CN113845107A - Method for preparing porous carbon nanosheet by virtue of two-dimensional covalent organic framework pyrolysis - Google Patents
Method for preparing porous carbon nanosheet by virtue of two-dimensional covalent organic framework pyrolysis Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 239000002135 nanosheet Substances 0.000 title claims abstract description 35
- 239000013310 covalent-organic framework Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 13
- 239000000376 reactant Substances 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 150000001412 amines Chemical class 0.000 claims abstract description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 15
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 12
- 150000001299 aldehydes Chemical class 0.000 claims description 11
- 239000012046 mixed solvent Substances 0.000 claims description 9
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical group C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical group O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims description 5
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 4
- 229920002866 paraformaldehyde Polymers 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 239000003575 carbonaceous material Substances 0.000 abstract description 4
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- WTTWSMJHJFNCQB-UHFFFAOYSA-N 2-(dibenzylamino)ethanol Chemical compound C=1C=CC=CC=1CN(CCO)CC1=CC=CC=C1 WTTWSMJHJFNCQB-UHFFFAOYSA-N 0.000 description 6
- 150000002894 organic compounds Chemical class 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- AAMATCKFMHVIDO-UHFFFAOYSA-N azane;1h-pyrrole Chemical compound N.C=1C=CNC=1 AAMATCKFMHVIDO-UHFFFAOYSA-N 0.000 description 2
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 239000013474 COF-1 Substances 0.000 description 1
- 239000013479 COF-300 Substances 0.000 description 1
- 239000002262 Schiff base Substances 0.000 description 1
- 150000004753 Schiff bases Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 239000013384 organic framework Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention discloses a method for preparing a porous carbon nanosheet by virtue of pyrolysis of a two-dimensional covalent organic framework, and relates to the method for preparing the porous carbon nanosheet. The invention aims to solve the technical problem that the specific capacitance of the existing porous carbon material prepared by COF is low. The method comprises the following steps: reacting an aldehyde reactant with an amine reactant under the protection of nitrogen to obtain a polymer; and then putting the polymer into a tubular furnace, and heating the polymer in a nitrogen atmosphere to obtain the porous carbon nanosheet. The specific surface area of the porous carbon nano sheet reaches 300.847m2g‑1～1496.588m2g‑1The aperture is 3.132 nm-3.713 nm. The specific capacitance of the electrode prepared by the porous carbon nano-sheet is 500-630F g‑1The impedance is 0.8-2.7 omega, and the electrochemical device can be used in the field of electrochemistry.
Description
Technical Field
The invention relates to a method for preparing porous carbon nanosheets.
Background
The covalent organic Compound (COF) is generally formed by covalent bonds formed among elements such as C, B, O, N, theoretically, the covalent organic compound has a long-range ordered framework, a nano porous structure and a huge pi conjugated system, so that a good path can be provided for electron transmission, and the covalent organic compound can be well used for preparing photoelectric devices, semiconductors, automobiles, electronic equipment and the like. Among them, a porous carbon material having a high specific surface area, high thermal stability and uniform pore size distribution can be prepared by carbonization using a covalent organic compound, and, for example, Chinese patent publication No. CN107720720A discloses a method for preparing porous carbon based on a covalent organic framework material, which uses COF-300, COF-320, COF-366, TPB-DMTP-COF, Dhatph-COF, TpPa-1-COF, IL COF-1, Tp-Azo-COF, Py-2,2 '-BPyPh COF, Pd @ Py-2, 2' -BPyPh COF, Mn/Pd @ Py-2,2 '-BPyPh, and [ HO ] Py-2, 2' -BPyCOF]Taking X% -Py-COFs and DhaTab-COF as raw materials, and carbonizing in a nitrogen atmosphere to obtain the micro/mesoporous framework material with high specific surface area and high physicochemical stability. The BET specific surface area of the porous carbon material reaches 1130m2And the mass specific capacitance of the porous carbon electrode is 50-90F/g. The capacitance value of the porous carbon electrode is relatively low.
Disclosure of Invention
The invention provides a method for preparing a porous carbon nanosheet by utilizing two-dimensional covalent organic framework pyrolysis, aiming at solving the technical problem that the specific capacitance of a porous carbon material prepared by using a COF (chip on film) is low.
The method for preparing the porous carbon nanosheet by utilizing the two-dimensional covalent organic framework pyrolysis comprises the following steps:
firstly, preparing a polymer: according to the mass ratio of the aldehyde reactant to the amine reactant of 1: (1.2-2), uniformly mixing an aldehyde reactant and an amine reactant, adding the mixture into a mixed solvent formed by mixing N, N-Dimethylformamide (DMF) and N-methylpyrrolidone (NMP), uniformly mixing, heating in an oil bath to 75-90 ℃ under the protection of nitrogen, and keeping reacting for 2-4 days to obtain a polymer; wherein when the aldehyde reactant is terephthalaldehyde, the amine reactant is diaminodiphenyl ether or p-phenylenediamine; when the aldehyde reactant is paraformaldehyde, the amine reactant is diaminodiphenyl ether;
II, annealing: and (3) putting the polymer prepared in the step one into a tube furnace, heating to 700-1000 ℃ in a nitrogen atmosphere, keeping for 2-3 hours, and cooling to obtain the porous carbon nanosheet.
Further, the volume ratio of the N, N-Dimethylformamide (DMF) to the N-methylpyrrolidone (NMP) in the mixed solvent described in the first step is 1: (1-1.5).
Furthermore, the ratio of the total substance amount of the aldehyde reactant and the amine reactant in the step one to the volume of the mixed solvent is 1mmol (1.5-3) mL.
Further, the oil bath described in step one was heated to 85 ℃ to maintain the reaction for 3 days.
Further, as described in step two, the heating was performed to 900 ℃ under a nitrogen atmosphere.
The porous carbon nanosheet product obtained by using terephthalaldehyde or paraformaldehyde as an aldehyde reactant and diaminodiphenyl ether or p-phenylenediamine as an amine reactant through a simple and convenient method after polymerization reaction and annealing treatment has a clearly visible sheet-shaped structure and a specific surface area of 300.847m2g-1～1496.588m2g-1The pore diameter is 3.132 nm-3.713 nm, and the ideal specific surface area and the proper pore diameter provide a good ion diffusion channel for the material and can accelerate the mass transfer process. The specific capacitance of the electrode prepared by utilizing the porous carbon nanosheet reaches 500-630F g-1And the impedance of the electrode is 0.8-2.7 omega, and the impedance is low. The specific capacitance of the symmetrical supercapacitor formed by the porous carbon nanosheet electrode reaches 97.5-165F g-1The rate capability reaches 58.9% -60%, the impedance is 0.8-2.7 omega, the conductivity is good, meanwhile, the porous carbon nano sheet is environment-friendly, pollution is avoided after assembly, and the porous carbon nano sheet can be used in the field of electrochemistry.
Drawings
FIG. 1 is a scanning electron micrograph of COF-900 prepared in example 1;
FIG. 2 is a scanning electron micrograph of the COF-900 prepared in example 1;
FIG. 3 is a scanning electron micrograph of COF-900 prepared in example 1;
FIG. 4 is an IR spectrum of DBEA polymer prepared in step one of example 1 and COF-700, COF-800, COF-900, COF-1000 prepared in step two;
FIG. 5 is a Raman spectrum of COF-700, COF-800, COF-900, COF-1000 prepared in example 1;
FIG. 6 is N of COF-700, COF-800, COF-900, COF-1000 prepared in example 12Adsorption curve diagram;
FIG. 7 is a graph of pore size distribution of COF-700, COF-800, COF-900, COF-1000 prepared in example 1;
FIG. 8 is XPS spectra of DBEA, a polymer prepared in step one of example 1, and COF-700, COF-800, COF-900, and COF-1000 prepared in step two;
FIG. 9 is a high resolution spectrum of N of COF-900;
FIG. 10 Cyclic voltammograms of COF-700, COF-800, COF-900, COF-1000 prepared in example 1;
FIG. 11 is a diagram of constant current charge and discharge of COF-700, COF-800, COF-900, COF-1000;
FIG. 12 is a graph of the AC impedances of COF-700, COF-800, COF-900, and COF-1000;
FIG. 13 is a graph of specific capacitance of COF-700, COF-800, COF-900, COF-1000;
FIG. 14 is a Ragon diagram of a symmetrical supercapacitor assembled with the COF-900 prepared in example 1;
FIG. 15 is a scanning electron micrograph of the COF-900 prepared in example 2;
FIG. 16 is a scanning electron micrograph of the COF-900 prepared in example 3.
Detailed Description
The following examples demonstrate the beneficial effects of the present invention:
example 1: the method for preparing the porous carbon nanosheet by utilizing the two-dimensional covalent organic framework pyrolysis comprises the following steps:
firstly, preparing a polymer: weighing 2.23g (16mmol) of terephthalaldehyde and 2g (10.8mmol) of diaminodiphenyl ether, uniformly mixing, adding the mixture into a mixed solvent formed by mixing 30mL of N, N-Dimethylformamide (DMF) and 30mL of N-methylpyrrolidone (NMP), ultrasonically mixing for 15 minutes, stirring for 15 minutes, heating in an oil bath to 85 ℃ under the protection of nitrogen, keeping the reaction for 3 days, carrying out vacuum filtration, and drying the solid phase at 80 ℃ in vacuum for 12 hours to obtain a polymer DBEA, which is recorded as COF;
II, annealing: and (3) putting the polymer DBEA prepared in the step one into a tube furnace, respectively heating to 700 ℃, 800, 900 and 1000 ℃ in a nitrogen atmosphere, keeping for 2 hours, and cooling to obtain porous carbon nano sheets which are respectively marked as COF-700, COF-800, COF-900 and COF-1000.
As shown in fig. 1, 2 and 3, it can be found from fig. 1, 2 and 3 that the porous carbon nanosheet COF-900 is composed of well-dispersed lamellae, and the more uniformly the lamellae are dispersed at a higher temperature, the larger specific surface area is provided by the dispersed lamellae, which is beneficial to charge transmission, and thus the electrochemical performance of the material is improved.
FIG. 4 is an IR spectrum of DBEA polymer prepared in step one of example 1 and COF-700, COF-800, COF-900, and COF-1000 prepared in step two. As can be seen from figure 4, C ═ N imine bond and C-O single bond are respectively corresponded at 1285 and 1695cm < -1 >, and characteristic peaks are integrated to prove the synthesis of Schiff base organic frameworks. And after the calcination treatment of the second step, the corresponding peak values are weakened or disappeared.
FIG. 5 is the COF-700, COF-800, C prepared in example 1The Raman spectra OF OF-900 and COF-1000 show the I OF COF-700, COF-800, COF-900 and COF-1000 in FIG. 5D/IGReaches 0.856-0.983, and I is increased with the temperatureD/IGThe ratio of (a) to (b) is also increasing, indicating that as the temperature increases, the higher the specific gravity of the carbon defect of the material, the more active centers the material provides, and the more desirable the electrochemical performance.
FIG. 6 is N of COF-700, COF-800, COF-900, COF-1000 prepared in example 12FIG. 7 is a graph showing the distribution of pore diameters of COF-700, COF-800, COF-900 and COF-1000 prepared in example 1. As can be seen from FIGS. 6 and 7, the specific surface areas of the COF-900 and the COF-1000 were 490.8m2g-1And 1496.588m2g-1The material has excellent specific surface area, and the pores are mainly micropores and mesopores, which shows that the material after high-temperature calcination has good ion diffusion channels and a large number of active sites, is favorable for improving the specific capacitance of the electrode material, and further optimizes the electrochemical performance of the material.
FIG. 8 shows XPS spectra of DBEA, a polymer prepared in step one of example 1, and COF-700, COF-800, COF-900, and COF-1000 prepared in step two. FIG. 9 is a high resolution spectrum of N of COF-900. As can be seen from FIGS. 8 and 9, after the calcination treatment, the products at different temperatures showed significant N1sPeaks, in addition, pyridine nitrogen, pyrrole nitrogen, graphite nitrogen and nitrogen oxygen peaks can be seen by analyzing an N fitting peak of DEBA-900, wherein the existence of the pyridine nitrogen and the pyrrole nitrogen is beneficial to improving the ion transmission efficiency of the material, so that the conductivity is improved.
The COF-700, COF-800, COF-900 and COF-1000 prepared in example 1 were placed under a three-electrode system, respectively, to evaluate their electrochemical properties. Wherein, FIG. 10 shows the cyclic voltammetry curves of COF-700, COF-800, COF-900 and COF-1000 prepared in example 1, FIG. 11 shows the constant current charging and discharging curves of COF-700, COF-800, COF-900 and COF-1000, FIG. 12 shows the AC impedance curves of COF-700, COF-800, COF-900 and COF-1000, and FIG. 13 shows the specific capacitance curves of COF-700, COF-800, COF-900 and COF-1000. As can be seen from FIGS. 10, 11, 12, and 13, the specific capacitances of COF-900 and COF-1000 respectively reachTo 590F g-1And 630F g-1The high-performance specific capacitance amplifier has excellent specific capacitance, the multiplying power performance reaches 65% and 50%, the multiplying power performance is good, the resistance is respectively 0.8 omega and 1.2 omega, and the resistance is small. Wherein the COF-1000 shows more ideal specific capacitance, which is related to the large specific surface area of the COF-1000. While COF-900 exhibits better rate capability and conductivity due to reasonable pore size of COF-900 to speed up electron transfer rate.
The functional density and energy density of the COF-900 prepared in example 1 are tested by assembling the symmetrical super capacitor, the Ragon graph is shown in FIG. 14, and as can be seen from FIG. 14, the power density of the symmetrical super capacitor is 522.4W kg-1When the energy density is 22.6Wh kg-1And when the power density is 2.5KW kg-1When the energy density is 20.3Wh kg-1. Indicating that a good energy density can be maintained at very high power densities.
Example 2: the method for preparing the porous carbon nanosheet by utilizing the two-dimensional covalent organic framework pyrolysis comprises the following steps:
firstly, preparing a polymer: weighing 2.23g (16mmol) of terephthalaldehyde and 1.16g (10.8mmol) of p-phenylenediamine, uniformly mixing, adding the mixture into a mixed solvent formed by mixing 30mL of N, N-Dimethylformamide (DMF) and 30mL of N-methylpyrrolidone (NMP), ultrasonically mixing for 15 minutes, stirring for 15 minutes, heating to 85 ℃ in an oil bath under the protection of nitrogen, keeping reacting for 3 days, carrying out vacuum filtration, and carrying out vacuum drying on a solid phase substance at 80 ℃ for 12 hours to obtain a polymer DBDB;
II, annealing: and (3) putting the polymer DBDB prepared in the step one into a tube furnace, respectively heating to 900 ℃ in a nitrogen atmosphere, keeping for 2 hours, and cooling to obtain the porous carbon nanosheet, which is marked as COF-900.
The scanning electron micrograph of the porous carbon nanosheet COF-900 obtained in example 2 is shown in fig. 15. As can be seen from fig. 15, the porous carbon nanosheet COF-900 consists of well-dispersed lamellae. The electrode prepared by utilizing the porous carbon nano sheet COF-900 has the current density of 1Ag-1The specific capacitance under the condition of (2) reaches 220F g-1When the current density rises to 50Ag-1At this time, the specific capacitance of the electrode was maintained at 90F g-1。
Example 3: the method for preparing the porous carbon nanosheet by utilizing the two-dimensional covalent organic framework pyrolysis comprises the following steps:
firstly, preparing a polymer: weighing 1.5g (16mmol) of paraformaldehyde and 2g (10.8mmol) of diaminodiphenyl ether, uniformly mixing, adding into a mixed solvent formed by mixing 30mL of N, N-Dimethylformamide (DMF) and 30mL of N-methylpyrrolidone (NMP), ultrasonically mixing for 15 minutes, stirring for 15 minutes, heating to 85 ℃ in an oil bath under the protection of nitrogen, keeping reacting for 3 days, vacuum filtering, and vacuum drying at 80 ℃ for 12 hours to obtain a polymer DJEA;
II, annealing: and (3) putting the polymer DJEA prepared in the step one into a tube furnace, heating to 900 ℃ in a nitrogen atmosphere, keeping for 2 hours, and cooling to obtain the porous carbon nanosheet, which is marked as COF-900.
The scanning electron micrograph of the porous carbon nanosheet COF-900 obtained in example 3 is shown in fig. 16, and it can be seen from fig. 16 that the porous carbon nanosheet COF-900 is composed of well-dispersed lamellae. The electrode prepared by utilizing the porous carbon nano sheet COF-900 has the current density of 1Ag-1The specific capacitance under the condition of (2) reaches 630F g-1When the current density rises to 50Ag-1While the specific capacitance of the electrode was maintained at 150F g-1。
Claims (5)
1. A method for preparing porous carbon nanosheets by virtue of two-dimensional covalent organic framework pyrolysis is characterized by comprising the following steps:
firstly, preparing a polymer: according to the mass ratio of the aldehyde reactant to the amine reactant of 1: (1.2-2), uniformly mixing an aldehyde reactant and an amine reactant, adding the mixture into a mixed solvent formed by mixing N, N-dimethylformamide and N-methylpyrrolidone, uniformly mixing, heating the mixture to 75-90 ℃ in an oil bath under the protection of nitrogen, and keeping the mixture to react for 2-4 days to obtain a polymer; wherein when the aldehyde reactant is terephthalaldehyde, the amine reactant is diaminodiphenyl ether or p-phenylenediamine; when the aldehyde reactant is paraformaldehyde, the amine reactant is diaminodiphenyl ether;
II, annealing: and (3) putting the polymer prepared in the step one into a tube furnace, heating to 700-1000 ℃ in a nitrogen atmosphere, keeping for 2-3 hours, and cooling to obtain the porous carbon nanosheet.
2. The method for preparing porous carbon nanosheets by virtue of pyrolysis of a two-dimensional covalent organic framework, as recited in claim 1, wherein the volume ratio of N, N-dimethylformamide to N-methylpyrrolidone in the mixed solvent in step one is 1: (1-1.5).
3. The method for preparing porous carbon nanosheets by virtue of two-dimensional covalent organic framework pyrolysis according to claim 1 or 2, wherein the ratio of the total substance amount of the aldehyde reactant and the amine reactant to the volume of the mixed solvent in the first step is 1mmol (1.5-3) mL.
4. The method for preparing porous carbon nanosheets by pyrolysis of a two-dimensional covalent organic framework according to claim 1 or 2, wherein in step one the oil bath is heated to 85 ℃ and left to react for 3 days.
5. The method for preparing porous carbon nanosheets by pyrolysis of a two-dimensional covalent organic framework according to claim 1 or 2, wherein in step two, heating is carried out to 900 ℃ under a nitrogen atmosphere.
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| CN105197925A (en) * | 2015-09-08 | 2015-12-30 | 哈尔滨工业大学 | Preparation method of nitrogen-doped activated carbon and application thereof |
| CN105870470A (en) * | 2016-04-27 | 2016-08-17 | 四川理工学院 | Nitrogen-rich hierarchical pore carbon material and preparation method |
| CN108083261A (en) * | 2018-01-02 | 2018-05-29 | 中国科学院上海硅酸盐研究所 | Three-dimensional porous carbon material, three-dimensional porous nitrating carbon material, its preparation method and application |
| CN110577207A (en) * | 2019-08-01 | 2019-12-17 | 厦门大学 | preparation method of nitrogen and phosphorus co-doped carbon nanosheet |
| CN113013391A (en) * | 2021-02-23 | 2021-06-22 | 北京工业大学 | Method for preparing nitrogen-doped multidimensional and hierarchical porous carbon material adaptive to sulfur anode carrier of aluminum-sulfur battery |
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