CN112591742A - Nitrogen-sulfur co-doped porous graphitized carbon nano material and preparation method thereof - Google Patents
Nitrogen-sulfur co-doped porous graphitized carbon nano material and preparation method thereof Download PDFInfo
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a nitrogen and sulfur co-doped porous graphitized carbon nano material and a preparation method thereof, belonging to the technical field of environment-friendly functional carbon material preparation. The porous graphitized carbon nano material is a porous graphitized carbon nano sheet with a nitrogen group and a sulfur group, the porosity comprises 2-50 nm mesopores and micropores with the pore diameter smaller than 2nm, the mass fraction of sulfur is 0.15-0.62%, and the atomic ratio of nitrogen to sulfur is (15-37): 1. the preparation method comprises the steps of calcining thiourea at 400-600 ℃ for 2-6 hours, adding the obtained powder and glucose into a mixed solution of acetic acid and absolute ethyl alcohol, grinding and drying, pyrolyzing the obtained powder at 500-600 ℃ for 1-4 hours under protective gas, and pyrolyzing the powder at 600-800 ℃ for 2-5 hours. According to the invention, nitrogen and sulfur heteroatoms are doped into the carbon atom framework, so that more active sites are increased, and the removal capability of organic pollutants in water is greatly improved.
Description
Technical Field
The invention belongs to the technical field of preparation of environment-friendly functional carbon materials, and particularly relates to a nitrogen-sulfur co-doped porous graphitized carbon nano material and a preparation method thereof.
Background
In recent years, antibiotics and organic dyes are widely present in various water bodies, are difficult to biodegrade in natural environment, can be accumulated in aquatic environment for a long time, and cause great harm to the environment and human health. Therefore, how to rapidly and effectively remove antibiotics and organic dyes in water becomes urgent.
At present, technologies such as adsorption, photocatalysis, Advanced Oxidation Process (AOP), membrane separation, ion exchange, etc. have been used to remove organic pollutants in wastewater. Among these technologies, the adsorption technology is a promising technology for removing organic pollutants from wastewater due to its low cost, simple operation, and no secondary pollution. In addition, the sulfate radical advanced oxidation process (SR-AOPs) has been widely and effectively applied in the treatment of organic pollutants due to its advantages of high speed, high efficiency, low cost, etc. More importantly, SR-AOPs can mineralize most organic pollutants into nontoxic and harmless micromolecule CO2And H2And O. In view of the advantages of the adsorption method and the SR-AOPs method, the combination of the adsorption method and the SR-AOPs method is considered as a potential strategy for improving the removal efficiency of organic pollutants in wastewater. Therefore, it is important to find new nanomaterials that synergistically remove organic pollutants by adsorption and catalytic degradation processes.
In recent years, because the non-metal heteroatom (B, N, O, P, S) doped on the carbon ring can change the chemical inertness of the carbon in the six-membered ring and create new active sites (defects, active species of nitrogen and thiophenic sulfur), the heteroatom-doped carbon nano material not only can remarkably improve the catalytic activity, but also can further promote the adsorption performance in the field of removing organic pollutants in water. Unfortunately, however, a great deal of literature research on non-metal heteroatom-doped carbon nanomaterials has focused primarily on (1) studies on electrochemical performance; (2) doping of a single non-metallic heteroatom; (3) a single process is used to remove antibiotics from water. The research on the carbon nano material doped with multiple non-metal heteroatoms is very little, and the traditional carbon nano material doped with non-metal heteroatoms has low reuse rate and is not beneficial to application.
At present, due to the problems of complex process, high cost, harsh treatment process and the like, the actual synthesis of the nitrogen and sulfur co-doped carbon nano material still faces certain challenges, so that the invention develops a preparation method of the nitrogen and sulfur co-doped mesoporous carbon nano material with great potential and simplicity, and removes organic pollutants in the environment through the synergistic action of adsorption and catalytic degradation. Has important theoretical and practical significance for developing novel carbon-based nano-catalyst and restoring water environment.
Disclosure of Invention
Aiming at the defects of the prior art and the requirements of research and application in the field, the invention aims to provide a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and a preparation method thereof.
The technical scheme of the invention is as follows:
the nitrogen-sulfur-codoped porous graphitized carbon nanomaterial is characterized in that the porous graphitized carbon nanomaterial is a porous graphitized carbon nanosheet with a nitrogen group and a sulfur group, the porosity comprises a mesopore with a pore diameter of 2-50 nm and a micropore with a pore diameter smaller than 2nm, the atomic mass fraction of sulfur in the porous graphitized carbon nanomaterial is 0.15-0.62%, and the atomic ratio of nitrogen to sulfur is (15-37): 1.
further, the specific surface area of the porous graphitized carbon nano material is 10-700 m2/g。
Further, the nitrogen group is one or more of pyridine type N, pyrrole type N and graphite type N.
Further, the sulfur group is thiophene S (C-S-C).
A preparation method of a nitrogen and sulfur co-doped porous graphitized carbon nano material comprises the following steps:
and 2, mixing the powder A obtained in the step 1 with glucose according to the ratio of (1-6): adding 1 mass ratio of acetic acid to absolute ethyl alcohol into a mixed solution with a volume ratio of 1 (3-6) to obtain a suspension, fully grinding and airing to obtain powder B; wherein the concentration of the powder A in the suspension is 0.05-0.3 g/mL;
Further, the glucose in the step 2 is replaced by lignin, cellulose or chitosan.
Further, the flow rate of the nitrogen or argon in the step 3 is 50-100 mL/min.
Further, the washing in the step 3 is washing for 3-5 times by using deionized water; the drying is vacuum drying at 80 ℃ for 8-12 h.
Preferably, the calcination temperature in step 1 is 600 ℃ and the time is 4 h.
The nitrogen-sulfur-codoped porous graphitized carbon nano material is an environment functional material with good commercial prospect, can be used in the fields of adsorption, photocatalysis, electro-catalysis degradation of organic pollutants in water and the like, and further provides application of the nitrogen-sulfur-codoped porous graphitized carbon nano material in degradation of organic pollutants in water.
The invention has the beneficial effects that:
1. the method adopts glucose as a carbon source and thiourea as a nitrogen-sulfur raw material, and simultaneously dopes nitrogen and sulfur heteroatoms in the carbon nano material by a high-temperature pyrolysis method, so that more active sites are added to the carbon nano material; nitrogen and sulfur doping in carbocyclic rings can positively charge adjacent carbon rings and through π-The pi interaction adsorbs organic pollutants and potassium persulfate, then the generated active oxidation species (sulfate radicals, hydroxyl radicals and singlet oxygen) further oxidize and degrade antibiotics in the system, the synergistic action of adsorption and catalytic degradation greatly improves the removal capacity of the antibiotics in water, and meanwhile, the catalyst has excellent removal stability and repeatability, and solves the problem of low reuse rate of the traditional catalyst;
2. compared with the traditional metal-based carbon nanomaterial, the nitrogen-sulfur co-doped porous graphitized carbon nanomaterial provided by the invention does not contain metal elements, so that the problem of secondary pollution health risk caused by metal dissolution in the metal-based carbon nanomaterial is solved;
3. the preparation method of the nitrogen-sulfur co-doped porous graphitized carbon nanomaterial provided by the invention is simple to operate, is green and environment-friendly, has low cost of used raw materials, is convenient for large-scale production, and has great popularization significance.
Drawings
FIG. 1 is an SEM image of a nitrogen and sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800) obtained in example 1 of the present invention;
FIG. 2 is a TEM image of a nitrogen and sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800) obtained in example 1 of the present invention;
FIG. 3 is a graph of BET test data for materials obtained in examples 1 to 3 of the present invention and comparative examples 1 and 2; wherein, (a) is a data graph of the specific surface area of the material obtained in examples 1-3, (b) is a data graph of the pore diameter of the material obtained in examples 1-3, (c) is a data graph of the specific surface area of the material obtained in comparative examples 1 and 2, and the inner graph is a pore diameter data graph;
FIG. 4 is an XPS plot of nitrogen and sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800) obtained in example 1 of the present invention;
FIG. 5 is an XRD pattern of materials obtained in examples 1 to 3 of the present invention and comparative example 1;
FIG. 6 is a graph showing the effect of the materials obtained in examples 1 to 3 and comparative examples 1 and 2 of the present invention in removing antibiotics in water for the first time through adsorption and catalytic degradation;
FIG. 7 is a graph showing the effect of the nitrogen and sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800) obtained in example 1 of the present invention in the cyclic removal of antibiotics in water.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example prepares a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800) comprising the following steps:
And performing SEM and TEM tests on the obtained NS-C-800 respectively, wherein the test images are shown in figures 1 and 2, the SEM test shows that the obtained NS-C-800 is a nano sheet with a porous structure, and the TEM test shows that the nano sheet is a thin graphitized carbon nano sheet.
According to the BET test results shown in FIG. 3, it is found that the obtained NS-C-800 has an average pore diameter of 2.0 to 50nm and a pore volume of 0.84m3(g) a specific surface area of 651.80m as determined by BJH test method2/g。
From the XPS chart shown in FIG. 4, it is known that 3 nitrogen configurations, pyridine type N (398.57eV), pyrrole type N (399.54eV) and graphite type N (401.3eV), are present in the obtained NS-C-800, and it can be found that the binding energies at 163.3eV and 164.2eV in FIG. 4(d) are S2P attributed to thiophene S (C-S-C)3/2Peak sum S2P1/2Peak, so sulfur in the resulting NS-C-800 is present in the form of thiophene S (C-S-C), indicating that nitrogen and sulfur heteroatoms were successfully incorporated into the carbon atom backbone of the porous graphitized carbon nanomaterial.
From the XRD pattern as shown in fig. 5, it is known that the obtained NS-C-800 has a structure of graphitized carbon at 2 θ ═ 26.3.
The NS-C-800 obtained in the example was tested for antibiotic removal performance in water by the following specific steps:
(1) a50 mL, 20mg/L solution was prepared with tetracycline and transferred to a 100mL Erlenmeyer flask without pH adjustment.
(2) Accurately weighing 10mg of the obtained NS-C-800, adding the NS-C-800 into an erlenmeyer flask, putting the erlenmeyer flask into a constant temperature oscillator, oscillating at 150rpm and 25 ℃ for 30min to reach adsorption balance, then adding 0.0675g of potassium persulfate into the mixture of the NS-C-800 and the TC, and starting catalytic degradation reaction; the test concentrations were sampled at regular intervals.
As can be seen from the effect chart of the first removal of antibiotics in water shown in FIG. 6, the NS-C-800 obtained in the embodiment has excellent antibiotic removal capability, and can reach a removal rate of about 90% in 60min by adsorption and catalytic degradation methods; according to the effect diagram of the cyclic removal of the antibiotics in water shown in FIG. 7, it can be seen that the removal rate of TC still reaches 87.8% by the adsorption and catalytic degradation method after the NS-C-800 obtained in the present example is subjected to five cycles, which indicates that the NS-C-800 has better stability and repeatability in the process of removing the antibiotics in water.
Example 2
In this embodiment, a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-700) is prepared, and compared with embodiment 1, the preparation method is different only in that the temperature of the second pyrolysis in step 3 is adjusted from 800 ℃ to 700 ℃, that is, the temperature is first raised to 550 ℃ at a rate of 2 ℃/min, the pyrolysis is performed for 2 hours, then the temperature is raised to 700 ℃ at a rate of 2 ℃/min, and the further pyrolysis is performed for 2 hours; the other steps are unchanged.
According to the BET test results shown in FIG. 3, it is found that the obtained NS-C-700 has an average pore diameter of 2.0 to 50nm and a pore volume of 0.38m3Per g, specific surface area 217.20m2/g。
From the XRD pattern shown in fig. 5, it is known that NS-C-700 also has a structure of graphitized carbon at 2 θ ═ 26.3.
The NS-C-700 obtained in the example is subjected to the removal performance test of the antibiotics in water by adopting the method the same as that in the example 1, and as can be seen from the effect chart of removing the antibiotics in water for the first time shown in FIG. 6, the NS-C-700 obtained in the example can reach the removal rate of about 70% in 60min by the methods of adsorption and catalytic degradation.
Example 3
In this embodiment, a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-600) is prepared, and compared with embodiment 1, the preparation method is different only in that the temperature of the second pyrolysis in step 3 is adjusted from 800 ℃ to 600 ℃, that is, the temperature is first raised to 550 ℃ at a rate of 2 ℃/min, the pyrolysis is performed for 2 hours, then raised to 600 ℃ at a rate of 2 ℃/min, and the further pyrolysis is performed for 2 hours; the other steps are unchanged.
According to the BET test results shown in FIG. 3, it is found that the obtained NS-C-600 has an average pore diameter of 2.0 to 50nm and a pore volume of 0.14m3Per g, specific surface area 31.96m2NS-C-600 in g.
From the XRD pattern as shown in fig. 5, it is known that NS-C-600 obtained exhibited a clear diffraction peak at 2 theta 27.7,shows C3N4Possibly due to its lower calcination temperature.
The NS-C-600 obtained in the embodiment is subjected to the removal performance test of the antibiotics in water by adopting the method the same as the embodiment 1, and as can be seen from the effect chart of removing the antibiotics in water for the first time shown in FIG. 6, the NS-C-600 obtained in the embodiment can reach the removal rate of about 40% in 60min by the methods of adsorption and catalytic degradation.
Comparative example 1
Compared with the preparation method of example 1, the preparation method is only different in that the powder A obtained in the step 1 is not added in the step 2, namely 0.5g of glucose is added into a mixed solution of acetic acid and ethanol with the volume ratio of 1: 5; the other steps are unchanged.
From the BET test results as shown in FIG. 3, it is understood that the specific surface area of the obtained C is 4.6m2Per g, pore volume of 0.014cm3/g。
From the XRD pattern as shown in fig. 5, it is known that the spectrum of XRD of the obtained C has the structure of graphitized carbon.
The removal performance test of the antibiotics in water is carried out on the C obtained in the embodiment by adopting the same method as the embodiment 1, and as can be seen from an effect chart of removing the antibiotics in water for the first time shown in FIG. 6, the removal rate of the C obtained in the embodiment is only about 25% in 60min by adopting the methods of adsorption and catalytic degradation.
Comparative example 2
Compared with the preparation method of example 1, the preparation method of the carbon nano material (PC) without glucose is only different in that no glucose is added in step 2, namely 1g of A obtained in step 1 is added into a mixed solution of acetic acid and ethanol with the volume ratio of 1: 5; the other steps are unchanged.
From the BET test result as shown in FIG. 3, it is understood that the specific surface area of the obtained PC is 12.71m2Per g, pore volume of 0.054cm3/g。
The PC obtained in the embodiment is subjected to the removal performance test of the antibiotics in water by adopting the same method as the embodiment 1, and as can be seen from an effect chart of removing the antibiotics in water for the first time shown in FIG. 6, the PC obtained in the embodiment has a removal rate of only about 20% in 60min by adopting an adsorption and catalytic degradation method.
In conclusion, compared with the graphitized carbon nanomaterial (C) not doped with nitrogen and sulfur and the carbon nanomaterial (PC) not containing glucose, the nitrogen and sulfur co-doped porous graphitized carbon nanomaterial prepared by the method provided by the invention has the advantages that the capability of removing antibiotics in water is remarkably improved, and particularly for NS-C-800 with the temperature of 800 ℃ for secondary pyrolysis, the graphitized carbon nanomaterial has the largest pore volume and specific surface area, can provide the most active sites for the carbon nanomaterial, and has the most excellent capability of removing antibiotics in water.
Claims (9)
1. The nitrogen-sulfur-codoped porous graphitized carbon nanomaterial is characterized in that the porous graphitized carbon nanomaterial is a porous graphitized carbon nanosheet with a nitrogen group and a sulfur group, the porosity comprises a mesopore with a pore diameter of 2-50 nm and a micropore with a pore diameter smaller than 2nm, the mass fraction of sulfur in the porous graphitized carbon nanomaterial is 0.15-0.62%, and the atomic ratio of nitrogen to sulfur is (15-37): 1.
2. the nitrogen-sulfur co-doped porous graphitized carbon nanomaterial according to claim 1, wherein the nitrogen group is one or more of pyridine type N, pyrrole type N, and graphite type N.
3. The nitrogen-sulfur co-doped porous graphitized carbon nanomaterial according to claim 1, wherein the sulfur group is thiophene S.
4. The nitrogen and sulfur co-doped porous graphitized carbon nanomaterial according to claim 1, wherein the specific surface area of the porous graphitized carbon nanomaterial is 10-700 m2/g。
5. The preparation method of the nitrogen and sulfur co-doped porous graphitized carbon nano material is characterized by comprising the following steps of:
step 1, putting thiourea in a muffle furnace, raising the temperature to 400-600 ℃ at a heating rate of 1-5 ℃/min, and calcining for 2-6 h to obtain powder A;
and 2, mixing the powder A obtained in the step 1 with glucose according to the ratio of (1-6): adding 1 mass ratio of acetic acid to absolute ethyl alcohol into a mixed solution with a volume ratio of 1 (3-6) to obtain a suspension, and grinding and airing to obtain powder B; wherein the concentration of the powder A in the suspension is 0.05-0.3 g/mL;
step 3, placing the powder B obtained in the step 2 into a tubular furnace, under the protection of nitrogen or argon, raising the temperature to 500-600 ℃ at a heating rate of 1-5 ℃/min, performing pyrolysis for 1-4 h, raising the temperature to 600-800 ℃ at the same heating rate, and performing pyrolysis for 2-5 h; and then cooling to room temperature, washing and drying to obtain the nitrogen and sulfur co-doped porous graphitized carbon nano material.
6. The method for preparing the nitrogen-sulfur co-doped porous graphitized carbon nanomaterial according to claim 5, wherein the glucose in the step 2 is replaced by lignin, cellulose or chitosan.
7. The preparation method of the nitrogen-sulfur co-doped porous graphitized carbon nanomaterial according to claim 5, wherein the flow rate of the nitrogen or argon in the step 3 is 50-100 mL/min.
8. The preparation method of the nitrogen and sulfur co-doped porous graphitized carbon nanomaterial according to claim 5, wherein the washing in the step 3 is washing with deionized water for 3 to 5 times; the drying is vacuum drying at 80 ℃ for 8-12 h.
9. The application of the nitrogen and sulfur co-doped porous graphitized carbon nanomaterial disclosed in any one of claims 1 to 4 in adsorption and degradation of organic pollutants in water.
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