CN105148744A - Adjustable and controllable ultrathin two-dimensional nano g-C3N4 film, and preparation method and application thereof - Google Patents
Adjustable and controllable ultrathin two-dimensional nano g-C3N4 film, and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of separating film materials, and discloses an adjustable and controllable ultrathin two-dimensional nano g-C3N4 film, and a preparation method and application thereof. The preparation method comprises the following steps of performing heat treatment on dicyandiamide or cyanurtriamide under an inert atmosphere to obtain caked g-C3N4; pulverizing the caked g-C3N4 and calcining under an air atmosphere to obtain g-C3N4 powder; dispersing the g-C3N4 powder in solvent to obtain g-C3N4 two-dimensional nanosheet solution; adding electrolyte solution for modifying; depositing a g-C3N4 two-dimensional nanosheet on a porous carrier of which the pore diameter is greater than 200 nanometers to form a two-dimensional g-C3N4 ultrathin film; and drying to remove the solvent so as to obtain the adjustable and controllable ultrathin two-dimensional nano g-C3N4 film loaded on the porous carrier. The g-C3N4 film is high in water permeability and high in separation efficiency, and has a wide application prospect.
Description
Technical field
The invention belongs to separation membrane material technical field, be specifically related to a kind of controllable ultra-thin two-dimension nanometer g-C
3n
4film and preparation method thereof and application.
Background technology
Along with fast-developing economically, it is convenient that people greatly enjoy that social progress brings, but the series of problems brought by economy is also very important.For the country that this per capita resources of China is poor, problem of environmental pollution seems particularly outstanding, and particularly various industry and sanitary sewage have coverd with one deck shade to the water resource natively extremely lacked.Therefore, the science and technology of saving water resource and utilization advanced person carries out process recycling to waste water, has important strategic importance, meets national resources economizing type, environmentally friendly developing policy.
Advantages such as in numerous water technologies, UF membrane is because it is without phase transformation, and energy consumption is low, and efficiency is high, and cost is few and cause the extensive concern of people, and indispensable status is more and more occupied in the industrial production application of reality.But although widely used organic film low price, easy-formation, exists and easily pollutes, and resist chemical and machinery newly can be poor, the problems such as service life is short.Although inorganic ceramic membrane solves the problem of corrosivity and mechanical performance, preparation cost is high, and assembling difficulty still hampers it and further develops.Therefore, develop a kind of new membrane simultaneously possessing above-mentioned advantage and just seem particularly important.
Within 2004, British scientist utilizes graphite to prepare the Graphene of monatomic thickness, and it has the feature of two-dimensional layer, and obtains the Nobel Prize of 2010 thus.Subsequently, two-dimensional layer material is developed in succession, and is developed and applied in optics, electricity, magnetics, semiconductor and sensor field.By two-dimensional layer nanometer sheet assembling film forming, the space between lamella is utilized to be separated quickly and efficiently mixed solution, a treating capacity order of magnitude at least higher than conventional film of unit are, this New Two Dimensional film has easy assembling, resist chemical and mechanical performance strong, low cost and other advantages, represents the developing direction of new membrane.At present, the kind of two-dimensional films is single, except the Graphene basement membrane extensively studied, rarely has the research report of other two-dimensional films.But the preparation process of Graphene is loaded down with trivial details, preparation needs to consume a large amount of reagent or the energy, and easily to environment, and Graphene basement membrane Modulatory character is poor.
Summary of the invention
In order to solve the shortcoming and defect part of above prior art, primary and foremost purpose of the present invention is to provide a kind of controllable ultra-thin two-dimension nanometer g-C
3n
4the preparation method of film.
Another object of the present invention is to provide a kind of controllable ultra-thin two-dimension nanometer g-C prepared by said method
3n
4film.
Another object of the present invention is to provide a kind of above-mentioned controllable ultra-thin two-dimension nanometer g-C
3n
4the application of film in water treatment.
The object of the invention is achieved through the following technical solutions:
A kind of controllable ultra-thin two-dimension nanometer g-C
3n
4the preparation method of film, comprises following preparation process:
(1) dicyandiamide or melamine are put into atmosphere furnace, heat treatment under inert atmosphere and 400 ~ 700 DEG C of temperature, obtain the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, calcine in air atmosphere and at 500 ~ 600 DEG C, obtain the g-C after calcining
3n
4powder;
(3) by the g-C after calcining
3n
4powder dispersion is in solvent, centrifugal after ultrasonic process, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution;
(4) in the solution of step (3), add electrolyte solution and carry out modification, then by modified solution by Assembling of Nanoparticles by g-C
3n
4two-dimensional nano sheet is deposited on aperture and is greater than on the porous carrier of 200nm, forms two-dimentional g-C
3n
4ultrathin membrane, final drying, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on porous carrier
3n
4film.
Solvent described in step (3) refer to can fine dispersion calcining after g-C
3n
4the solvent of powder; Preferably, described solvent is water, methyl alcohol, ethanol, isopropyl alcohol or propyl alcohol.
The preferred KCl solution of electrolyte solution described in step (4), NaCl solution, NaOH solution or HCl solution.
Described Assembling of Nanoparticles refers to can by g-C
3n
4two-dimensional nano sheet is carried on the technology on porous carrier; Preferably, described Assembling of Nanoparticles refers to vacuum filtration, rotary coating, spraying or evaporation drying.
Preferably, described porous carrier refers to polycarbonate membrane, acetyl cellulose film, polyvinylidene fluoride film or anodic alumina films.
A kind of controllable ultra-thin two-dimension nanometer g-C
3n
4film, is prepared by above method.
Described controllable ultra-thin two-dimension nanometer g-C
3n
4the thickness of film is less than 1 micron.
Above-mentioned controllable ultra-thin two-dimension nanometer g-C
3n
4the application of film in water treatment, embody rule process is: will be carried on the controllable ultra-thin two-dimension nanometer g-C on porous carrier
3n
4film is fixed in separator, the nanometer impurity of different size and character in Separation of Water.
Preferably, described nanometer impurity refers to rhodamine B, azovan blue, nm of gold or methyl blue.
Principle of the present invention is: two-dimensional nano sheet is with electric charge, so that stable existence in the solution.In two-dimensional films forming process, due to the effect of Van der Waals force, namely like charges repels mutually, and the electric charge in nanometer sheet directly decides the size of interlamellar spacing.By adding electrolyte in solution, the quantity of electric charge in nanometer sheet and character all change, and then regulation and control interlamellar spacing, in order to the nanometer impurity of separation different size, and keep higher water flux simultaneously.
Preparation method of the present invention and the product tool obtained have the following advantages and beneficial effect:
(1) g-C of the present invention
3n
4by force, pliability is good for film resistance to chemical corrosion and mechanical performance, and water permeable ability is strong, and separative efficiency is high, and correspondingly can select the film of different layers spacing according to pollutant characteristics different in water;
(2) preparation process of the present invention does not use the material to human body and bad environmental, thus can not cause secondary pollution;
(3) preparation method of the present invention is simple, with low cost, favorable reproducibility, applicability strong, can mass industrialized production.
Accompanying drawing explanation
Fig. 1 is the g-C of embodiment 2
3n
4aFM (AFM) figure of two-dimensional nano sheet;
Fig. 2 is the controllable ultra-thin two-dimension nanometer g-C be carried on anodic alumina films of embodiment 3
3n
4the surface scan Electronic Speculum figure of film;
Fig. 3 is the controllable ultra-thin two-dimension nanometer g-C be carried on anodic alumina films of embodiment 3
3n
4the cross-sectional scans Electronic Speculum figure of film.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) dicyandiamide is put into atmosphere furnace, under an inert atmosphere, be raised to 700 DEG C of heat treatment 0.5h with 1 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 500 DEG C of calcining 3h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 1g calcining is got
3n
4powder dispersion is in 1500ml deionized water, and ultrasonic process 8h, then with the centrifugal 50min of 2000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.04mg/ml;
(4) the KCl solution adding 0.02mM in the solution of step (3) carries out modification, is then the polyvinylidene fluoride film of 450nm by aperture by modified solution under vacuum filtration condition, makes g-C
3n
4two-dimensional nano sheet is deposited on polyvinylidene fluoride film, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on polyvinylidene fluoride film
3n
4film.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on polyvinylidene fluoride film
3n
4film is fixed in filter, and process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, and its water permeable ability is 200L/m
2barh is 95% to the efficiency that retains of rhodamine B.
Embodiment 2
(1) dicyandiamide is put into atmosphere furnace, under an inert atmosphere, be raised to 550 DEG C of heat treatment 3h with 3 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 500 DEG C of calcining 2h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 0.5g calcining is got
3n
4powder dispersion is in 1000ml deionized water, and ultrasonic process 8h, then with the centrifugal 50min of 5000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.03mg/ml;
(4) the KCl solution adding 0.005mM in the solution of step (3) carries out modification, is then the polycarbonate membrane of 450nm by aperture by modified solution under vacuum filtration condition, makes g-C
3n
4two-dimensional nano sheet is deposited on polycarbonate membrane, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on polycarbonate membrane
3n
4film.
To the g-C that the present embodiment step (3) obtains
3n
4g-C in two-dimensional nano sheet solution
3n
4two-dimensional nano sheet carries out AFM (AFM) test, and result as shown in Figure 1.As seen from Figure 1: the thickness of nanometer sheet is about 1nm, show that there is monoatomic layer thickness.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on polycarbonate membrane
3n
4film is fixed in filter, and process size is 2nm, and concentration is the electronegative methylene blue dye aqueous solution of 20mg/L, and its water permeable ability is 300L/m
2barh is 93% to the efficiency that retains of methylene blue.
Embodiment 3
(1) melamine is put into atmosphere furnace, under an inert atmosphere, be raised to 600 DEG C of heat treatment 4h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 550 DEG C of calcining 2h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 2g calcining is got
3n
4powder dispersion is in 1500ml deionized water, and ultrasonic process 8h, then with the centrifugal 30min of 8000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.035mg/ml;
(4) the KCl solution adding 0.001mM in the solution of step (3) carries out modification, is then the anodic alumina films of 200nm by aperture by modified solution under vacuum filtration condition, makes g-C
3n
4two-dimensional nano sheet is deposited on anodic alumina films, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on anodic alumina films
3n
4film.
The controllable ultra-thin two-dimension nanometer g-C that what the present embodiment obtained be carried on anodic alumina films
3n
4the surperficial Electronic Speculum figure of film and cross section Electronic Speculum figure respectively as shown in Figures 2 and 3.As can be seen from Fig. 2 and Fig. 3, the controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the thickness of film is about 160nm.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on anodic alumina films
3n
4film is fixed in filter, and process size is 5nm, and concentration is the uncharged nm of gold aqueous solution of 500ppm, and its water permeable ability is 500L/m
2barh, retaining efficiency to nm of gold is 99%.
Embodiment 4
(1) melamine is put into atmosphere furnace, under an inert atmosphere, be raised to 400 DEG C of heat treatment 5h with 5 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 600 DEG C of calcining 1h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 2g calcining is got
3n
4powder dispersion is in 1000ml deionized water, and ultrasonic process 8h, then with the centrifugal 30min of 5000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.1mg/ml;
(4) NaCl solution adding 0.02mM in the solution of step (3) carries out modification, is then the acetyl cellulose film of 450nm by aperture under vacuum filtration condition by modified solution, makes g-C
3n
4two-dimensional nano sheet is deposited on acetyl cellulose film, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film is fixed in filter, and process size is 3nm, and concentration is the electronegative azovan blue aqueous dye solutions of 40mg/L, and its water permeable ability is 400L/m
2barh is 98% to the efficiency that retains of azovan blue.
Embodiment 5
(1) dicyandiamide is put into atmosphere furnace, under an inert atmosphere, be raised to 550 DEG C of heat treatment 3h with 3 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 500 DEG C of calcining 3h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 1g calcining is got
3n
4powder dispersion is in 1500ml deionized water, and ultrasonic process 8h, then with the centrifugal 30min of 5000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.05mg/ml;
(4) NaOH solution adding pH=12 in the solution of step (3) carries out modification, is then the acetyl cellulose film of 450nm by aperture under vacuum filtration condition by modified solution, makes g-C
3n
4two-dimensional nano sheet is deposited on acetyl cellulose film, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film is fixed in filter, and process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, and its water permeable ability is 300L/m
2barh is 93% to the efficiency that retains of rhodamine B.
Embodiment 6
(1) dicyandiamide is put into atmosphere furnace, under an inert atmosphere, be raised to 550 DEG C of heat treatment 3h with 3 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, in air atmosphere, be raised to 500 DEG C of calcining 3h with 2 DEG C/min, then Temperature fall is to normal temperature, obtains the g-C after calcining
3n
4powder;
(3) g-C after 1g calcining is got
3n
4powder dispersion is in 1500ml deionized water, and ultrasonic process 8h, then with the centrifugal 30min of 5000r/min, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution, recording its concentration by ultraviolet-visible spectrophotometer is 0.05mg/ml;
(4) the HCl solution adding pH=2 in the solution of step (3) carries out modification, is then the acetyl cellulose film of 450nm by aperture under vacuum filtration condition by modified solution, makes g-C
3n
4two-dimensional nano sheet is deposited on acetyl cellulose film, forms two-dimentional g-C
3n
4ultrathin membrane, then puts it in vacuum desiccator dry, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film.
The controllable ultra-thin two-dimension nanometer g-C of the present embodiment
3n
4the application of film in water treatment: by the above-mentioned controllable ultra-thin two-dimension nanometer g-C be carried on acetyl cellulose film
3n
4film is fixed in filter, and process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, and its water permeable ability is 150L/m
2barh is 98% to the efficiency that retains of rhodamine B.
Comparative example 1
Be fixed in filter by commercial ultra-filtration PS membrane, process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, its water permeable ability 300L/m
2barh is 16% to the efficiency that retains of rhodamine B.
Comparative example 2
Be fixed in filter by commercial ultra-filtration polycarbonate membrane, process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, its water permeable ability 12L/m
2barh is 53% to the efficiency that retains of rhodamine B.
Comparative example 3
Be fixed in filter by commercial ultra-filtration acetyl cellulose film, process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, its water permeable ability 5L/m
2barh is 87% to the efficiency that retains of rhodamine B.
Comparative example 4
Be fixed in filter by two dimensional oxidation graphene film, process size is 2nm, and concentration is the rhdamine B aqueous solution of 20mg/L positively charged, its water permeable ability 50L/m
2barh is 85% to the efficiency that retains of rhodamine B.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a controllable ultra-thin two-dimension nanometer g-C
3n
4the preparation method of film, is characterized in that: comprise following preparation process:
(1) dicyandiamide or melamine are put into atmosphere furnace, heat treatment under inert atmosphere and 400 ~ 700 DEG C of temperature, obtain the g-C lumpd
3n
4;
(2) by the g-C of caking
3n
4grind, again put into atmosphere furnace, calcine in air atmosphere and at 500 ~ 600 DEG C, obtain the g-C after calcining
3n
4powder;
(3) by the g-C after calcining
3n
4powder dispersion is in solvent, centrifugal after ultrasonic process, gets its supernatant, can obtain g-C
3n
4two-dimensional nano sheet solution;
(4) in the solution of step (3), add electrolyte solution and carry out modification, then by modified solution by Assembling of Nanoparticles by g-C
3n
4two-dimensional nano sheet is deposited on aperture and is greater than on the porous carrier of 200nm, forms two-dimentional g-C
3n
4ultrathin membrane, final drying, except the solvent on striping, can obtain the controllable ultra-thin two-dimension nanometer g-C be carried on porous carrier
3n
4film.
2. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 1
3n
4the preparation method of film, is characterized in that: the solvent described in step (3) is water, methyl alcohol, ethanol, isopropyl alcohol or propyl alcohol.
3. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 1
3n
4the preparation method of film, is characterized in that: the electrolyte solution described in step (4) refers to KCl solution, NaCl solution, NaOH solution or HCl solution.
4. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 1
3n
4the preparation method of film, is characterized in that: described Assembling of Nanoparticles refers to vacuum filtration, rotary coating, spraying or evaporation drying.
5. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 1
3n
4the preparation method of film, is characterized in that: described porous carrier refers to polycarbonate membrane, acetyl cellulose film, polyvinylidene fluoride film or anodic alumina films.
6. a controllable ultra-thin two-dimension nanometer g-C
3n
4film, is characterized in that: prepared by the method described in any one of Claims 1 to 5.
7. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 6
3n
4film, is characterized in that: described controllable ultra-thin two-dimension nanometer g-C
3n
4the thickness of film is less than 1 micron.
8. a kind of controllable ultra-thin two-dimension nanometer g-C described in claim 6 or 7
3n
4the application of film in water treatment, is characterized in that embody rule process is: will be carried on the controllable ultra-thin two-dimension nanometer g-C on porous carrier
3n
4film is fixed in separator, the nanometer impurity of different size and character in Separation of Water.
9. a kind of controllable ultra-thin two-dimension nanometer g-C according to claim 8
3n
4the application of film in water treatment, is characterized in that: described nanometer impurity refers to rhodamine B, azovan blue, nm of gold or methyl blue.
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