CN110697714A - Radish-derived nitrogen-doped graded porous carbon and preparation method and application thereof - Google Patents
Radish-derived nitrogen-doped graded porous carbon and preparation method and application thereof Download PDFInfo
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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
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- 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
- Y02E60/30—Hydrogen technology
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Abstract
The invention relates to nitrogen-doped hierarchical porous carbon derived from radishes and a preparation method and application thereof. The hierarchical porous carbon not only keeps the natural porous structure of radish, but also has the characteristics of high graphitization degree, high nitrogen doping level and the like, and is suitable for electrode materials of new energy systems such as fuel cells, lithium ion batteries, super capacitors and the like.
Description
Technical Field
The invention belongs to the field of biomass energy, and particularly relates to radish-derived nitrogen-doped graded porous carbon and a preparation method and application thereof.
Background
Energy is the most basic motivation for human beings to live and develop in the new century. However, with the exhaustion of fossil fuels and the aggravation of environmental pollution, advanced energy conversion and storage technology is one of the major problems that need to be solved in the world today, and how to develop a new green and sustainable energy source in the future is a common problem facing the world at present. With the discovery and utilization of more new energy sources, such as solar, wind, tidal, biomass, etc., the demand for an energy storage and conversion device has increased dramatically. Fuel cells, lithium ion batteries, supercapacitors, and the like have a relatively high energy density, and are commonly used energy storages.
The porous carbon material has high specific surface area, good chemical stability and conductivity and low cost, and is widely used as an electrode material. Biomass, such as needle mushroom, leaves, peanut shells and the like, not only has rich carbon and nitrogen, but also channels for conveying nutrients in the biomass are templates for preparing a porous structure. The biomass charcoal takes biomass as a precursor, is simple to prepare, has sufficient and wide sources, and is environment-friendly, so that the exploration of a new biomass charcoal material as an electrode material of a battery has great significance.
The existing method for preparing the biomass charcoal material mainly comprises a self-activation method, a chemical activation method, a template method and the like for improving the pore structure, wherein the self-activation method is carried out at the temperature of 700 ~ 1000 ℃ and H2O，CO2And air as an activator, and forming pores by using an oxidation-reduction reaction with the precursor; the chemical activation method is to use alkali (KOH, NaOH), K2CO3、H3PO4Or ZnCl2Chemical substances such as the like chemically corrode the precursor, and the specific surface area is increased through pyrolysis polycondensation reaction in the activation process to form a rich pore structure; the template method is to introduce a material with ordered pores, soak the precursor in the template, make the pores react, and prepare the carbon material with single pore diameter by utilizing the self-limiting function of the template. The biomass carbon prepared by the method has the advantages of smaller specific surface area, low graphitization degree and damage to natural pores of biomassAnd (5) structure.
These conventional porous carbon preparation methods have the following disadvantages: firstly, the natural pore structure of biomass is seriously damaged in the high-temperature carbonization or activation process, and the transmission and diffusion of reaction substances are hindered. Secondly, the high temperature carbonization or activation process results in a loss of nitrogen content in the char. Thirdly, through a series of high temperature treatment processes, the yield of the biomass charcoal is low due to the generation and release of carbon dioxide, which causes the waste of carbon resources and aggravates the greenhouse effect. Therefore, the prepared biomass carbon has smaller specific surface area and low graphitization degree, and the natural pore structure of the biomass is damaged.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the nitrogen-doped hierarchical porous carbon derived from radish and the preparation method and application thereof. The hierarchical porous carbon obtained by the invention not only keeps the natural porous structure of the radish, but also has the characteristics of high graphitization degree, high nitrogen doping level and the like. The radish-derived nitrogen-doped hierarchical porous carbon is suitable for electrode materials of new energy systems such as fuel cells, lithium ion batteries, super capacitors and the like.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: a method of preparing radish-derived nitrogen-doped graded porous carbon, comprising the steps of:
(1) peeling and cleaning radish, drying, and crushing into powder;
(2) immersing the carbon powder into saturated aqueous solution of a metal salt activating agent, and performing hydrothermal carbonization or drying and direct pyrolysis carbonization on the mixed solution to obtain carbon solid powder;
(3) activating the obtained carbon solid powder; washing with hydrochloric acid and deionized water to neutrality, and drying to obtain black powder;
(4) and (3) treating the black powder for 1-3 hours at the temperature of 700-1000 ℃ in a tubular furnace under the atmosphere of ammonia gas, and then cooling the black powder to room temperature along with the furnace to finally obtain the nitrogen-doped hierarchical porous carbon.
In a preferred embodiment of the present invention, the radish used in step (1) is a mature or incompletely mature white radish, red radish, watery radish or the like.
In a preferred embodiment of the present invention, in the step (2), the metal salt activator is a saturated solution of mixed metal salt of one or more of sodium, zinc and iron; more preferably, the mixed saturated solution of sodium chloride and zinc chloride, sodium chloride and ferric chloride, zinc chloride and ferric chloride, and sodium chloride, zinc chloride and ferric chloride is used.
In a preferred embodiment of the invention, in the step (2), the temperature of the hydrothermal carbonization is 160 ~ 220 ℃ and the time of the hydrothermal carbonization is 6 ~ 24h, and the condition of the pyrolysis carbonization is that the low-temperature treatment is carried out at 400 ~ 700 ℃ for 1-3h under nitrogen or argon.
In a preferred embodiment of the invention, in the step (3), the activation treatment is to activate the carbon solid powder with potassium hydroxide at 550 ℃ for 1-3h, wherein the mass ratio of potassium hydroxide to the carbon solid powder is 2:1, the obtained activated product is placed in a hydrochloric acid solution to be stirred and washed, then washed with deionized water and dried to obtain black powder, and the concentration of the hydrochloric acid solution is 1 ~ 3 mol/L.
In a preferred embodiment of the present invention, in the step (4), the temperature increase rate is 5 ~ 10 ℃/min.
The invention also provides radish-derived nitrogen-doped hierarchical porous carbon which is prepared by the preparation method and has rich micropore, mesopore and macropore structures, the atomic percentage content of nitrogen element is 0.1-5 at%, and the specific surface area is 1074.98-1756.68 m2g-1Characterization of graphitization degree index ID/IGIs 1.08-1.16.
The invention also protects the radish-derived nitrogen-doped hierarchical porous carbon for preparing electrode materials of lithium batteries, fuel cells and supercapacitors.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts radish as a carbon precursor, adds metal salt as an activating agent, and pretreats the radish by using a saturated solution of the metal salt to keep the natural pore structure of the radish. The radish-based porous carbon has a developed pore structure, contains abundant micropores, mesopores and macropores, is hexagonal, has a high specific surface area and a high graphitization degree, contains 0.1-5 at% of nitrogen element in atomic percentage, and has a specific surface area as high as 1074.98-1756.68 m2g-1Characterization of graphitization degree index ID/IGIs 1.08-1.16.
(2) Conventional pyrolytic charring or activation processes can disrupt the natural pore structure of biomass, and secondly, high temperature charring and/or activation processes can result in significant loss of primary nitrogen. In addition, after a series of high-temperature treatment processes, the yield of biomass charcoal is low due to the generation and release of a large amount of carbon dioxide, which not only results in the waste of a large amount of charcoal resources, but also aggravates the greenhouse effect. Hypersaline solution (NaCl, ZnCl)2，FeCl3) The biomass treated by the super-salt solution not only can effectively retain the natural pore structure of the biomass, but also can fully utilize carbon and nitrogen in the biomass through liquid impregnation and ion exchange, so that a novel and feasible carbonization and activation path can be provided by treating the biomass by the super-salt solution.
(3) The radish-based hierarchical porous carbon prepared by the method maintains the original biological pore structure and the original nitrogen element, and has excellent oxygen reduction catalytic activity and electrochemical stability. The radish-based porous carbon with high specific surface area and hierarchical pore structure is prepared by using radish as a precursor through carbonization and activation, and the oxygen reduction electrocatalytic activity and stability of the radish-based porous carbon are higher than those of commercial platinum carbon through tests.
(4) The radish precursor adopted by the invention has rich sources, high radish yield, low cost, environmental friendliness, simple preparation method and operation, and suitability for large-scale production.
Drawings
The invention will be further described with reference to the accompanying drawings, which are only schematic illustrations and illustrations of the invention, and do not limit the scope of the invention.
FIG. 1 is an electron microscope image of the micro-morphology of the radish-based porous carbon prepared in example 1;
FIG. 2 is a transmission electron micrograph of a micro-morphology of the radish-based porous carbon prepared in example 1;
FIG. 3 is a graph showing a pore size distribution curve and nitrogen isothermal adsorption and desorption of the porous carbon prepared in example 1;
FIG. 4 is an N, C, O atomic XPS survey of the porous carbon component prepared in example 1;
FIG. 5 is an electron micrograph of a micro-morphology of the radish-based porous carbon prepared in example 2;
FIG. 6 is a polarization diagram of the graded porous carbon prepared in example 1 (electrolyte solution is 0.1 mol/L KOH solution);
FIG. 7 is a chronoamperometric graph of the porous carbon in example 1 (electrolyte solution is 0.1 mol/L KOH solution).
Detailed Description
In order to clearly understand the objects, technical solutions and technical effects of the present invention, the present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.
"exemplary" means "serving as an example, instance, or illustration" herein, and any illustration, embodiment, or steps described as "exemplary" herein should not be construed as a preferred or advantageous alternative.
Example 1
Cleaning radish, drying, grinding, crushing, soaking radish powder in saturated solution of sodium chloride, zinc chloride and ferric chloride, carbonizing in a hydrothermal oven at 190 ℃ for 12h, washing with deionized water, and drying to obtain carbon solid powder; mixing the obtained carbon solid powder with KOH solid powder according to the mass ratio of 1:2, and then carrying out potassium hydroxide activation treatment for 2h at the temperature of 550 ℃; then washing the porous carbon by using 3mol/L hydrochloric acid and deionized water until the porous carbon is neutral, and drying the porous carbon to obtain porous carbon; and (3) placing the porous carbon in a tubular furnace under the atmosphere of ammonia gas, heating to 900 ℃ at the speed of 5 ︒/min, preserving heat for 2h, and naturally cooling to room temperature to obtain the radish-based porous carbon.
The radish-derived nitrogen-doped hierarchical porous carbon prepared in example 1 has a sheet-like structure as shown in fig. 1, and has a rich pore structure including micropores, mesopores, and macropores, and the pores can be seen as hexagons in a transmission view as shown in fig. 2. The specific surface area of the obtained porous carbon reaches 1595.42 m through a nitrogen isothermal adsorption and desorption test2g-1The nitrogen adsorption and desorption and the pore size distribution are shown in figure 3; the nitrogen content was 2.38at%, the oxygen content was 13.68% and the carbon content was 81.51% as measured by X-ray photoelectron spectroscopy as shown in FIG. 4.
Example 2
Cleaning radish, drying, grinding, pulverizing, soaking radish powder in saturated solution of sodium chloride, zinc chloride and ferric chloride, drying at room temperature, treating at 400 deg.C for 3 hr, treating at 700 deg.C for 2 hr, and naturally cooling to room temperature to obtain carbonized product; mixing the carbonized product obtained above and KOH solid powder in a mass ratio of 1:2, mixing, and then carrying out potassium hydroxide activation treatment for 2 hours at the temperature of 550 ℃; then washing the porous carbon by using 3mol/L hydrochloric acid and deionized water until the porous carbon is neutral, and drying the porous carbon to obtain porous carbon; and (3) placing the porous carbon in a tubular furnace under the atmosphere of ammonia gas, heating to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 2h, and naturally cooling to room temperature to obtain the radish-based porous carbon.
The radish-derived nitrogen-doped hierarchical porous carbon prepared in example 2 has a lamellar structure, as shown in fig. 5, and has a rich pore structure including micropores, mesopores, and macropores. Tests show that the specific surface area of the obtained porous carbon reaches 1480.66m2g-1The nitrogen content was 2.21at%, the oxygen content was 14.23%, and the carbon content was 79.31%.
Example 3
The method comprises the following steps: weighing 5 mg of the radish-based porous carbon prepared in example 1, dispersing the radish-based porous carbon into 1 mL of ethanol solution, performing ultrasonic treatment for 30min, adding 50 muL of Nafion membrane solution, mixing, and performing ultrasonic treatment for 10 min to prepare a catalyst solution. And (3) taking 10 mu L of the catalyst solution prepared in the step 1, and uniformly spin-coating the catalyst solution on a glassy carbon electrode to obtain an electrode to be tested.
A test electrode of a commercial platinum carbon catalyst was prepared using the method of step one.
Step two: and (3) assembling a three-electrode system by taking the electrode prepared in the step one as a working electrode, a carbon rod as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out electrochemical performance test, wherein 0.1 mol/L KOH solution is used as electrolyte. As shown in fig. 6, the radish-based porous carbon showed excellent oxygen reduction catalytic activity, superior to that of the commercial platinum carbon catalyst.
Step three: the chronoamperometric test of the radish-based porous carbon tested with the three-electrode system in step two, as shown in fig. 7, the radish-based porous carbon showed excellent electrochemical stability, superior to the commercial platinum carbon catalyst.
It should be understood that although the present description has been described in terms of various embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and those skilled in the art will recognize that the embodiments described herein may be combined as suitable to form other embodiments, as will be appreciated by those skilled in the art.
The above list of details is only a concrete description of the feasible examples of the present invention and they are not intended to limit the scope of the present invention, and all equivalent embodiments or modifications such as combinations, divisions or repetitions of the features, which do not depart from the concept and technical solution of the present invention, should be included in the scope of the present invention.
Claims (8)
1. A method for preparing radish-derived nitrogen-doped graded porous carbon, which is characterized by comprising the following steps:
(1) peeling and cleaning radish, drying, and crushing into powder;
(2) immersing the carbon powder into saturated aqueous solution of a metal salt activating agent, and performing hydrothermal carbonization or drying and direct pyrolysis carbonization on the mixed solution to obtain carbon solid powder;
(3) activating the obtained carbon solid powder; washing with hydrochloric acid and deionized water to neutrality, and drying to obtain black powder;
(4) and (3) treating the black powder for 1-3 hours at the temperature of 700-1000 ℃ in a tubular furnace under the atmosphere of ammonia gas, and then cooling the black powder to room temperature along with the furnace to finally obtain the nitrogen-doped hierarchical porous carbon.
2. The method according to claim 1, wherein the radish used in step (1) is a mature or incompletely mature white radish, red radish or watery radish.
3. The preparation method according to claim 1, wherein in the step (2), the metal salt activator is a saturated solution of mixed metal salt of one or more of sodium, zinc and iron; more preferably, the mixed saturated solution of sodium chloride and zinc chloride, sodium chloride and ferric chloride, zinc chloride and ferric chloride, and sodium chloride, zinc chloride and ferric chloride is used.
4. The preparation method according to claim 1, wherein in the step (2), the temperature of the hydrothermal carbonization is 160 ~ 220 ℃, the time of the hydrothermal carbonization is 6 ~ 24h, and the condition of the pyrolysis carbonization is that the low-temperature treatment is carried out for 1-3h at 400 ~ 700 ℃ under nitrogen or argon.
5. The preparation method according to claim 1, wherein in the step (3), the activation treatment is to activate the carbon solid powder with potassium hydroxide at 550 ℃ for 1-3h, the mass ratio of potassium hydroxide to the carbon solid powder is 2:1, the obtained activated product is placed in a hydrochloric acid solution, stirred and washed, then washed with deionized water and dried to obtain black powder, and the concentration of the hydrochloric acid solution is 1 ~ 3 mol/L.
6. The production method according to claim 1, wherein in the step (4), the temperature increase rate is 5 ~ 10 ℃/min.
7. Radish derivative produced by the method according to any one of claims 1 to 6The nitrogen-doped hierarchical porous carbon is characterized by having rich micropore, mesopore and macropore structures, the atomic percentage content of nitrogen element is 0.1-5 at%, and the specific surface area is 1074.98-1756.68 m2g-1Characterization of graphitization degree index ID/IGIs 1.08-1.16.
8. The radish-derived nitrogen-doped graded porous carbon as claimed in claim 7, which is used for preparing electrode materials of lithium batteries, fuel cells and supercapacitors.
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| CN113942995A (en) * | 2021-11-15 | 2022-01-18 | 中国空间技术研究院 | Heteroatom-doped porous carbon material and preparation method and application thereof |
| CN113942995B (en) * | 2021-11-15 | 2023-12-08 | 中国空间技术研究院 | Heteroatom doped porous carbon material and preparation method and application thereof |
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