CN110364370B - Pyridyl porous carbon material and preparation method and application thereof - Google Patents
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 43
- 125000004076 pyridyl group Chemical group 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000013317 conjugated microporous polymer Substances 0.000 claims abstract description 11
- HSOAIPRTHLEQFI-UHFFFAOYSA-N 1-(3,5-diacetylphenyl)ethanone Chemical compound CC(=O)C1=CC(C(C)=O)=CC(C(C)=O)=C1 HSOAIPRTHLEQFI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000003934 aromatic aldehydes Chemical class 0.000 claims abstract description 9
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 7
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 7
- 230000002378 acidificating effect Effects 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 11
- 238000000197 pyrolysis Methods 0.000 claims description 11
- 239000003990 capacitor Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- 238000007363 ring formation reaction Methods 0.000 claims description 7
- 150000001299 aldehydes Chemical class 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical group O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 20
- 229910052799 carbon Inorganic materials 0.000 description 20
- 239000011148 porous material Substances 0.000 description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000001179 sorption measurement Methods 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 9
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 8
- 238000002336 sorption--desorption measurement Methods 0.000 description 6
- 238000012983 electrochemical energy storage Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZDRMMTYSQSIGRY-UHFFFAOYSA-N 1,3,5-triethynylbenzene Chemical compound C#CC1=CC(C#C)=CC(C#C)=C1 ZDRMMTYSQSIGRY-UHFFFAOYSA-N 0.000 description 1
- LFMWZTSOMGDDJU-UHFFFAOYSA-N 1,4-diiodobenzene Chemical compound IC1=CC=C(I)C=C1 LFMWZTSOMGDDJU-UHFFFAOYSA-N 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention relates to a pyridyl porous carbon material and a preparation method and application thereof. The preparation method comprises the following steps: mixing 1,3, 5-triacetyl benzene, aromatic aldehyde and ammonium acetate, reacting under an acidic condition, washing, filtering, drying in vacuum, and pyrolyzing the obtained pyridyl conjugated microporous polymer. The method is simple to operate, large-scale preparation can be realized, and the obtained pyridyl porous carbon material mainly takes micropores and has potential application value in the aspect of supercapacitors.
Description
Technical Field
The invention belongs to the field of porous carbon materials and preparation and application thereof, and particularly relates to a pyridyl porous carbon material and a preparation method and application thereof.
Background
The super capacitor is used as a novel electrochemical energy storage device, is between a traditional capacitor and a rechargeable battery, has the advantages of high charging and discharging speed, simple preparation, environmental protection and the like, and becomes an energy device which is widely applied. The energy storage mechanism can be divided into an electric double layer capacitor and a pseudo capacitor, and the electric double layer capacitor and the pseudo capacitor respectively store charges through an electric double layer structure and a redox reaction.
The porous carbon material is a carbon material with different pore structures, has the characteristics of large specific surface area, heat and electricity conduction, high thermal stability and chemical stability and the like, and has important application in a super capacitor as an electrode material. However, the pores with different pore diameters have different effects on electrochemical transmission, so that the specific capacitance of most porous carbon materials is not ideal. It is reported in the literature that micropores, especially ultramicropores, contribute significantly better to electrochemical energy storage than other pores. The conjugated microporous polymer is used as a precursor, so that the porous carbon material with more micropores can be obtained, nitrogen atoms are easily introduced, the pseudo capacitance is increased, and the specific capacitance of the carbon material is favorably improved. However, most of the current conjugated microporous polymers are complex to synthesize, and large-scale synthesis is difficult to realize. For example, Jiang et al synthesized CMP-1 and CMP-1-NH2 using a Pd-catalyzed Sonogashira-Hagohara coupling method, and carbonized these two conjugated microporous polymers as precursors in an atmosphere of N2 or NH3 to obtain different porous carbon Materials (Journal of Materials Chemistry A,2016,4, 7665).
Disclosure of Invention
The invention aims to solve the technical problem of providing a pyridyl porous carbon material, a preparation method and application thereof, so as to overcome the defect of poor specific capacitance of the carbon material in the prior art.
The invention provides a preparation method of a pyridyl porous carbon material, which comprises the following steps:
mixing 1,3, 5-triacetylbenzene, aromatic aldehyde and ammonium acetate, carrying out amine cyclization reaction under an acidic condition, washing, carrying out suction filtration and vacuum drying to obtain a pyridyl conjugated microporous polymer, and then carrying out pyrolysis to obtain the pyridyl porous carbon material, wherein the molar ratio of the aromatic aldehyde containing carbonyl to the 1,3, 5-triacetylbenzene is 1:2-2.2, and the molar ratio of the sum of the ammonium acetate, the 1,3, 5-triacetylbenzene and the aromatic aldehyde containing carbonyl is 5: 1-20: 1.
The aromatic aldehyde is terephthalaldehyde or trimesic aldehyde.
The acidic condition is under acetic acid condition.
The amine cyclization reaction temperature is 110-120 ℃, and the amine cyclization reaction time is 8-12 h.
The washing is as follows: firstly, washing with an alkali solution at room temperature, and then sequentially washing with deionized water and an organic solvent at 55-65 ℃ for 20-26 h.
The alkali solution is 1mol/L ammonia water.
The organic solvent is methanol.
The vacuum drying temperature is 60-80 ℃, and the vacuum drying time is 20-24 h.
The pyrolysis process parameters are as follows: the pyrolysis temperature is 800-1100 ℃ under the argon atmosphere, the pyrolysis time is 1h, and the heating rate is 5 ℃/min.
The invention also provides the pyridyl porous carbon material prepared by the method.
The invention also provides application of the pyridyl porous carbon material prepared by the method in a super capacitor.
Advantageous effects
(1) The invention adopts Chihchibabin amine cyclization reaction principle, does not use pyridyl derivatives as raw materials, can synthesize a large amount of pyridyl conjugated microporous polymers under mild conditions, and further pyrolyzes to obtain the pyridyl porous carbon material. The reaction operation is simple, the large-scale preparation can be realized, and the obtained pyridyl porous carbon material is mainly microporous.
(2) The synthesized pyridyl porous carbon material has potential application value in the aspect of super capacitors as an electrode material.
Drawings
FIG. 1 shows N at 77.4K of the pyridyl-based porous carbon material synthesized in example 12Adsorption-desorption curve of (a);
FIG. 2 is a pore size distribution curve of the pyridyl-based porous carbon material-1 synthesized in example 1 at 77.4K using NLDFT as a calculation method;
FIG. 3 shows the pyridine-based porous carbon material synthesized in example 1, namely, 1 in a three-electrode system and 0.5M H2SO4CV curve in electrolyte;
FIG. 4 shows the pyridine-based porous carbon material synthesized in example 1, namely, 1 in a three-electrode system and 0.5M H2SO4GCD profile in electrolyte;
FIG. 5 shows N at 77.4K of the pyridyl-based porous carbon material synthesized in example 22Adsorption-desorption curve of (a);
FIG. 6 is a pore size distribution curve of the pyridyl-based porous carbon material-1 synthesized in example 1 at 77.4K using NLDFT as a calculation method;
FIG. 7 shows the pyridine-based porous carbon material synthesized in example 2, in a three-electrode system and 0.5M H2SO4CV curve in electrolyte;
FIG. 8 shows the pyridine-based porous carbon material synthesized in example 2, in a three-electrode system and 0.5M H2SO4GCD profile in electrolyte.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Trimesic aldehyde (Shanghai Bide pharmaceutical science and technology Co., Ltd.), p-benzaldehyde, 1,3, 5-triacetylbenzene (Chishieiyi chemical industry development Co., Ltd.), ammonium acetate (national chemical reagent Co., Ltd.), glacial acetic acid (Shanghai Lingfeng chemical reagent Co., Ltd.)
Example 1
Terephthalaldehyde (134.1mg, 1mmol) and 1,3, 5-triacetylbenzene (408.4mg, 2mmol) were mixed and placed in a 100ml round bottom flask, ammonium acetate (2.31g, 30mmol) was added, then 60ml acetic acid was added to dissolve the above mixed powder completely, and finally the mixture was put in a 120 ℃ oil bath and stirred for reaction for 8 hours. And after the reaction is finished, performing suction filtration, firstly stirring and washing for 24 hours at room temperature by using 1mol/L ammonia water, then washing for 24 hours at 60 ℃ by using deionized water and anhydrous methanol respectively, and after the suction filtration, placing in a vacuum oven at 60 ℃ for drying for 24 hours to obtain the pyridyl-containing conjugated microporous polymer. Then, heating the obtained pyridyl conjugated microporous polymer to 1000 ℃ at a heating rate of 5 ℃/min under an argon atmosphere for pyrolysis for 1h, and cooling to room temperature to obtain a pyridyl porous carbon material, namely a carbon material-1, wherein the BET specific surface area of the pyridyl conjugated microporous polymer is 1232m2/g。
The pore size distribution curve of the carbon material-1 obtained in this example at 77.4K by NLDFT is shown in fig. 2, and it is understood that the pore volumes are all contributed by pores having a pore diameter of 2nm or less, and there is substantially no significant fluctuation in pore volume at 2nm or more, which proves that the pores of the carbon material-1 are mainly micropores and a certain amount of ultramicropores exist.
The carbon material-1 obtained in this example was in a three-electrode system and 0.5M H2SO4As shown in FIG. 3, the CV curves in the electrolyte showed different scanning rates (5mV s)-1，10mV s-1，20mV s-1，50mV s-1) An obvious redox peak exists at 0.4-0.5V, which proves that pyridyl exists; as the scan rate increased, the CV curve shifted significantly to the right, as did the redox peaks, again demonstrating the stable presence of pyridine nitrogen in carbon material-1.
The carbon material-1 obtained in this example was in a three-electrode system and 0.5M H2SO4The GCD curve in the electrolyte is shown in figure 4, and the specific capacitance of the carbon material-1 at the current density of 0.1A/g is 297.5F/g which is better than that of the common porous carbon material (the common porous carbon material at the current density of 0.1A/g does not exceed 250F/g), so that the introduction of the pyridyl and the increase of the micropore volume are beneficial to improving the electrochemical energy storage of the carbon material. The specific capacitances at current densities of 0.2, 0.5, 1, 2, 5, 10A/g were 262.2, 233.5, 212.7, 197.6, 177, 157.7F/g, respectively.
Example 2
The procedure of example 1 was repeated except for changing "terephthalaldehyde (134.1mg, 1 mmol)" into "trimesic aldehyde (162.1mg, 1 mmol)" and the like to obtain a pyridyl-based porous carbon material having a BET specific surface area of 1056m, designated as carbon material-2, according to example 12/g。
The pore size distribution curve of the carbon material-2 obtained in this example at 77.4K by using NLDFT as a calculation method is shown in fig. 6, and it is understood that the pore volumes are all contributed by pores having a pore diameter of 2nm or less, and that there is substantially no significant fluctuation in pore volume at 2nm or more, which proves that the pores of the carbon material-2 are mainly micropores and a large amount of ultramicropores exist.
The carbon material-2 obtained in this example was in a three-electrode system and 0.5M H2SO4As shown in FIG. 7, the CV curves in the electrolyte showed different scanning rates (5mV s)-1，10mV s-1，20mV s-1，50mV s-1) An obvious redox peak exists at 0.4-0.5V, which proves that pyridyl exists; as the scan rate increased, the CV curve shifted significantly to the right, as did the redox peaks, again demonstrating the stable presence of pyridine nitrogen in carbon material-2.
The carbon material-2 obtained in this example was in a three-electrode system and 0.5M H2SO4The GCD curve in the electrolyte is shown in FIG. 8, and the specific capacitance of the carbon material-2 is 324F/g under the current density of 0.1A/g, which is obviously superior to that of the common porous carbon material, so that the introduction of the pyridyl and the increase of the micropore volume are beneficial to improving the electrochemical energy storage of the carbon material. The specific capacitance at current densities of 0.2, 0.5, 1, 2, 5, 10A/g were 282, 239.5, 226, 212.6, 196, 182.4F/g, respectively.
Comparative example 1
1,3, 5-Triethynylbenzene (300mg,2.0mmol), 1, 4-diiodobenzene (660mg,2.0mmol), tetrakis (triphenylphosphine) palladium (100mg) and copper iodide (30mg) were dissolved in a mixture of toluene (2.5mL) and triethylamine (2.5mL), heated to 80 ℃ under a nitrogen atmosphere and stirred for 72 h. Cooling the mixture to room temperature, filtering, sequentially washing with chloroform, water, methanol and acetone, performing Soxhlet extraction with methanol as solvent for 48 hr, vacuum filtering, and collecting the productVacuum drying at 70 deg.c for 24 hr to obtain the conjugated microporous polymer CMP-1. And then heating the CMP-1 to 800 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere for pyrolysis for 2h, and cooling to room temperature to obtain the porous carbon material C1-CMP-1. Then in NH3Heating the C1-CMP-1 to 800 ℃ at the heating rate of 5 ℃/min under the atmosphere for pyrolysis for 2h to obtain the nitrogen-containing porous carbon material N3-CMP-1, wherein the BET specific surface area of the nitrogen-containing porous carbon material N3-CMP-1 is 1436m2(ii) in terms of/g. In a three-electrode system and 1M H2SO4The specific capacitance of the electrolyte measured by using N3-CMP-1 as an electrode material at a current density of 0.1A/g is 175.3F/g.
Claims (7)
1. A preparation method of a pyridyl porous carbon material comprises the following steps:
mixing 1,3, 5-triacetylbenzene, aromatic aldehyde and ammonium acetate, carrying out amine cyclization reaction under an acidic condition, washing, carrying out suction filtration and vacuum drying to obtain a pyridyl conjugated microporous polymer, and then carrying out pyrolysis to obtain the pyridyl porous carbon material, wherein the molar ratio of the aromatic aldehyde to the 1,3, 5-triacetylbenzene is 1:2-2.2, the molar ratio of the ammonium acetate to the sum of the 1,3, 5-triacetylbenzene and the aromatic aldehyde containing carbonyl is 5: 1-20: 1, and the aromatic aldehyde is terephthalaldehyde or trimesic aldehyde.
2. The method of claim 1, wherein the acidic conditions are under acetic acid conditions.
3. The method according to claim 1, wherein the amine cyclization reaction temperature is 110-120 ℃ and the amine cyclization reaction time is 8-12 h.
4. The method of claim 1, wherein the washing is: firstly, washing with an alkali solution at room temperature, and then sequentially washing with deionized water and an organic solvent at 55-65 ℃ for 20-26 h.
5. The method of claim 1, wherein the pyrolysis process parameters are: the pyrolysis temperature is 800-1100 ℃ under the argon atmosphere, the pyrolysis time is 1h, and the heating rate is 5 ℃/min.
6. A pyridyl porous carbon material prepared by the method of claim 1.
7. The application of the pyridyl porous carbon material prepared by the method in claim 1 in a super capacitor.
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| CN107871615A (en) * | 2016-09-27 | 2018-04-03 | 国家纳米科学中心 | A kind of porous carbon nanomaterial and its production and use |
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| CN104177576A (en) * | 2014-08-12 | 2014-12-03 | 吉林大学 | Imino organic porous polymer framework material and preparation method thereof |
| CN104495791A (en) * | 2015-01-06 | 2015-04-08 | 日照格鲁博新材料科技有限公司 | Preparation method of porous carbon |
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| Title |
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| "Acetic acid-ammonium acetate reactions. An improved chichibabin pyridine synthesis";Weiss M;《Journal of the American Chemical Society》;19521231;第74卷;第200-202页 * |
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