CN111463017A - Asphalt alkenyl porous carbon nanosheet for supercapacitor and preparation method thereof - Google Patents
Asphalt alkenyl porous carbon nanosheet for supercapacitor and preparation method thereof Download PDFInfo
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- 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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- 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
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Abstract
The invention belongs to the field of preparation of carbon materials, and particularly relates to an asphalt alkenyl porous carbon nanosheet for a supercapacitor and a preparation method thereof. The method comprises the following steps: (1) extracting, filtering and separating the kerosene coprocessing residue by using a solvent to obtain asphaltene which is rich in condensed rings and has concentrated molecular weight distribution; (2) oxidizing asphaltene by using nitric acid to obtain oxidized asphaltene; (3) and carbonizing the oxidized asphaltene, the melamine and the potassium citrate at high temperature to obtain the asphalt alkenyl porous carbon nanosheet. Compared with the prior art, the method has the advantages of simple process, low cost and excellent performance of the porous carbon nanosheets, and provides a new way for utilizing the kerosene coprocessing residue.
Description
Technical Field
The invention relates to an asphalt alkenyl porous carbon nanosheet for a supercapacitor and a preparation method thereof, and belongs to the field of preparation of carbon materials.
Background
The kerosene coprocessing residue is a solid residue obtained by liquefying and hydrogenating coal and residual oil, which not only contains a condensed aromatic structural unit with 1-6 rings and a hydrogenated aromatic structure partially hydrogenated and saturated, but also contains a series of n-alkanes with different carbon numbers which exist on the aromatic structural unit in a side chain form. According to the invention, most of ash and heteroatoms in the kerosene coprocessing residue can be removed through proper solvent and continuous process method treatment, so that the asphaltene with relatively concentrated molecular weight and adjustable chemical structure is obtained. The asphaltene of the kerosene coprocessing residue has the characteristics of low price, high carbon residue rate and good fluidity, and is a raw material of a high-quality carbon material.
The two-dimensional nano flaky porous carbon material has a large surface-to-volume ratio, a continuous electron transfer channel, is easy to contact with electrolyte, remarkably improves power and energy density, and shows excellent energy density in the aspects of fuel cells and supercapacitors. Furthermore, the introduction of heteroatoms in the material can improve the capacitance, surface wettability and conductivity of the material. And the surface is easy to modify, so that the two-dimensional nano porous carbon material is an important precursor for preparing a novel nano composite material or a hybrid material. At present, when asphalt is used as a raw material to prepare a nano flaky porous carbon material, the nano flaky porous carbon material is synthesized by a hard template method or a molten salt method. The process of preparing the carbon nano-sheet by the template method is complex, the template is required to be synthesized in the early stage, and a large amount of acid washing and water washing are required to remove the template in the later stage; when the molten salt method is used for preparing the carbon nano-sheets, the composite salt with high proportion is needed.
Disclosure of Invention
The preparation process is complicated, the production cost is high, and the preparation method is not suitable for large-scale preparation and application of the porous carbon nanosheet.
According to the invention, the nitrogen atom-doped asphalt-based porous carbon nanosheet is prepared by one-step direct carbonization by using cheap kerosene coprocessing residues as a carbon source, melamine as a nitrogen source and potassium citrate as a template agent and an activating agent.
In order to achieve the purpose, the invention adopts the following technical scheme:
super capacitorThe specific surface area of the asphalt alkenyl porous carbon nanosheet is more than or equal to 2350m2G, pore volume is more than or equal to 1.12cm3(ii)/g; when the current density is 1A/g, the specific capacitance is more than or equal to 270F/g; under the condition of high current density of 50A/g, the multiplying power performance is more than or equal to 82.2 percent. The porous carbon nanosheet with a developed microporous structure and high nitrogen content is synthesized by the method. The developed pore structure improves the double electric layer capacitance of the material and provides a continuous migration channel for electrons; the surface wettability/conductivity of the material is increased by doping of N atoms, and additional pseudo capacitance is contributed; the lamellar structure is beneficial to the rapid diffusion of the electrolyte, thereby obviously improving the power and the energy density. Therefore, the material exhibits excellent electrochemical properties.
The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor comprises the following steps:
step 1, extracting, filtering and separating the kerosene coprocessing residue by using a solvent to obtain asphaltene which is rich in condensed rings and has concentrated molecular weight distribution;
step 2, oxidizing the asphaltene by nitric acid to obtain oxidized asphaltene;
and 3, carbonizing the oxidized asphaltene, the melamine and the potassium citrate at high temperature to obtain the asphalt alkenyl porous carbon nanosheet. The method realizes the preparation of the heteroatom-doped asphalt-based porous carbon nanosheet by one-step direct carbonization, and can simply and effectively control the morphology, surface chemistry and pore structure of the carbon nanosheet.
Further, the coal-oil co-processing residue in the step 1 is solid residue obtained by hydrogenation or non-hydrogenation reaction of coal and residual oil at 300-500 ℃ and 1-25 MPa, and the ash content of the solid residue is high, so that the solid residue is low in combustion power generation efficiency and is usually used as solid waste. However, asphaltene containing polycyclic fused aromatic hydrocarbons and alkyl substituent components thereof in kerosene coprocessing residues is suitable as a precursor for preparing carbon materials because of its high aromaticity and carbon content, easy polymerization or crosslinking, high carbon formation rate and easy graphitization.
Further, in the step 1, the molecular weight distribution of the asphaltene is mainly concentrated at 250-800, the structure of a reaction product is easier to directionally regulate, the content of the asphaltene is 5-50%, and the ash content is below 30%.
Further, in the step 2, the asphaltene is oxidized by nitric acid to obtain oxidized asphaltene, which specifically comprises:
mixing asphaltene and nitric acid in a container, heating and stirring at 80 deg.C for 12h to completely oxidize asphaltene into oxidized asphaltene, repeatedly washing with deionized water to neutrality, and oven drying to obtain oxidized asphaltene. In the process, nitric acid and asphaltene generate polymerization reaction, so that a large amount of oxygen-containing and nitrogen-containing functional groups are loaded on the surface of the oxidized asphaltene, the pyrolysis temperature of the asphaltene is improved, the carbon residue rate is improved, and the yield of the product is increased.
Further, the weight ratio of the asphaltene to the nitric acid is 1: 5-1: 10, and the asphaltene can be completely oxidized into the oxidized asphaltene with the use of the oxidant as little as possible.
Further, in the step 3, the oxidized asphaltene, the melamine and the potassium citrate are carbonized at high temperature to obtain the asphaltene-based porous carbon nanosheet, which specifically comprises the following steps:
fully grinding and uniformly mixing oxidized asphaltene, melamine and potassium citrate, then placing the mixture in a muffle furnace, gradually heating to 850-1000 ℃ in a nitrogen atmosphere, carbonizing at a constant temperature for 1-3 h, washing the carbonized mixture to be neutral by 1 mol/L hydrochloric acid and deionized water in sequence, and drying to obtain the asphalt alkenyl porous carbon nanosheet2CO3Particles covering and embedded on the surface of the carbon matrix asphaltene oxide to form an interconnected lamellar network structure, and K is increased with the temperature2CO3CO produced by further decomposition2、K2The O and potassium vapors further etch the carbon matrix, forming a large number of pore structures. In the method, the potassium citrate not only contributes to the formation of the sheet layer, but also plays the role of an activating agent.
Further, the weight ratio of the oxidized asphaltene to the melamine to the potassium citrate is 1:1: 1-1: 3: 9. The specific surface area, the pore structure and the nitrogen content of the asphalt alkenyl carbon nanosheet are changed by adjusting the use amounts of the carbon source, the nitrogen source and the potassium citrate, and then the influence of the performance of the asphalt alkenyl carbon nanosheet is inspected.
Further, the heating rate is 5-10 ℃/min, and potassium citrate can be decomposed to generate a large amount of potassium steam at the temperature of more than 830 ℃, so that the carbonization temperature is 850-1000 ℃, and the retention time is 1-3 h.
Further, the residue of the coal-oil co-treatment in the step 1 is extracted, filtered and separated by a solvent, and specifically comprises the following steps: the extraction solvent is tetrahydrofuran, the weight ratio of the kerosene coprocessing residue to the extraction solvent is 1: 4-1: 10, the extraction temperature is 25-150 ℃, the extraction time is 2-12 hours, effective components in the residue are extracted as much as possible to improve the yield, and large particle components which are not beneficial to reaction control are completely removed by filtering through a filter screen with more than 1000 meshes.
The evaluation standard of the asphalt alkenyl porous carbon nanosheet for the supercapacitor is as follows: mixing asphalt alkenyl porous carbon nano-sheets ACN with polytetrafluoroethylene and carbon black at a ratio of 85:5:10(w/w), uniformly coating the mixture on 1cm x 1cm of foamed nickel (about 4mg), tabletting, drying, soaking in 6M KOH solution for 12h, and measuring the electrochemical performance of the three-electrode system.
Compared with the prior art, the invention has the following advantages:
the method for preparing the nitrogen atom-doped asphalt-based porous carbon nanosheet by one-step direct carbonization has the advantages of simple preparation method, low equipment requirement and easiness in industrialization; the prepared material has the advantages of developed pore structure and high specific surface area. The material is applied to a three-electrode system, shows excellent electrochemical performance, and is a super capacitor electrode material with wide application prospect.
Drawings
Fig. 1 is an SEM image of an asphalt-based porous carbon nanosheet prepared according to the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by way of examples below.
Example 1
The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor comprises the following steps:
step 1, uniformly mixing 100g of kerosene coprocessing residues (45 ten thousand tons of extended petroleum group/year kerosene coprocessing residues) and 400g of tetrahydrofuran at room temperature, extracting at 25 ℃ for 12 hours, separating, filtering by a filter screen with more than 1000 meshes, and recovering a solvent to obtain asphaltene which has a softening point of 78 ℃, is ash-free, is rich in condensed rings and has a molecular weight distribution of 300-600, wherein the yield of the asphaltene is 43%.
Step 2, mixing 10g of asphaltene and nitric acid in a round-bottom flask according to the weight-to-weight ratio of 1:5, heating and stirring at 80 ℃ for 12h, repeatedly washing with deionized water to neutrality, and drying to obtain 14g of asphaltene oxide;
step 3, sufficiently grinding and uniformly mixing the oxidized asphaltene, the melamine and the potassium citrate according to the ratio of 1:1:1, then placing the mixture in a muffle furnace, heating the mixture to 850 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere, carbonizing the mixture at the constant temperature for 1h, washing the carbonized sample by 1 mol/L hydrochloric acid and deionized water in sequence to be neutral, and drying the product to obtain the asphalt alkenyl porous carbon nanosheet, wherein the specific surface area of the asphalt alkenyl porous carbon nanosheet is 2400m2G, pore volume of 1.15cm3/g。
Mixing the asphalt alkenyl carbon nanosheet with polytetrafluoroethylene and carbon black at a ratio of 85:5:10(w/w), uniformly coating the mixture on 1cm x 1cm of foamed nickel (about 4mg), tabletting, drying, soaking in 6M KOH solution for 12h, and measuring the electrochemical performance of the three-electrode system. When the current density is 1A/g, the specific capacitance reaches 272F/g, and under the condition of high current density of 50A/g, the specific capacitance still has high specific capacitance of 230F/g, and the multiplying power performance reaches 84.6% (based on 1A/g-272F/g).
Example 2
The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor comprises the following steps:
step 1, uniformly mixing 100g of kerosene coprocessing residues (45 ten thousand tons of extended petroleum group/year kerosene coprocessing residues) and 600g of tetrahydrofuran at room temperature, extracting at 50 ℃ for 8 hours, separating, filtering by a filter screen with more than 1000 meshes, and recovering a solvent to obtain asphaltene which has a softening point of 76 ℃, is ash-free, is rich in condensed rings and has a molecular weight distribution of 280-650, wherein the yield of the asphaltene is 44%.
Step 2, mixing 10g of asphaltene and nitric acid in a round-bottom flask according to the weight-to-weight ratio of 1:7, heating and stirring at 80 ℃ for 12h, repeatedly washing with deionized water to neutrality, and drying to obtain 14g of asphaltene oxide;
step 3, sufficiently grinding and uniformly mixing the oxidized asphaltene, the melamine and the potassium citrate according to the ratio of 1:2:4, then placing the mixture in a muffle furnace, heating the mixture to 900 ℃ at the heating rate of 7 ℃/min under the nitrogen atmosphere, carbonizing the mixture at the constant temperature for 2h, washing the carbonized sample by 1 mol/L hydrochloric acid and deionized water in sequence to be neutral, and drying the product to obtain the asphaltene-based porous carbon nanosheet, wherein the specific surface area of the asphaltene-based porous carbon nanosheet is 2350m2G, pore volume of 1.12cm3/g。
Mixing asphalt alkenyl carbon nanosheets ACN with polytetrafluoroethylene and carbon black at a ratio of 85:5:10(w/w), uniformly coating the mixture on 1cm x 1cm of foamed nickel (about 4mg), tabletting, drying, soaking in 6M KOH solution for 12h, and measuring the electrochemical performance of the three-electrode system. When the current density is 1A/g, the specific capacitance reaches 270F/g, and under the condition of high current density of 50A/g, the specific capacitance still has high specific capacitance of 222F/g, and the multiplying power performance reaches 82.2% (based on 1A/g-237F/g).
Example 3
The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor comprises the following steps:
step 1, uniformly mixing 100g of kerosene coprocessing residues (45 ten thousand tons of extended petroleum group/year kerosene coprocessing residues) and 800g of tetrahydrofuran at room temperature, extracting at 100 ℃ for 4 hours, separating, filtering by a filter screen with more than 1000 meshes, and recovering a solvent to obtain asphaltene which has a softening point of 74 ℃, is ash-free, is rich in condensed rings and has a molecular weight distribution of 260-750, wherein the yield of the asphaltene is 46%.
Step 2, mixing 10g of asphaltene and nitric acid in a round-bottom flask according to the weight ratio of 1:8, heating and stirring at 80 ℃ for 12h, repeatedly washing with deionized water to neutrality, and drying to obtain 14.1g of oxidized asphaltene;
step 3, sufficiently grinding and uniformly mixing the oxidized asphaltene, the melamine and the potassium citrate according to the ratio of 1:3:5, then placing the mixture in a muffle furnace, then heating the mixture to 950 ℃ at the heating rate of 8 ℃/min under the nitrogen atmosphere, carbonizing the mixture at the constant temperature for 1.5h, washing the carbonized sample with 1 mol/L hydrochloric acid and deionized water in sequence to be neutral, drying and dryingThen obtaining the asphalt alkenyl porous carbon nano sheet with the specific surface area of 2420m2G, pore volume of 1.16cm3/g。
Mixing asphalt alkenyl carbon porous nano-sheets ACN with polytetrafluoroethylene and carbon black at a ratio of 85:5:10(w/w), uniformly coating the mixture on 1cm x 1cm of foamed nickel (about 4mg), tabletting, drying, soaking in 6M KOH solution for 12h, and measuring the electrochemical performance of the three-electrode system. When the current density is 1A/g, the specific capacitance reaches 274F/g, and under the condition of high current density of 50A/g, the specific capacitance still has high 231F/g, and the multiplying power performance reaches 84.3% (based on 1A/g-259F/g).
Example 4
The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor comprises the following steps:
step 1, uniformly mixing 100g of kerosene coprocessing residues (45 ten thousand tons of extended petroleum group/year kerosene coprocessing residues) and 1000g of tetrahydrofuran at room temperature, extracting at 150 ℃ for 2 hours, separating, filtering by a filter screen with more than 1000 meshes, and recovering a solvent to obtain asphaltene which has a softening point of 72 ℃, is ash-free, is rich in condensed rings and has a molecular weight distribution of 250-800, wherein the yield of the asphaltene is 48%.
Step 2, mixing 10g of asphaltene and nitric acid in a round-bottom flask according to the weight ratio of 1:10, heating and stirring at 80 ℃ for 12h, repeatedly washing with deionized water to neutrality, and drying to obtain 14.2g of oxidized asphaltene;
step 3, sufficiently grinding and uniformly mixing the oxidized asphaltene, the melamine and the potassium citrate according to the ratio of 1:3:9, then placing the mixture in a muffle furnace, heating the mixture to 1000 ℃ at the heating rate of 10 ℃/min under the nitrogen atmosphere, carbonizing the mixture at the constant temperature for 3h, washing the carbonized sample by 1 mol/L hydrochloric acid and deionized water in sequence to be neutral, and drying the product to obtain the asphaltene-based porous carbon nanosheet, wherein the specific surface area of the asphaltene-based porous carbon nanosheet is 2432m2G, pore volume of 1.16cm3/g。
Mixing asphalt alkenyl porous carbon nano-sheets ACN with polytetrafluoroethylene and carbon black at a ratio of 85:5:10(w/w), uniformly coating the mixture on 1cm x 1cm of foamed nickel (about 4mg), tabletting, drying, soaking in 6M KOH solution for 12h, and measuring the electrochemical performance of the three-electrode system. When the current density is 1A/g, the specific capacitance reaches 278F/g, and under the condition of high current density of 50A/g, the specific capacitance still has high 237F/g, and the multiplying power performance reaches 85.3% (based on 1A/g-274F/g).
Fig. 1 is an SEM image of the asphalt alkenyl porous carbon nanosheet prepared by the present invention, and it can be known from the SEM image that the asphalt alkenyl porous carbon nanosheet prepared by the present invention is a sheet-like material with good uniformity.
In the four embodiments, the kerosene coprocessing residue is solid residue obtained by hydrogenation or non-hydrogenation reaction of coal and residual oil at 300-500 ℃ and 1-25 MPa.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. Asphalt alkenyl porous carbon nano-sheet for super capacitor, its characterized in that: the specific surface area of the asphalt alkenyl porous carbon nanosheet is more than or equal to 2350m2G, pore volume is more than or equal to 1.12cm3(ii)/g; when the current density is 1A/g, the specific capacitance is more than or equal to 270F/g; under the condition of high current density of 50A/g, the multiplying power performance is more than or equal to 82.2 percent.
2. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor is characterized by comprising the following steps of: the method comprises the following steps:
step 1, extracting, filtering and separating the kerosene coprocessing residue by using a solvent to obtain asphaltene which is rich in condensed rings and has concentrated molecular weight distribution;
step 2, oxidizing the asphaltene by nitric acid to obtain oxidized asphaltene;
and 3, carbonizing the oxidized asphaltene, the melamine and the potassium citrate at high temperature to obtain the asphalt alkenyl porous carbon nanosheet.
3. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 2, wherein: the coal-oil co-processing residue in the step 1 is solid residue obtained by hydrogenation or non-hydrogenation reaction of coal and residual oil at 300-500 ℃ and 1-25 MPa.
4. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 2, wherein: in the step 1, the molecular weight distribution of the asphaltene is 250-800, the content of the asphaltene is 5% -50%, and the ash content is below 30%.
5. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 2, wherein: in the step 2, the asphaltene is oxidized by nitric acid to obtain oxidized asphaltene, which specifically comprises the following steps:
mixing asphaltene and nitric acid in a container, heating and stirring at 80 ℃ for 12h, repeatedly washing with deionized water to neutrality, and drying to obtain asphaltene oxide.
6. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 2, wherein: in the step 3, the oxidized asphaltene, the melamine and the potassium citrate are carbonized at high temperature to obtain the asphaltene-based porous carbon nanosheet, which specifically comprises the following steps:
fully grinding and uniformly mixing the oxidized asphaltene, the melamine and the potassium citrate, then placing the mixture in a muffle furnace, gradually heating to 850-1000 ℃ under the nitrogen atmosphere, carbonizing at a constant temperature for 1-3 h, washing the carbonized mixture to be neutral by 1 mol/L hydrochloric acid and deionized water in sequence, and drying to obtain the asphaltene-based porous carbon nanosheet.
7. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 5, wherein: the weight ratio of the asphaltene to the nitric acid is 1: 5-1: 10.
8. The preparation method of the asphalt alkenyl porous carbon nanosheet for the supercapacitor according to claim 6, wherein: the weight ratio of the oxidized asphaltene to the melamine to the potassium citrate is 1:1: 1-1: 3: 9.
9. The preparation method of the porous carbon nanosheet for the supercapacitor according to claim 6, wherein: the heating rate is 5-10 ℃/min, the carbonization temperature is 850-1000 ℃, and the retention time is 1-3 h.
10. The preparation method of the porous carbon nanosheet for the supercapacitor according to claim 2, wherein: the residue of the coal-oil co-treatment in the step 1 is extracted, filtered and separated by a solvent, and specifically comprises the following steps: the extraction solvent is tetrahydrofuran, the weight ratio of the kerosene coprocessing residue to the extraction solvent is 1: 4-1: 10, the extraction temperature is 25-150 ℃, the extraction time is 2-12 h, and the extraction solvent is filtered by a filter screen with more than 1000 meshes.
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| CN114275777A (en) * | 2021-12-28 | 2022-04-05 | 盐城工学院 | Preparation method of high-graphitization-degree carbon-based material for lithium battery negative electrode |
| CN115228398A (en) * | 2022-06-28 | 2022-10-25 | 同方工业有限公司 | Continuous extraction preparation method and device of coal-based organic micro-nano spheres |
| CN115228398B (en) * | 2022-06-28 | 2023-09-26 | 同方工业有限公司 | Continuous extraction preparation method and device for coal-based organic micro-nanospheres |
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