CN115215305A - Method for effectively dispersing graphite phase carbon nitride - Google Patents
Method for effectively dispersing graphite phase carbon nitride Download PDFInfo
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- CN115215305A CN115215305A CN202210832663.4A CN202210832663A CN115215305A CN 115215305 A CN115215305 A CN 115215305A CN 202210832663 A CN202210832663 A CN 202210832663A CN 115215305 A CN115215305 A CN 115215305A
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
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Abstract
The invention relates to nanoparticle dispersion, in particular to a method for effectively dispersing graphite-phase carbon nitride; firstly, removing nickel oxide on the surface of foam nickel by acid treatment; secondly, soaking the processed foam nickel in an ethanol solution containing melamine, then taking out the foam nickel from the solution, and putting the foam nickel in a muffle furnace for calcination to obtain a mixture of graphite-phase carbon nitride and foam nickel; finally, dispersing the mixture in an acid solution for soaking to remove the nickel foam, and collecting the solid suspended in the acid solution by a centrifugal cleaning and drying method to obtain the graphite-phase carbon nitride with good dispersibility; the graphite phase carbon nitride precursor is dispersed in the foam nickel, so that the dispersibility of the graphite phase carbon nitride nanosheet is improved. The added foam nickel can remove NH generated during calcination 3 Catalytic decomposition into H 2 O, reduction of NH while dispersing graphite-phase carbon nitride 3 The release of the active ingredients meets the development concept of green environmental protection.
Description
Technical Field
The invention relates to nanoparticle dispersion, in particular to a method for effectively dispersing graphite-phase carbon nitride.
Background
Graphite phase carbon nitride (g-C) 3 N 4 ) The composite material has the advantages of large specific surface area, good physical and chemical properties, environmental friendliness, simplicity and convenience in preparation, low cost and the like, and is widely applied to design of functional materials such as fuel cells, supercapacitors, photocatalysis and the like. Furthermore, g-C with graphene-like structure 3 N 4 Having abundant surface groups (e.g. -NH) 2 or-NH groups) and good mechanical properties, which can be used to enhance the overall performance, properties of the polymer matrix.
Among the various methods currently being explored, ultrasonic stripping, thermal etching and ball milling methods have been used to convert bulk g-C 3 N 4 Layered into a monolayer or several layers of nanoplatelets. In fact, g-C 3 N 4 The reasonable strategy of layering is a template method, which can be divided into a soft template method and a hard template method according to different using methods. The soft template method adopts a soft structure directing agent comprising an amphiphilic molecule, an ionic liquid or a surfactant and a block copolymer, has self-assembly characteristics and enables g-C 3 N 4 Has a fine nano-porous structure. In contrast, the hard template method is a method using mesoporous SiO 2 Anodic aluminium oxide or CaCO 3 Nano-particle template fabrication of nano-structures g-C 3 N 4 This is nearly similar to typical nano-casting techniques. Although these methods produce different g-C 3 N 4 Controllable form, improved photoactivity and broad prospects in the field of sustainable chemical applications, but these methods often use expensive and toxic reagents and more complex preparation processes. Therefore, the g-C with low development cost, simple process and environmental protection 3 N 4 The layering method is important.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method for effectively dispersing graphite phase carbon nitride. By dispersing the graphite phase carbon nitride precursor in the foam nickel, the foam nickel can simultaneously remove NH generated during calcination 3 Catalytic decomposition into H 2 O, reduction of NH while dispersing graphite-phase carbon nitride 3 Is released.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for effectively dispersing graphite phase carbon nitride comprises the steps of firstly, removing nickel oxide on the surface of foam nickel by acid treatment; secondly, soaking the processed foam nickel in an ethanol solution containing melamine, taking out the foam nickel from the solution, and calcining the foam nickel in a muffle furnace to obtain a mixture of graphite-phase carbon nitride and foam nickel; and finally, dispersing the mixture in an acid solution for soaking to remove the nickel foam, and collecting the solid suspended in the acid solution by a centrifugal cleaning and drying method to obtain the graphite-phase carbon nitride with good dispersibility.
The present invention provides a direct and green process for preparing few-layer porous graphite-phase Carbon Nitride Nanoplates (CNNS) by heating melamine rich nickel foam in air, in contrast to bulk graphite-phase carbon nitride (BCN) prepared by traditional direct calcination. It is noteworthy that nickel is a promising NH 3 A decomposition catalyst which is low in cost but high in activity. Decomposition of NH 3 Catalytically generated H 2 The O atmosphere effectively separates the graphite phase carbon nitride nanosheets and leaves a pore structure on the nanosheets, thereby increasing the specific surface area of the graphite phase carbon nitride and improving the physical and chemical properties of the graphite phase carbon nitride.
A method for effectively dispersing graphite phase carbon nitride specifically comprises the following steps:
step (1), foam nickel pretreatment: cutting the foamed nickel into squares, placing the square in an acid solution for ultrasonic treatment, and then washing the square with deionized water until the square is neutral;
step (2), preparing a graphite phase carbon nitride/foamed nickel mixture: soaking the foamed nickel treated in the step (1) in an ethanol solution of melamine, drying the foamed nickel by using a vacuum oven, putting the dried foamed nickel into a crucible of 5ml, covering the crucible with a cover, and calcining the foamed nickel in a muffle furnace;
and (3) separating graphite phase carbon nitride: and dispersing the mixture of graphite-phase carbon nitride and foamed nickel obtained after the calcination treatment in an acid solution, performing ultrasonic treatment to remove foamed nickel, taking the turbid suspension of the upper layer, placing the suspension in a centrifuge for centrifugation, washing the solid obtained by centrifugation with deionized water and ethanol to be neutral, and finally drying to obtain the graphite-phase carbon nitride with good dispersibility.
Preferably, the area of the foam nickel after cutting in the step (1) is 3 to 5cm 2 The acid solution in the step (1) is hydrochloric acid solution with the concentration of 1-4M, and the ultrasonic time in the acid solution in the step (1) is 5-20min.
Preferably, the concentration of the melamine ethanol solution in the step (2) is 40 to 60 percent, and the soaking time of the nickel foam in the melamine ethanol solution in the step (2) is 4 to 12h.
Preferably, the drying parameters of the vacuum oven in the step (2) are as follows: vacuum at 60-80 deg.c for 2-6 hr, and cooling naturally to room temperature.
Preferably, the calcination parameters in the muffle furnace in the step (2) are as follows: under the air condition, the heating rate is 1 to 5 ℃/min, the temperature is raised to 500 to 600 ℃, then the temperature is kept for 1 to 3 hours, and then the mixture is naturally cooled to the room temperature.
Preferably, the acid solution in the step (3) is a hydrochloric acid solution with the concentration of 1 to 4M, and the ultrasonic time of the mixture in the acid solution is 2 to 4h.
Preferably, the centrifugation parameters in step (3) are: rotating speed: 6000 to 8000r/min, and the time is 3 to 5min.
In addition, the invention also provides application of the method for effectively dispersing graphite-phase carbon nitride in nanoparticle dispersion.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for effectively dispersing graphite phase carbon nitride, which improves the dispersibility of graphite phase carbon nitride nanosheets by dispersing a graphite phase carbon nitride precursor in foamed nickel.
Compared with the prior art, the added foam nickel can remove NH generated during calcination 3 Catalytic decomposition into H 2 O, reduction of NH while dispersing graphite-phase carbon nitride 3 The release of the active carbon meets the development concept of environmental protection. Decomposition of NH 3 Catalytically generated H 2 O atmosphere is effectiveThe graphite phase carbon nitride nanosheets are separated and leave a pore structure on the nanosheets, so that the specific surface area of the graphite phase carbon nitride is increased, and the physical and chemical properties of the graphite phase carbon nitride are improved.
Drawings
Fig. 1 is an SEM image of graphite-phase carbon nitride prepared in example 1 of the present invention and comparative example 1.
Fig. 2 is an XRD spectrum of graphite-phase carbon nitride prepared in example 1 of the present invention and comparative example 1.
Fig. 3 is a graph showing FITR of graphite-phase carbon nitride prepared in example 1 of the present invention and comparative example 1.
Fig. 4 is a TG diagram of graphite-phase carbon nitride prepared in example 1 of the present invention and comparative example 1.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
Cutting foamed nickel into 20mm-20mm squares, placing the squares in a 3M hydrochloric acid solution for ultrasonic treatment for 15min, and then washing the squares to be neutral by using deionized water; soaking the processed foam nickel in 50% melamine ethanol solution for 12h, drying for 4h at 80 ℃ in a vacuum oven, placing the dried foam nickel in a crucible of 5ml, covering the crucible, heating to 550 ℃ in a muffle furnace in the air atmosphere at a heating rate of 5 ℃/min, keeping for 2h, and naturally cooling to room temperature; and dispersing the mixture of graphite-phase carbon nitride and foamed nickel obtained after calcination treatment in a 3M hydrochloric acid solution for 3h by ultrasonic treatment to remove foamed nickel, taking the turbid suspension at the upper layer, placing the turbid suspension in a centrifuge, centrifuging the turbid suspension for 5min at a speed of 8000r/min, washing the turbid suspension to be neutral by deionized water and ethanol, and finally drying the turbid suspension to obtain the graphite-phase carbon nitride with good dispersibility.
An SEM image of the graphite-phase Carbon Nitride Nanosheets (CNNS) prepared in this example is shown in fig. 1b, and it can be seen that the nanosheets after treatment have a lamellar structure. The XRD pattern of the graphite phase carbon nitride nanosheet prepared in this example is shown in FIG. 2, and two distinct diffraction peaks are present at 12.3 ° and 27.8 ° respectively due to the inter-planar structure stacking ((100) and the inter-layer stacking structure (002)The FITR map of the rice flakes is shown in FIG. 3, notably at 1105cm -1 There is a distinct peak corresponding to the C-O oscillation of CNNS indicating the presence of a group containing O. This should be caused by a steam reforming reaction or an oxidation etching. The TG diagram of the graphite-phase carbon nitride nanosheets prepared in this example is shown in fig. 4, and CNNS also shows a broad endothermic peak around 250 ℃, which is related to the removal of — OH.
Comparative example 1:
the difference from the above example is that:
directly calcining the precursor without adding foamed nickel in the calcining process;
and (3) calcining 0.5g of melamine in a muffle furnace, grinding the graphite-phase carbon nitride obtained after the calcining treatment, and collecting the solid to obtain the comparative graphite-phase carbon nitride (BCN).
The SEM image of the graphite phase carbon nitride prepared in this comparative example is shown in FIG. 1, which shows that the nanoparticles are greatly agglomerated. The XRD pattern of the graphite-phase carbon nitride prepared in this comparative example is shown in fig. 2. The FITR map of the graphite-phase carbon nitride prepared in this comparative example is shown in FIG. 3. The TG pattern of the graphite-phase carbon nitride prepared in this comparative example is shown in FIG. 4.
Example 2
Cutting foamed nickel into 20mm-20mm squares, putting the squares into a 1M hydrochloric acid solution, performing ultrasonic treatment for 20min, and then washing the squares to be neutral by using deionized water; soaking the processed foam nickel in 40% melamine ethanol solution for 12h, drying for 4h at 80 ℃ in a vacuum oven, placing the dried foam nickel in a crucible of 5ml, covering the crucible with a cover, heating to 500 ℃ in a muffle furnace in the air atmosphere at a heating rate of 5 ℃/min, keeping for 3h, and naturally cooling to room temperature; and dispersing the mixture of the graphite-phase carbon nitride and the foamed nickel obtained after the calcination treatment in a 3M hydrochloric acid solution for 3h by ultrasonic treatment to remove the foamed nickel, taking the turbid suspension at the upper layer, placing the turbid suspension in a centrifuge, centrifuging the turbid suspension for 5min at the speed of 6000r/min, washing the turbid suspension to be neutral by deionized water and ethanol, and finally drying the turbid suspension to obtain the graphite-phase carbon nitride with good dispersibility.
Example 3
Cutting foamed nickel into 20mm-20mm squares, placing the squares in a 4M hydrochloric acid solution, performing ultrasonic treatment for 5min, and then washing the squares to be neutral by using deionized water; soaking the processed foam nickel in an ethanol solution of melamine with the concentration of 60% for 4h, drying the foam nickel in a vacuum oven at the temperature of 80 ℃ for 4h, placing the dried foam nickel in a crucible with the volume of 5ml, covering the crucible, heating the foam nickel to 600 ℃ in a muffle furnace in the air atmosphere at the heating rate of 5 ℃/min, keeping the foam nickel for 2h, and naturally cooling the foam nickel to the room temperature; and dispersing the mixture of graphite-phase carbon nitride and foamed nickel obtained after calcination treatment in a 2M hydrochloric acid solution, performing ultrasonic treatment for 4h to remove foamed nickel, taking the turbid suspension liquid at the upper layer, placing the turbid suspension liquid in a centrifuge, centrifuging the turbid suspension liquid at a speed of 7000r/min for 5min, washing the turbid suspension liquid with deionized water and ethanol to be neutral, and finally drying the turbid suspension liquid to obtain the graphite-phase carbon nitride with good dispersibility.
Claims (9)
1. A method for effectively dispersing graphite phase carbon nitride is characterized in that firstly, foam nickel is treated by acid to remove surface nickel oxide; secondly, soaking the processed foam nickel in an ethanol solution containing melamine, then taking out the foam nickel from the solution, and putting the foam nickel in a muffle furnace for calcination to obtain a mixture of graphite-phase carbon nitride and foam nickel; and finally, dispersing the mixture in an acid solution for soaking to remove the nickel foam, and collecting the solid suspended in the acid solution by a centrifugal cleaning and drying method to obtain the graphite-phase carbon nitride with good dispersibility.
2. The method of claim 1, further comprising the steps of:
step (1), foam nickel pretreatment: cutting the foamed nickel into squares, placing the square in an acid solution for ultrasonic treatment, and then washing the square with deionized water until the square is neutral;
step (2), preparing a graphite phase carbon nitride/foamed nickel mixture: soaking the foamed nickel treated in the step (1) in an ethanol solution of melamine, drying the foamed nickel by using a vacuum oven, placing the dried foamed nickel in a crucible of 5ml, covering the crucible with a cover, and calcining the foamed nickel in a muffle furnace;
and (3) separating graphite phase carbon nitride: and dispersing the mixture of the graphite-phase carbon nitride and the foamed nickel obtained after the calcination treatment in an acid solution, performing ultrasonic treatment to remove the foamed nickel, taking the turbid suspension on the upper layer, centrifuging the suspension in a centrifuge, washing the centrifuged solid to be neutral by deionized water and ethanol, and finally drying to obtain the graphite-phase carbon nitride with good dispersibility.
3. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the area of the nickel foam after being cut in the step (1) is 3 to 5cm 2 And (2) performing ultrasonic treatment on the acid solution in the step (1) for 5 to 20min, wherein the acid solution in the step (1) is a hydrochloric acid solution with the concentration of 1 to 4M.
4. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the concentration of the melamine ethanol solution in the step (2) is 40 to 60 percent, and the soaking time of the nickel foam in the melamine ethanol solution in the step (2) is 4 to 12h.
5. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the drying parameters of the vacuum oven in the step (2) are as follows: vacuum at 60-80 deg.c for 2-6 hr, and cooling naturally to room temperature.
6. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the calcination parameters in the muffle furnace in the step (2) are as follows: under the air condition, the heating rate is 1 to 5 ℃/min, the temperature is raised to 500 to 600 ℃, then the temperature is kept for 1 to 3 hours, and then the mixture is naturally cooled to the room temperature.
7. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the acid solution in the step (3) is hydrochloric acid solution with concentration of 1 to 4M, and the ultrasonic time of the mixture in the acid solution is 2 to 4h.
8. The method for effectively dispersing graphite-phase carbon nitride according to claim 2, wherein the centrifugation parameters in the step (3) are as follows: rotating speed: 6000 to 8000r/min, and the time is 3 to 5min.
9. Use of a method of effectively dispersing graphite phase carbon nitride as described in claims 1-8 in nanoparticle dispersion.
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