CN114212790A - Preparation method of nitrogen-doped porous biochar and method for preparing electrode material - Google Patents
Preparation method of nitrogen-doped porous biochar and method for preparing electrode material Download PDFInfo
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to the technical field of capacitor electrode production, in particular to a preparation method of nitrogen-doped porous biochar and a method for preparing an electrode material, which comprises the following steps: (1) pretreatment of raw materials: mixing and pretreating algae biomass and terrestrial biomass; (2) adding an activating agent: mixing the pretreated raw materials with an activating agent; (3) carbonization and acid washing: and (3) carbonizing the mixture obtained in the step (2) under the protection of inert gas, carrying out acid washing on the obtained biochar to be neutral after the reaction is finished, and drying to obtain the nitrogen-doped porous biochar.
Description
Technical Field
The invention relates to the technical field of capacitor electrode production, in particular to a preparation method of nitrogen-doped porous biochar and a method for preparing an electrode material.
Background
Along with the development and the utilization of new energy technology, the storage problem of the energy also arouses people's attention gradually, develops novel energy storage device and can solve the unstable problem of the energy for the energy is exported with high efficiency, stable form, thereby satisfies people's ever-increasing energy demand. The super capacitor is a novel energy storage component and is closely concerned by the majority of scientific researchers. The biomass-derived carbon material (hereinafter referred to as biochar) is a carbon material with a unique pore structure, and has the advantages of developed pore structure, large specific surface area, good conductivity, high temperature resistance, corrosion resistance and the like. Compared with mesoporous carbon, graphene, carbon nanotubes, graphene-like low-dimensional carbon materials and the like, the biological carbon has a three-dimensional interpenetrating pore structure, is rich in source, low in preparation cost, green, environment-friendly and sustainable. In recent years, biochar has important application in the field of supercapacitors due to its advantages of unique physicochemical properties, complex microstructures, abundant surface functional groups, good stability and the like. The conversion of biomass into a high value-added biological carbon material is one of the important means for realizing the high-value utilization of biomass.
At present, the preparation methods of nitrogen-doped porous carbon are various, and patent CN201610132400.7 discloses a method for preparing nitrogen-doped porous carbon material by using jujube kernel, which specifically comprises pre-carbonizing jujube shell in mixed gas composed of inert gas, ammonia gas and carbon dioxide, and further adding an activator for carbonization to generate nitrogen-doped porous carbon material; the method is a two-step method, different gases are involved in the preparation process, and the process is complex; meanwhile, ammonia gas used in the preparation process has certain dangerousness. In patent CN201710009138.1, peanut shells are used as raw materials of porous carbon, melamine is used as nitrogen source, and nitrogen-doped porous carbon is obtained by carbonization, activation and purification; in patent CN201710006532.X, cellulose amino acid methyl ester is used as a raw material, urea is used as a nitrogen source, and nitrogen-doped porous carbon is obtained by carbonizing after treatment with a sodium hydroxide solution; the three modes all use chemical raw materials as introduced nitrogen sources, and a large amount of chemical raw materials are consumed in large-scale industrial application, so that the cost is increased.
Disclosure of Invention
In order to solve the problems of complex preparation process and high cost of the existing nitrogen-doped porous carbon, the invention provides a preparation method of nitrogen-doped porous biochar, which can simplify the preparation process and reduce the cost.
The technical scheme is as follows: the preparation method of the nitrogen-doped porous biochar is characterized by comprising the following steps of:
(1) pretreatment of raw materials: mixing and pretreating algae biomass and terrestrial biomass;
(2) adding an activating agent: mixing the pretreated raw materials with an activating agent;
(3) carbonization and acid washing: and (3) carbonizing the mixture obtained in the step (2) under the protection of inert gas, carrying out acid washing on the obtained biochar to be neutral after the reaction is finished, and drying to obtain the nitrogen-doped porous biochar.
The method is further characterized in that the terrestrial biomass and the algae biomass used in the step (1) are both dry powder, the terrestrial biomass comprises one or more of reed, reed flower, bagasse, taro stem and catkin, and the algae biomass comprises large-scale seaweed and microalgae;
in the step (1), the mass ratio of the terrestrial biomass to the algal biomass is 1: 0.2-1: 5, mixing modes comprise a dry mixing method and a hydrothermal method;
in the step (2), the activating agent comprises one or more of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, potassium oxalate and sodium oxalate, and the mass ratio of the pretreatment raw material to the activating agent is 1: 1-1: 10;
in the step 3), the carbonization temperature is 700-950 ℃, the heating rate is 3-10 ℃/min, and the carbonization temperature is kept for 1-3 h after reaching the preset temperature.
A method for preparing an electrode material by using the nitrogen-doped porous biochar is characterized by comprising the following steps:
putting 0.002-0.005 g of nitrogen-doped porous biochar into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into an ultrasonic instrument, vibrating for 0.5-2 hours, adding 100-200 mu L of 5% Nafion D-520 dispersion liquid after the ultrasonic treatment, continuing to perform ultrasonic treatment for 2-5 hours, uniformly coating the liquid in the centrifuge tube on foamed nickel after the vibration treatment, and extruding to prepare the supercapacitor electrode material.
After the invention is adopted, the algae biomass widely existing in nature is taken as a nitrogen source, so that a good nitrogen-rich reaction environment can be provided, rich algae resources can be fully utilized, environmental problems such as red tide, water bloom and the like caused by the enrichment of the algae biomass are prevented, and cellulose, hemicellulose and lignin in terrestrial biomass can generate a synergistic effect with protein in the algae biomass in the high-temperature reaction process of the nitrogen-containing algae biomass and the terrestrial biomass based on a biomass coupling mechanism, so that the formation of nitrogen-doped biochar is promoted, the surface microstructure of carbon is improved, and the electrochemical performance of the nitrogen-doped biochar is enhanced; the internal pore structure of the nitrogen-doped porous carbon is obviously improved through an activation reaction in a high-temperature environment, an effective interpenetrating pore channel is formed, the specific surface area is enlarged, and the buffer storage of electrolyte and the rapid transmission of electrolyte ions are improved; the method has the advantages that the pH value of the system is adjusted to be neutral, the impurities remained in the activation process can be effectively removed, the preparation method is simple to operate, the used raw materials are cheap and easy to obtain, the waste is changed into valuable, the cost is reduced, and meanwhile, a set of simple preparation process is provided, so that the method is a green, environment-friendly, economic, feasible, efficient and feasible preparation method of the nitrogen-containing porous carbon material for the high-performance supercapacitor; the electrode material for the super capacitor, which is obtained by the invention, has the advantages of very high mass specific capacitance, higher energy density, excellent rate capability and cycle stability.
Drawings
FIG. 1 is a schematic diagram of the morphological structure of nitrogen-doped porous carbon derived from a reed-chlorella coupling mechanism;
FIG. 2 is an XPS spectrum of nitrogen-containing porous carbon derived from the reed-chlorella coupling mechanism;
FIG. 3 is an XRD pattern of nitrogen-doped porous carbon derived from the reed-chlorella coupling mechanism;
FIG. 4 is a Raman spectrum of nitrogen-doped porous carbon derived from the reed-chlorella coupling mechanism;
FIG. 5 is a BET plot of nitrogen-doped porous carbon derived from the Phragmites communis-Chlorella coupled mechanism;
FIG. 6 is a graph of pore size distribution of nitrogen-doped porous carbon derived from the reed-chlorella coupling mechanism;
FIG. 7 is a Cyclic Voltammetry (CV) curve for nitrogen doped porous carbon derived from the Phragmites-Chlorella coupling mechanism;
fig. 8 is a charge-discharge (GCD) curve of nitrogen-doped porous carbon derived from the reed-chlorella coupled derivative mechanism.
Detailed Description
A preparation method of nitrogen-doped porous biochar comprises the following steps:
(1) pretreatment of raw materials: mixing terrestrial biomass and algae biomass according to the proportion of 1: 0.2-1: 5, performing mixing pretreatment according to a mass ratio, wherein the terrestrial biomass and the algae biomass are dry powder, the terrestrial biomass comprises one or more of reed, reed flower, bagasse, taro stem and catkin, the algae biomass comprises kelp, Enteromorpha prolifera, gulfweed, laver, Hizikia fusiforme and other large-scale seaweeds and microalgae such as chlorella, scenedesmus obliquus, spirulina, blue algae and the like, and the mixing mode comprises a dry mixing method and a hydrothermal method; the dry mixing method is that terrestrial biomass and algae biomass in a certain proportion are put into a mortar or a ball mill for full grinding, so that the terrestrial biomass and the algae biomass are fully contacted to obtain a pretreatment raw material; the hydrothermal method comprises the steps of putting a mixture of terrestrial biomass and algae biomass in a certain proportion into a hydrothermal kettle, adding deionized water, wherein the proportion of the mixture to the deionized water is 1g/20 ml-1 g/25ml, the reaction temperature is 80-200 ℃, the reaction time is 0.5-12 h, taking out solid residues in the reaction kettle after the reaction is finished, cleaning the solid residues with 200ml of deionized water for three times, and drying the solid residues in a drying box at 80 ℃ to obtain a pretreatment raw material;
(2) adding an activating agent: mixing the pretreated raw material with an activating agent, wherein the activating agent comprises one or more of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, potassium oxalate and sodium oxalate, and the mass ratio of the pretreated raw material to the activating agent is 1: 1-1: 10;
(3) carbonization and acid washing: and (3) putting the mixture obtained in the step (2) into a tubular furnace, carbonizing under the protection of inert gas, wherein the carbonization temperature is 700-950 ℃, the heating rate is 3-10 ℃/min, keeping for 1-3 h after the preset temperature is reached, pickling the obtained biochar to be neutral after the reaction is finished, and drying to obtain the nitrogen-doped porous biochar.
A method for making an electrode material using the nitrogen-doped porous biochar, comprising the steps of: putting 0.002-0.005 g of nitrogen-doped porous biochar into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into an ultrasonic instrument, vibrating for 0.5-2 hours, adding 100-200 mu L of 5% Nafion D-520 dispersion liquid after the ultrasonic treatment, continuing to perform ultrasonic treatment for 2-5 hours, uniformly coating the liquid in the centrifuge tube on foamed nickel after the vibration treatment, and extruding to prepare the supercapacitor electrode material.
The following is a specific description.
Example 1:
preparation of nitrogen-doped porous biochar:
(1) pretreatment of raw materials: grinding and mixing 1g of bagasse and 0.5g of scenedesmus obliquus uniformly;
(2) adding an activating agent: grinding the pretreated raw materials and potassium hydroxide according to the mass ratio of 1:1 to uniformly mix the raw materials and the potassium hydroxide;
(3) carbonization and acid washing: placing the mixture in the step (2) in a tube furnace, heating to 700 ℃ at a heating rate of 3 ℃/min under the argon atmosphere, preserving heat for 1h, and then naturally cooling to room temperature to obtain nitrogen-doped porous carbon; then, putting the obtained nitrogen-doped porous carbon into 200ml of 1mol/L hydrochloric acid solution, and stirring for 24 hours at room temperature; and finally, washing the acid-washed nitrogen-doped porous carbon with deionized water to be neutral, and drying in an oven at 105 ℃ for 24 hours to obtain the nitrogen-containing porous carbon material for the supercapacitor.
Preparing an electrode material in a three-electrode test system:
putting 0.002g of nitrogen-doped porous carbon into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into ultrasonic, vibrating for 0.5h, adding 100 mu L of 5% Nafion D-520 dispersion liquid after the reaction is finished, continuing to carry out ultrasonic treatment for 2h, then uniformly coating the liquid in the centrifuge tube on foamed nickel, and putting into a vacuum drying oven for drying for 24h at the temperature of 80 ℃.
Finally, the electrode was pressed for 30 seconds under a pressure of 3MPa with a tablet press to form a 10mm by 10mm electrode. The specific capacitance of a three-electrode system consisting of a platinum electrode and a mercury/mercury oxide electrode is 215F/g when the current density is 1A/g in a test of 6M KOH electrolyte.
Example 2:
preparation of nitrogen-doped porous biochar:
(1) pretreatment of raw materials: grinding and mixing 1g of reed powder and 1.2g of chlorella uniformly;
(2) adding an activating agent: grinding the pretreated raw materials and potassium bicarbonate according to the mass ratio of 1:4 to uniformly mix the raw materials and the potassium bicarbonate;
(3) carbonization and acid washing: placing the mixture in the step (2) in a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the argon atmosphere, preserving heat for 2h, and then cooling to room temperature; putting the obtained sample into 150ml of 2mol/L hydrochloric acid solution, and stirring for 24 hours at room temperature; and finally, washing the acid-washed material to be neutral, and drying in an oven at 105 ℃ for 24h to obtain the nitrogen-containing porous carbon material for the supercapacitor.
Preparing an electrode material in a three-electrode test system:
putting 0.003g of nitrogen-doped porous biochar into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into ultrasonic, oscillating for 1h, adding 100 mu L of 5% Nafion D-520 dispersion liquid after the oscillation is finished, continuing the ultrasonic treatment for 3h, and then uniformly coating the liquid in the centrifuge tube on foamed nickel.
Finally, the electrode was pressed for 100 seconds under a pressure of 10MPa with a tablet press to form a 10mm by 10mm electrode. And in a three-electrode system consisting of a platinum electrode and a mercury/mercury oxide electrode, in a test of 6M KOH electrolyte, the specific capacitance is 340F/g when the current density is 1A/g.
Relevant experimental data are given in figures 1 to 8.
Example 3:
preparation of nitrogen-doped porous biochar:
(1) pretreatment of raw materials: putting 1g of catkin and 5g of enteromorpha into a hydrothermal kettle, adding 30ml of deionized water, reacting at 80 ℃ for 12h, taking out solid residues in the reaction kettle after the reaction is finished, washing the solid residues with 200ml of deionized water for three times, and drying the solid residues in a drying box at 80 ℃ to obtain a pretreatment raw material;
(2) adding an activating agent: grinding the pretreated raw materials and potassium oxalate according to the mass ratio of 1:10 to uniformly mix the raw materials and the potassium oxalate;
(3) carbonization and acid washing: placing the mixture in the step (2) in a tube furnace, heating to 950 ℃ at a heating rate of 10 ℃/min under the argon atmosphere, preserving heat for 5 hours, and then cooling to room temperature; then, putting the obtained sample into 200ml of 2mol/L hydrochloric acid solution, and stirring for 24 hours at room temperature; and finally, washing the acid-washed material to be neutral, and drying in an oven at 105 ℃ for 24h to obtain the nitrogen-containing porous carbon material for the supercapacitor.
Preparing an electrode material in a three-electrode test system:
putting 0.005g of nitrogen-doped porous biochar into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into ultrasonic, vibrating for 5h, adding 100 mu L of 5% Nafion D-520 dispersion liquid after the vibration is finished, continuing to perform ultrasonic treatment for 5h, and then uniformly coating the liquid in the centrifuge tube on foamed nickel.
Finally, the electrode was pressed for 10 seconds under a pressure of 10MPa with a tablet press to form a 10mm by 10mm electrode. The specific capacitance of a three-electrode system consisting of a platinum electrode and a mercury/mercury oxide electrode is 203F/g when the current density is 1A/g in a test of 6M KOH electrolyte.
The algae biomass resource has the advantages of rich content, fast growth period, no land competition with people and the like, and is gradually attracted by people. Algal biomass contains a large amount of nitrogen-containing compounds and a small amount of inorganic elements such as phosphorus and sulfur, and is an ideal nitrogen source. Therefore, based on a biomass coupling mechanism, the nitrogen-containing algae biomass is combined with other terrestrial biomass to prepare the nitrogen-containing porous carbon with rich pores, so that the method is a green and economic synthesis mode. The nitrogen-doped porous carbon can fully utilize biomass resources, has a rich pore structure, a high specific surface area and excellent electrochemical performance, and has a high commercial application value. The obtained electrode material for the super capacitor has very high mass specific capacitance, high energy density, excellent rate capability and cycling stability. Therefore, the nitrogen-doped porous carbon disclosed by the invention can be applied to electrode materials of supercapacitors.
Claims (6)
1. The preparation method of the nitrogen-doped porous biochar is characterized by comprising the following steps of:
(1) pretreatment of raw materials: mixing and pretreating algae biomass and terrestrial biomass;
(2) adding an activating agent: mixing the pretreated raw materials with an activating agent;
(3) carbonization and acid washing: and (3) carbonizing the mixture obtained in the step (2) under the protection of inert gas, carrying out acid washing on the obtained biochar to be neutral after the reaction is finished, and drying to obtain the nitrogen-doped porous biochar.
2. The method for preparing nitrogen-doped porous biochar according to claim 1, wherein the terrestrial biomass and the algae biomass used in the step (1) are dry powder, the terrestrial biomass comprises one or more of reed, reed flower, bagasse, taro stem and catkin, and the algae biomass comprises macroalgae and microalgae.
3. The method for preparing nitrogen-doped porous biochar according to claim 1, wherein in the step (1), the mass ratio of the terrestrial biomass to the algal biomass is 1: 0.2-1: 5, the mixing mode comprises a dry mixing method and a hydrothermal method.
4. The method for preparing nitrogen-doped porous biochar according to claim 1, wherein in the step (2), the activating agent comprises one or more of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, potassium oxalate and sodium oxalate, and the mass ratio of the pretreatment raw material to the activating agent is 1: 1-1: 10.
5. The method for preparing nitrogen-doped porous biochar according to claim 1, wherein in the step 3), the carbonization temperature is 700-950 ℃, the temperature rise rate is 3-10 ℃/min, and the temperature is kept for 1-3 hours after the preset temperature is reached.
6. A method for preparing an electrode material by using the nitrogen-doped porous biochar is characterized by comprising the following steps: putting 0.002-0.005 g of nitrogen-doped porous biochar into a centrifuge tube, adding 1ml of absolute ethyl alcohol, putting into an ultrasonic instrument, vibrating for 0.5-2 hours, adding 100-200 mu L of 5% Nafion D-520 dispersion liquid after the ultrasonic treatment, continuing to perform ultrasonic treatment for 2-5 hours, uniformly coating the liquid in the centrifuge tube on foamed nickel after the vibration treatment, and extruding to prepare the supercapacitor electrode material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959739A (en) * | 2022-06-10 | 2022-08-30 | 佛山科学技术学院 | Bagasse-based Ni 2+ 、Co 2+ Preparation method of ion-doped biochar material |
| CN115043479A (en) * | 2022-05-17 | 2022-09-13 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN115424870A (en) * | 2022-08-30 | 2022-12-02 | 南昌工程学院 | Biomass-derived carbon material and preparation method and application thereof |
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2021
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043479A (en) * | 2022-05-17 | 2022-09-13 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN115043479B (en) * | 2022-05-17 | 2024-02-27 | 山西财经大学 | Nitrogen-doped biochar as well as preparation method and application thereof |
| CN114959739A (en) * | 2022-06-10 | 2022-08-30 | 佛山科学技术学院 | Bagasse-based Ni 2+ 、Co 2+ Preparation method of ion-doped biochar material |
| CN115424870A (en) * | 2022-08-30 | 2022-12-02 | 南昌工程学院 | Biomass-derived carbon material and preparation method and application thereof |
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