CN114671417B - Preparation method and application of nitrogen vacancy type carbon nitride with high specific surface area - Google Patents
Preparation method and application of nitrogen vacancy type carbon nitride with high specific surface area Download PDFInfo
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Abstract
The invention discloses a preparation method and application of nitrogen vacancy type carbon nitride with high specific surface area, and belongs to the technical field of nano material preparation. The invention takes melamine as raw material, and carries out high-temperature calcination polymerization to obtain yellow carbon nitride intermediate material; and placing the carbon nitride intermediate material into a tube furnace, introducing a mixed gas of small molecular organic acid steam and argon, performing high-temperature heat treatment, and cooling to obtain the nitrogen vacancy type carbon nitride with high specific surface area. The high specific surface area nitrogen vacancy type carbon nitride nanosheets synthesized by the method have the advantages of high yield, simple synthesis process, mild conditions, low cost and easy realization of large-scale preparation; the synthesis process only needs cheap melamine, lactic acid and formic acid as raw materials, and no special treatment equipment is needed; the prepared carbon nitride nano-sheet has large specific surface area, and a large number of nitrogen defects are introduced in the process of synthesizing the nano-sheet, so that the separation of electrons and holes is facilitated, and the photocatalytic performance is effectively improved.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method and application of nitrogen vacancy type carbon nitride with high specific surface area.
Background
Carbon nitride has been attracting attention in the field of photocatalysis due to its unique electronic structure, good thermal stability, simple preparation, rich raw materials, and the like. Since Wang first discovered photocatalytic hydrogen production of carbon nitride (nat. Mater.,2009,8,76-80), considerable effort has been directed to developing carbon nitride-based photocatalysts due to their great potential for solar energy conversion and chemical synthesis. Unfortunately, the direct high temperature thermal polycondensation synthesis of carbon nitride greatly limits the application of such materials in photocatalytic solar energy conversion due to its low specific surface area, rapid photo-generated charge carrier recombination, and weak adsorption and activation properties of substrate molecules. To overcome the above problems, various strategies have been employed for carbon nitride performance improvement, such as heteroatom doping, construction of heterojunctions and nanostructure designs have been developed to improve the electronic and catalytic properties of carbon nitride. Among them, vacancy/defect engineering is considered as an effective method for improving photocatalytic performance of carbon nitride. For example, zhang and colleagues reported that nitrogen vacancy-modified carbon nitrides may improve charge carrier separation, and thus the modified carbon nitrides have significantly enhanced photocatalytic hydrogen production capability (adv. We have discovered that carbon vacancies can promote CO 2 Activation, while stabilizing COOH intermediates, to increase CO 2 Kinetics of the reduction reaction (Angew.chem.int.ed., 2019,58,1134-1137). Despite great progress in the design and construction of carbon nitride vacancies/defects, the performance improvements remain limited. In addition, most reported vacancy/defect implantation methods require complex and cumbersome preparation procedures. Therefore, there is an urgent need to develop a simple and efficient method for implanting vacancy/defect sites on the surface of carbon nitride.
Disclosure of Invention
Aiming at the problems of complex synthesis process, poor controllability, pollution in the preparation process and the like of the existing vacancy-type carbon nitride, the invention provides a preparation method and application of the high-specific-surface-area nitrogen vacancy-type carbon nitride.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of nitrogen vacancy type carbon nitride with high specific surface area comprises the following steps:
step 1, taking melamine as a raw material, and performing high-temperature calcination polymerization to obtain a yellow carbon nitride intermediate material;
and 2, placing the carbon nitride intermediate material obtained in the step 1 into a tube furnace, introducing a mixed gas of small molecular organic acid steam and argon, performing high-temperature heat treatment, and cooling to obtain the nitrogen vacancy type carbon nitride with high specific surface area. The tube furnace is selected to prepare for ventilation in the early stage, so that the carbon nitride intermediate is ensured to react in the steam atmosphere of the micromolecular organic acid; small molecular organic acid is selected, and the small molecular organic acid is easy to decompose at high temperature; argon is used as carrier gas to introduce small molecular organic acid into the tube furnace, and the small molecular organic acid is decomposed to generate different oxygen-containing and carbon-containing free radicals under the high temperature condition, and the high-energy free radicals can attack the carbon nitride sheet layer to generate the nitrogen vacancy carbon nitride product.
Further, the temperature of the high temperature calcination polymerization in step 1 was 550 ℃. The melamine precursor has different polymerization degrees under different temperature treatments, wherein the 550 ℃ treatment is used for increasing the reaction degree and improving the polymerization degree.
Further, the constant temperature time of the high temperature calcination polymerization in the step 1 is 3 hours. The polymerization of the carbon nitride precursor has been substantially completed.
Further, the small molecular organic acid in the step 2 is lactic acid or formic acid. Lactic acid 122 ℃ and formic acid 108 ℃ have lower gasification decomposition temperature.
Further, the temperature of the high-temperature heat treatment in the step 2 is 100-600 ℃, and the time of the high-temperature heat treatment is 0.5-6 h. The purpose of the high temperature treatment is to control the degree of formic acid decomposition and to adjust the radical concentration. Formic acid has a boiling point of 100.8℃and the effect of the temperature on the extent of the reaction is investigated from the formic acid vapour temperature to a higher decomposition temperature. The degree of reaction between the free radicals and the carbon nitride intermediate can be adjusted by different treatment times, and the influence of the degree of reaction between the free radicals and the carbon nitride intermediate on the concentration of nitrogen vacancies is also investigated.
Further, the reaction heating rate in the high-temperature heat treatment process in the step 2 is 1-20 ℃/min.
Further, the pumping amount of the micromolecular organic acid steam in the step 2 is 0.1-20 mL/h; the flow rate of argon is 10-200 mL/min. The pumping quantity of the small molecular organic acid is regulated by regulating the flow rate of argon, so that the concentration of the free radical reactant is controlled.
Further, the volume ratio of the small molecular organic acid steam to the argon in the step 2 is 1/10000-1/10. And regulating the pumping amount of the small molecular organic acid and controlling the concentration of the free radical reactant.
The high specific surface area nitrogen vacancy type carbon nitride prepared by the preparation method is applied to photocatalytic carbon dioxide reduction and water decomposition hydrogen production under visible light, and has excellent photocatalytic performance.
Compared with the prior art, the invention has the following advantages:
(1) The high specific surface area nitrogen vacancy type carbon nitride nano-sheet synthesized by the invention has high yield and is easy to realize large-scale preparation;
(2) The synthesis process has the advantages of simple raw materials, mild conditions and few process steps;
(3) The invention has low synthesis cost, and the synthesis process only needs cheap melamine, lactic acid and formic acid as raw materials, and does not need special treatment equipment;
(4) The carbon nitride nano-sheet prepared by the method has large specific surface area, and a large number of nitrogen defects are introduced in the process of synthesizing the nano-sheet, so that the separation of electrons and holes is facilitated, and the photocatalytic performance is effectively improved.
Drawings
FIG. 1 is an X-ray powder diffraction pattern (XRD) of a carbon nitride intermediate and a nitrogen-vacancy-type carbon nitride nanosheet synthesized in example 1 of the present invention;
FIG. 2 is an electron paramagnetic resonance spectrum (EPR) of a carbon nitride intermediate and a carbon nitride nanoplatelet synthesized with example 1 of the present invention to obtain a nitrogen vacancy type;
FIG. 3 is a graph showing the isothermal desorption of nitrogen from a carbon nitride intermediate and a nitrogen-vacancy-type carbon nitride nanosheet synthesized in example 1;
FIG. 4 shows photocatalytic carbon dioxide reduction performance under visible light irradiation of bulk graphite phase carbon nitride and the nitrogen-vacancy-type carbon nitride nanoplatelets prepared in example 1 of the present invention.
FIG. 5 shows photocatalytic hydrogen evolution performance of bulk graphite phase carbon nitride and the nitrogen vacancy type carbon nitride nanoplatelets prepared in example 1 of the present invention under irradiation of visible light.
Detailed Description
The invention is further illustrated by the following examples of the invention, but the invention is not limited thereto.
Example 1
Step 1, 10g of melamine is taken and added into a ceramic crucible with a cover, high-temperature polymerization is carried out in a muffle furnace, the polymerization temperature is 550 ℃, the temperature is kept for 3 hours, and a yellow massive solid is obtained after cooling; grinding the sample to obtain yellow powder, namely a carbon nitride intermediate;
step 2, taking 0.2g of the carbon nitride intermediate prepared in the step 1, and introducing lactic acid steam/Ar mixed gas into a tube furnace, wherein the flow rate of the mixed gas is 100mL/min, the pumping amount of the lactic acid steam is 6mL/h, and the flow rate of argon is 99.9 mL/min; the volume ratio of the lactic acid steam to Ar is 1:1000; the reaction treatment temperature is 500 ℃, the reaction time is 3 hours, and the heating rate is 5 ℃/min. After the reaction is cooled to room temperature, the high specific surface area nitrogen vacancy type carbon nitride nano-sheet with the specific surface area of 160m can be obtained 2 And/g. Under the high temperature condition, small molecular organic acid is decomposed to generate different oxygen-containing and carbon-containing free radicals, and the high-energy free radicals can attack the carbon nitride sheet layer to generate a nitrogen vacancy carbon nitride product, and voids and hollows generated by vacancies increase the specific surface area of carbon nitride to a certain extent.
Example 2
Step 1, 10g of melamine is taken and added into a ceramic crucible with a cover, high-temperature polymerization is carried out in a muffle furnace, the polymerization temperature is 550 ℃, the temperature is kept for 3 hours, and a yellow massive solid is obtained after cooling; grinding the sample to obtain yellow powder, namely a carbon nitride intermediate;
step 2, taking 0.2g of the carbon nitride intermediate prepared in the step 1), and introducing lactic acid steam/Ar mixed gas into a tube furnace, wherein the flow rate of the mixed gas is 100mL/min, the pumping amount of the lactic acid steam is 15mL/h, and the flow rate of argon is 99.75 mL/min; the volume ratio of the lactic acid steam to Ar is 1:400; the reaction treatment temperature is 500 ℃, the reaction time is 2 hours, and the heating rate is 7 ℃/min. And cooling the reaction to room temperature to obtain the nitrogen vacancy type carbon nitride nano-sheet with high specific surface area.
Example 3
Step 1, 10g of melamine is taken and added into a ceramic crucible with a cover, high-temperature polymerization is carried out in a muffle furnace, the polymerization temperature is 550 ℃, the temperature is kept for 3 hours, and a yellow massive solid is obtained after cooling; grinding the sample to obtain yellow powder, namely a carbon nitride intermediate;
step 2, taking 0.2g of the carbon nitride intermediate prepared in the step 1), and introducing lactic acid steam/Ar mixed gas into a tube furnace, wherein the flow rate of the mixed gas is 100mL/min, the pumping amount of the lactic acid steam is (2.4 mL/h), and the flow rate of argon is (99.96 mL/min); the volume ratio of the lactic acid steam to Ar is 1:2500; the reaction treatment temperature is 500 ℃, the reaction time is 6 hours, and the heating rate is 10 ℃/min. And cooling the reaction to room temperature to obtain the nitrogen vacancy type carbon nitride nano-sheet with high specific surface area.
Example 4
Step 1, 10g of melamine is taken and added into a ceramic crucible with a cover, high-temperature polymerization is carried out in a muffle furnace, the polymerization temperature is 550 ℃, the temperature is kept for 3 hours, and a yellow massive solid is obtained after cooling; grinding the sample to obtain yellow powder, namely a carbon nitride intermediate;
step 2, taking 0.2g of the carbon nitride intermediate prepared in the step 1), and introducing formic acid steam/Ar mixed gas into a tube furnace, wherein the flow rate of the mixed gas is 50mL/min, the pumping amount of the formic acid steam is 6mL/h, and the flow rate of argon is 49.9 mL/min; the volume ratio of the formic acid steam to Ar is 1:500; the reaction treatment temperature is 500 ℃, the reaction time is 4 hours, and the heating rate is 15 ℃/min. And cooling the reaction to room temperature to obtain the nitrogen vacancy type carbon nitride nano-sheet with high specific surface area.
Example 5
Step 1, 10g of melamine is taken and added into a ceramic crucible with a cover, high-temperature polymerization is carried out in a muffle furnace, the polymerization temperature is 550 ℃, the temperature is kept for 3 hours, and a yellow massive solid is obtained after cooling; grinding the sample to obtain yellow powder, namely a carbon nitride intermediate;
step 2, taking 0.2g of the carbon nitride intermediate prepared in the step 1), and introducing formic acid steam/Ar mixed gas into a tube furnace, wherein the flow rate of the mixed gas is 200mL/min, the pumping amount of the formic acid steam is 12mL/h, and the flow rate of argon is 99.9 mL/min; the volume ratio of the formic acid steam to Ar is 1:1000; the reaction treatment temperature is 500 ℃, the reaction time is 1h, and the heating rate is 10 ℃/min. And cooling the reaction to room temperature to obtain the nitrogen vacancy type carbon nitride nano-sheet with high specific surface area.
Performance testing
Fig. 1 is an XRD pattern of a carbon nitride intermediate and a nitrogen-vacancy-type carbon nitride nano-sheet synthesized in the present invention, and it can be found that characteristic peaks (13.0 ° and 27.3 °) of the carbon nitride intermediate and the nitrogen-vacancy-type carbon nitride nano-sheet synthesized in the present invention have no significant change, indicating that the basic structure of carbon nitride remains unchanged after the high-temperature treatment of formic acid vapor in the present application.
FIG. 2 is an EPR spectrum of a carbon nitride intermediate and a nitrogen vacancy type carbon nitride nano-sheet synthesized by the invention, and the EPR signal of the carbon nitride after the high-temperature treatment of formic acid steam is obviously enhanced, which shows that the high-temperature treatment of the formic acid steam can successfully introduce nitrogen vacancies.
Fig. 3 nitrogen adsorption and desorption isotherm plot shows a significant increase in the specific surface area of nitrogen vacancy functionalized carbon nitride.
FIG. 4 is a graph showing photocatalytic carbon dioxide reduction performance of a carbon nitride intermediate and a nitrogen-vacancy-type carbon nitride nanosheet synthesized in accordance with the present invention under irradiation of visible light. By contrast, the high specific surface area nitrogen vacancy type carbon nitride nano-sheet prepared by the invention shows more excellent photocatalytic carbon dioxide reduction performance.
FIG. 5 is a graph showing photocatalytic hydrogen evolution properties of carbon nitride intermediates and nitrogen-vacancy-type carbon nitride nanoplatelets synthesized in accordance with the present invention under visible light irradiation. From the figure, it can be found that the nitrogen vacancy functionalized carbon nitride nano-sheet has significantly improved photocatalytic hydrogen gas precipitation performance.
Comparative example 1
A preparation method of high specific surface area defective carbon nitride comprises the following steps:
(1) Placing melamine in a muffle furnace, and roasting for 3 hours at 400 ℃ to obtain a carbon nitride intermediate; and (3) placing the carbon nitride intermediate and the ball mill ball into a ball milling tank of a planetary ball mill according to the mass ratio of the ball mill ball to the carbon nitride intermediate of 50:1, and ball milling for 6 hours at the rotating speed of 1500rpm to obtain the ball-milled carbon nitride intermediate.
(2) And (3) placing the ball-milled carbon nitride intermediate obtained in the step (1) in a muffle furnace, and roasting for 4 hours at 550 ℃ to obtain the high specific surface area defective carbon nitride. The specific surface area and the pore volume were 16.1m, respectively 2 /g and 0.068cm 3 /g。
Table 1 comparison results table
In summary, compared with the carbon nitride material without introducing the mixed gas of the small molecular organic acid steam and the argon, the nitrogen vacancy type carbon nitride has the specific surface area of 160m 2 Per g, the specific surface area is increased by 80 times compared with the carbon nitride intermediate; the synthesis process has the advantages of simple raw materials, mild conditions and few process steps, and is easier to realize large-scale preparation, and the specific comparison is shown in Table 1.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
What is not described in detail in the present specification belongs to the prior art known to those skilled in the art. While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.
Claims (4)
1. A preparation method of nitrogen vacancy type carbon nitride with high specific surface area is characterized by comprising the following steps: the method comprises the following steps:
step 1, taking melamine as a raw material, and performing high-temperature calcination polymerization to obtain a yellow carbon nitride intermediate material;
step 2, placing the carbon nitride intermediate material obtained in the step 1 into a tube furnace, introducing a mixed gas of small molecular organic acid steam and argon, performing high-temperature heat treatment, and cooling to obtain high-specific-surface-area nitrogen vacancy type carbon nitride;
the small molecular organic acid in the step 2 is lactic acid and formic acid; the pumping amount of the micromolecular organic acid steam in the step 2 is 0.1-20 mL/h;
the high-temperature calcination polymerization temperature in the step 1 is 550 ℃;
the temperature of the high-temperature heat treatment in the step 2 is 100-600 ℃, and the time of the high-temperature heat treatment is 0.5-6 h;
the flow rate of argon in the step 2 is 10-200 mL/min;
and 2, the volume ratio of the small molecular organic acid steam to the argon is 1/10000-1/10.
2. The method for producing a high specific surface area nitrogen-vacancy-type carbon nitride according to claim 1, characterized in that: the constant temperature time of the high temperature calcination polymerization in step 1 is 3h.
3. The method for producing a high specific surface area nitrogen-vacancy-type carbon nitride according to claim 1, characterized in that: and in the step 2, the reaction heating rate in the high-temperature heat treatment process is 1-20 ℃ per minute.
4. The use of the high specific surface area nitrogen vacancy-type carbon nitride produced by the production method according to any one of claims 1 to 3, characterized in that: the high specific surface area nitrogen vacancy type carbon nitride is applied to photocatalytic carbon dioxide reduction and water decomposition hydrogen production under visible light, and has excellent photocatalytic performance.
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