two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet membrane comprises the following steps:
(1) Melamine, sodium hydroxide and water are mixed according to the mass volume ratio of (1-3) g: (0.5-1) g: (50-100) mL, and uniformly mixing to obtain electrolyte; the platinum sheet is used as an electrode, a direct current power supply with the voltage of 3-10V is used, the electrifying reaction time is 1-3 h, and the g-C is obtained after the centrifugalization and dialysis treatment of the electrolyte after the reaction 3 N 4 A nanoplatelet solution;
(2) Will beThe treated porous substrate is fixed in the middle of a U-shaped groove, carbon plates are inserted into two ends to serve as electrodes, and g-C is added into one side of the U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nanosheet solution, electrifying to perform electrophoretic deposition, taking out the substrate after the deposition is completed, and performing drying treatment to obtain two-dimensional g-C 3 N 4 A nanoplatelet film.
Preferably, the rotational speed of the centrifugation in the step (1) is 5000-10000 rpm; the centrifugation time is 30-60 min.
Preferably, the molecular weight of the dialysis bag used in the dialysis in the step (1) is 1000-5000 Da; the dialysis time is 3-5 days.
Preferably, the conditions of the electrophoretic deposition in step (2): the voltage is 15-30V and the time is 30-60 min.
Preferably, the g-C in step (2) 3 N 4 The thickness of the two-dimensional nano sheet film is 350-630 nm.
The second object of the invention is achieved by the following technical scheme:
two-dimensional g-C 3 N 4 The nano sheet film is prepared by the preparation method.
The third object of the present invention is achieved by the following technical scheme:
two-dimensional g-C 3 N 4 Use of nanoplatelet membranes in ion separation.
Specifically, the two-dimensional g-C 3 N 4 Use of a nanoplatelet membrane in ion separation comprising the steps of:
two-dimensional g-C 3 N 4 The nanometer sheet film is placed in an ion interception device, one side of the film is added with an ionic compound solution, and the other side of the film is added with water, so that ion interception is realized.
Preferably, the concentration of the ionic compound solution is 0.01 to 2mol/L.
Preferably, the concentration of the ionic compound solution is 0.1 to 0.2mol/L.
Preferably, the ionic compound is NaCl, liCl, caCl 2 ，MgCl 2 ，AlCl 3 ，CuSO 4 ，CdSO 4 Or MnSO 4 One of them.
Preferably, the water is ultrapure water or deionized water.
Compared with the prior art, the invention has the following advantages:
(1) The electrochemical method for preparing the two-dimensional g-C in the invention 3 N 4 The nano sheet film has the advantages of simple process, low energy consumption, less required raw materials, low cost, high repeatability and wide applicability, and is suitable for industrial production;
(2) The invention utilizes the two-dimensional g-C prepared by the electrophoretic deposition method 3 N 4 The nano sheet film has the advantages of good stability, strong pollution resistance and the like;
(3) The invention prepares the two-dimensional g-C by electrophoretic deposition 3 N 4 When the nano sheet film is used for ion interception, the nano sheet film has a higher interception effect on ions.
(4) g-C prepared by the invention patent 3 N 4 The nano-sheet membrane is mainly used for ion separation and mainly used for desalination treatment of seawater and brackish water.
Drawings
FIG. 1 is a two-dimensional g-C 3 N 4 Schematic preparation of the nanoplatelet film;
FIG. 2 is a two-dimensional g-C of example 1 3 N 4 A nanoplatelet Scanning Electron Microscope (SEM) image;
FIG. 3 is a two-dimensional g-C of example 1 3 N 4 A surface Scanning Electron Microscope (SEM) image of the nanoplatelet film;
FIG. 4 is a two-dimensional g-C of example 1 3 N 4 Cross-sectional Scanning Electron Microscope (SEM) images of the nanoplatelets film;
FIG. 5 is a two-dimensional g-C of example 1 3 N 4 The nanosheet membrane was tested against 0.2mol/LNaCl solution permeation, where the ordinate is the permeate side solution conductivity and the abscissa is time.
Detailed Description
The following describes the technical scheme of the present invention in further detail by referring to examples, but the embodiments and the protection scope of the present invention are not limited thereto.
The treated porous substrate referred to in this embodiment means that the substrate is first subjected to a metal spraying treatment.
Example 1
Two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet film specifically comprises the following steps:
(1) Dissolving 1g melamine and 1g sodium hydroxide in 50mL water as electrolyte, using platinum sheet as electrode, applying 5V voltage to two ends of the electrode by using DC power supply, centrifuging at 8000 rpm for 30min after reacting for 1 hr, and dialyzing for 3 days to obtain two-dimensional g-C 3 N 4 A nanoplatelet solution;
(2) Fixing the treated porous substrate in the middle of U-shaped groove, inserting carbon plates as electrodes at two ends, adding g-C at one side of U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nanosheet solution, electrifying to perform electrophoretic deposition, pouring out the solution, taking out the substrate, and vacuum drying in a vacuum drying tank to obtain two-dimensional g-C 3 N 4 Nanosheet film prepared by electrophoretic deposition method and used for preparing two-dimensional g-C 3 N 4 A schematic of the nanoplatelet film is shown in fig. 1.
Drying the two-dimensional g-C 3 N 4 The nanometer sheet film is placed into a U-shaped groove for middle fixation, raw material liquid is added to one side of the film, ultrapure water is added to the other side of the film, stirring is carried out by adding stirring rods to the two sides of the film, the change of the conductivity of pure water measurement solution along with time is measured, and the permeation quantity of different ions can be obtained through conversion.
g-C obtained in this example 3 N 4 The appearance of the nano sheet is shown in figure 2, and the nano sheet is loaded on the two-dimensional g-C of the anodic aluminum oxide film 3 N 4 The surface electron microscope image and the cross-section electron microscope image of the nano sheet film are respectively shown in fig. 3 and 4, and as can be seen from fig. 4, the two-dimensional g-C prepared in the embodiment 3 N 4 The thickness of the nanoplatelet film is about 450nm.
Two-dimensional g-C prepared in this example 3 N 4 Use of nanoplatelet membranes in ion separation:
mixing the prepared two-dimensional g-C 3 N 4 Gasket for nano sheet filmFixed in the middle channel of the ion permeability test U-shaped groove device, and NaCl, liCl, caCl with the mole/liter of 0.2 is respectively added at one side of the U-shaped groove 2 Or MgCl 2 A solution; 50mL of ultrapure water was added to the permeate side, stirred with stirring bars on both sides at 400rpm, and conductivity changes of the permeate side water were measured at room temperature using a conductivity meter. After 4h detection, two-dimensional g-C was found 3 N 4 Pair of nanoplatelets NaCl, liCl, caCl 2 Or MgCl 2 Average molar transfer rates of 2.63×10 respectively -2 mol/m 2 /h、1.86×10 -2 mol/m 2 /h、7.43×10 -2 mol/m 2 /h、3.59×10 -2 mol/m 2 Per h, 1mol/m compared to the permeation rate 2 The substrate of/h has a significant interception effect.
FIG. 4 is a graph of permeation testing of 0.2mol/LNaCl solution in application example 1 of the present invention, with the ordinate indicating the permeation side solution conductivity, and the abscissa indicating time.
Example 2
Two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet film specifically comprises the following steps: :
(1) Dissolving 0.8g melamine and 0.5g sodium hydroxide in 80mL water to obtain electrolyte, using platinum sheet as electrode, applying 3V voltage to two ends of the electrode by using DC power supply, centrifuging at 5000rpm for 60min after 2 hr reaction, and dialyzing for 4 days to obtain two-dimensional g-C 3 N 4 A nanoplatelet solution;
(2) Fixing the treated porous substrate in the middle of U-shaped groove, inserting carbon plates as electrodes at two ends, adding g-C at one side of U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nanosheet solution, and electrifying to perform electrophoretic deposition; the constant voltage is 30V, and the time is 60min; pouring out the solution, taking out the substrate, and vacuum drying in a vacuum drying tank to obtain two-dimensional g-C 3 N 4 A nanoplatelet film;
drying the two-dimensional g-C 3 N 4 The nanometer sheet film is placed into a U-shaped groove for middle fixing, raw material liquid is added into one side of the film, ultrapure water is added into the other side of the film, and stirring is added into the two sides of the filmStirring the mixture, measuring the change of the conductivity of the pure water measurement solution along with time, and obtaining the permeation quantity of different ions through conversion.
Two-dimensional g-C prepared in this example 3 N 4 The thickness of the nanoplatelet film is about 630nm.
Two-dimensional g-C prepared in this example 3 N 4 Use of nanoplatelet membranes in ion separation:
two-dimensional g-C to be prepared 3 N 4 The nanometer sheet film is fixed in the middle channel of the U-shaped groove device for ion transmission testing by a gasket, and 0.2mol/L MgCl is added at one side of the U-shaped groove 2 A solution; 50mL of ultrapure water was added to the permeate side, stirred with stirring bars on both sides at 400rpm, and conductivity change of the permeate side water was measured at room temperature using a conductivity meter. After 4h detection, the membrane was found to be MgCl 2 Average molar transfer rate of 2.35×10 -2 mol/m 2 Per h, 1mol/m compared to the permeation rate 2 The substrate of/h has a significant interception effect.
Example 3
Two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet film specifically comprises the following steps: (1) Dissolving 3g melamine and 1g sodium hydroxide in 100mL water as electrolyte, using platinum sheet as electrode, applying 10V voltage to two ends of the electrode by using DC power supply, centrifuging the obtained product solution at 10000rpm for 40min after 3h reaction, and dialyzing for 5 days to obtain two-dimensional g-C 3 N 4 A nanoplatelet solution;
(2) Fixing the treated porous substrate in the middle of U-shaped groove, inserting carbon plates as electrodes at two ends, adding g-C at one side of U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nano-sheet solution, and electrifying to perform electrophoretic deposition. The constant voltage is 30V, and the time is 30min; pouring out the solution, taking out the substrate, and vacuum drying in a vacuum drying tank to obtain two-dimensional g-C 3 N 4 A nanoplatelet film;
drying the two-dimensional g-C 3 N 4 The nanometer sheet film is placed in a U-shaped groove for middle fixing, raw material liquid is added to one side of the film, ultrapure water is added to the other side of the film, and two films are arrangedStirring by adding a stirrer at the side, measuring the change of the conductivity of the pure water measurement solution along with time, and obtaining the permeation quantity of different ions through conversion.
Two-dimensional g-C prepared in this example 3 N 4 The thickness of the nanoplatelet film is about 450nm.
Two-dimensional g-C prepared in this example 3 N 4 Use of nanoplatelet membranes in ion separation:
two-dimensional g-C to be prepared 3 N 4 The nanometer sheet film is fixed in the middle channel of the ion transmission testing U-shaped groove device by a gasket, and MgCl with the concentration of 1mol/L is added at one side of the U-shaped groove 2 A solution; 50mL of ultrapure water was added to the permeate side, stirred with stirring bars on both sides at 400rpm, and conductivity change of the permeate side water was measured at room temperature using a conductivity meter. After 4h detection, the membrane was found to be MgCl 2 Average molar transfer rate of 6.23×10 -2 mol/m 2 Per h, compared to a permeation rate of 8mol/m 2 The substrate of/h has a significant interception effect.
Example 4
Two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet film specifically comprises the following steps:
(1) Dissolving 1.5g melamine and 0.7g sodium hydroxide in 60mL water as electrolyte, using platinum sheet as electrode, applying 9V voltage to two ends of the electrode by using DC power supply, centrifuging the obtained product solution at 6000rpm for 60min after 2h of reaction, and dialyzing for 4 days to obtain two-dimensional g-C 3 N 4 A nanoplatelet solution;
(2) Fixing the treated porous substrate in the middle of U-shaped groove, inserting carbon plates as electrodes at two ends, adding g-C at one side of U-shaped groove 3 N 4 Adding ultrapure water to the other side of the nanosheet solution, and electrifying to perform electrophoretic deposition; the constant voltage is 30V, and the time is 30min; pouring out the solution, taking out the substrate, and vacuum drying in a vacuum drying tank to obtain two-dimensional g-C 3 N 4 A nanoplatelet film.
Drying the two-dimensional g-C 3 N 4 The nanometer sheet film is placed into a U-shaped groove for middle fixing, and the original is added at one side of the filmAnd adding ultrapure water to the other side of the membrane, adding stirring rods to stir the membrane, measuring the change of the conductivity of the pure water measurement solution along with time, and obtaining the permeation quantity of different ions through conversion.
Two-dimensional g-C prepared in this example 3 N 4 The thickness of the nanoplatelet film is about 450nm.
Two-dimensional g-C prepared in this example 3 N 4 Use of nanoplatelet membranes in ion separation:
two-dimensional g-C to be prepared 3 N 4 The nanometer sheet film is fixed in the middle channel of the ion transmission testing U-shaped groove device by a gasket, and MgCl with the concentration of 2mol/L is added at one side of the U-shaped groove 2 A solution; 50mL of ultrapure water was added to the permeate side, stirred with stirring bars on both sides at 400rpm, and conductivity change of the permeate side water was measured at room temperature using a conductivity meter. After 4h detection, the membrane was found to be MgCl 2 Average molar transfer rate of 8.75X10) -2 mol/m 2 Permeability rate of 12mol/m compared to the substrate 2 And/h has obvious interception effect.
The above examples are only preferred embodiments of the present invention, and are intended to be illustrative of the present invention, and not limiting, and any changes, substitutions, combinations, simplifications, modifications, etc. which would be made by those skilled in the art without departing from the spirit and principles of the present invention should be considered equivalent thereto, and are intended to be included in the scope of the present invention.
Claims (6)
1. Two-dimensional g-C 3 N 4 The electrochemical preparation method of the nano sheet film is characterized by comprising the following steps:
(1) Melamine, sodium hydroxide and water are mixed according to the mass volume ratio of (1-3) g: (0.5-1) g: (50-100) mL, and uniformly mixing to obtain electrolyte; the platinum sheet is used as an electrode, a direct current power supply with the voltage of 3-10V is used, the electrifying reaction time is 1-3 h, and the g-C is obtained after the centrifugalization and dialysis treatment of the electrolyte after the reaction 3 N 4 A nanoplatelet solution;
(2) The treated porous substrate is placed in the middle of the U-shaped groove for fixation, and carbon plates are inserted at two ends for electric conductionThe pole, one side of the U-shaped groove is added with g-C 3 N 4 Adding ultrapure water to the other side of the nanosheet solution, electrifying to perform electrophoretic deposition, taking out the substrate after the deposition is completed, and performing drying treatment to obtain two-dimensional g-C 3 N 4 A nanoplatelet film;
conditions of the electrophoretic deposition in step (2): the voltage is 15-30V, and the time is 30-60 min;
the g-C in step (2) 3 N 4 The thickness of the two-dimensional nano sheet film is 350-630 nm;
the molecular weight of a dialysis bag used in the dialysis in the step (1) is 1000-5000 Da; the dialysis time is 3-5 days.
2. The two-dimensional g-C of claim 1 3 N 4 The electrochemical preparation method of the nano sheet membrane is characterized in that the rotational speed of the centrifugation in the step (1) is 5000-10000 rpm; the centrifugation time is 30-60 min.
3. Two-dimensional g-C 3 N 4 A nanoplatelet film, characterized in that it is prepared according to the preparation method of any one of claims 1 to 2.
4. A two-dimensional g-C according to claim 3 3 N 4 Use of a nanoplatelet membrane for ion separation, characterized in that the ionic compound used in the ion separation is NaCl, liCl, caCl 2 Or MgCl 2 One of them.
5. The two-dimensional g-C of claim 4 3 N 4 Use of nanoplatelet membranes for ion separation, characterized in that the two-dimensional g-C 3 N 4 Use of a nanoplatelet membrane in ion separation comprising the steps of:
two-dimensional g-C 3 N 4 The nanometer sheet film is placed in an ion interception device, one side of the film is added with an ionic compound solution, and the other side of the film is added with water, so that ion interception is realized.
6. The two-dimensional g-C of claim 4 3 N 4 The application of the nano sheet membrane in ion separation is characterized in that the concentration of the ionic compound solution is 0.01-2 mol/L.
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