CN108455596B - Method for preparing nitrogen-rich hierarchical pore carbon material with high specific surface area by one-step carbonization method and application thereof - Google Patents
Method for preparing nitrogen-rich hierarchical pore carbon material with high specific surface area by one-step carbonization method and application thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing a nitrogen-rich hierarchical pore carbon material with a high specific surface area by a one-step carbonization method, which is characterized by comprising the following steps of: the method comprises the following steps: (1) grinding and mixing a nitrogen-containing heterocyclic compound serving as a precursor and an activating agent, and drying; (2) adding a template agent into the product obtained in the step (1) for grinding and mixing; (3) and (3) putting the product obtained in the step (2) into an inert atmosphere for carbonization treatment, and obtaining the nitrogen-rich hierarchical porous carbon material with high specific surface area after acid washing and water washing. The invention can obtain the nitrogen-rich hierarchical pore carbon material with high yield and adjustable pore size distribution and high specific surface area by utilizing a simple template-activation one-step carbonization method and adjusting process parameters. The preparation process is very simple and easy to operate, and has good application prospects in the fields of new energy, adsorption, catalyst carriers and the like.
Description
Technical Field
The invention relates to a method for preparing a nitrogen-rich hierarchical pore carbon material with a high specific surface area by a one-step carbonization method and application thereof, belonging to the field of energy materials and application.
Background
The energy crisis and the environmental problem are the core problems of human sustainable development and are key factors influencing energy decision and science and technology guidance of all countries in the world at present. The rapid development of supercapacitors in recent years has complied with the human demand for new energy. The super capacitor is an energy storage device between a traditional capacitor and a battery, and has the advantages of high power density, long cycle life, low cost and the like. The electrode mainly comprises a current collector, an electrode material and an electrolyte. Among them, the electrode material is a critical factor determining the performance and production cost of the supercapacitor. The development of a simple, efficient and practical supercapacitor electrode material becomes the core content of research.
The porous carbon has the advantages of good cycle stability, developed void structure, no toxicity, low price and the like, and is often used as an electrode material of a super capacitor. However, pure microporous, mesoporous, or macroporous carbons have difficulty achieving optimal performance of the carbon material in one aspect. Meanwhile, researches find that the ion transmission rate of the carbon electrode can be effectively improved by a macroporous-mesoporous-microporous intercommunicated hierarchical pore structure. Meanwhile, the intercommunicated skeleton structure effectively improves the transmission speed of electrons. Therefore, the pore structure of the carbon material is regulated and controlled, and the electrochemical performance of the carbon material can be effectively improved.
The currently reported method for preparing the hierarchical porous carbon material is generally subject to long synthesis period and complex preparation method; special process requirements (e.g. CO)2Supercritical drying); a large amount of organic solvent is consumed, and the method is not environment-friendly; low yield and the like. Therefore, it is necessary to develop a simple, efficient and high-yield method of nitrogen-enriched hierarchical porous carbon. The hierarchical porous carbon material is prepared by a solid-phase reaction by utilizing the chemical action between a carbon source and an activating agent and combining a template-activation one-step carbonization method, so that the porous carbon material can be efficiently and quickly prepared, and the yield of the carbon material can be greatly improved compared with the traditional template-activation composite two-step carbonization method.
The surface properties of the carbon material are also an aspect that affects the electrochemical performance of the carbon material. At present, it is common to incorporate heteroatoms such as N, S, P, B into the carbon skeleton to improve the electrochemical performance of the carbon material by improving the conductivity of the material and the surface wettability of the carbon material and electrolyte ions. Among them, nitrogen-doped porous carbon materials have become one of the hot spots in the field of international carbon materials. Nitrogen-containing reagents (e.g. NH) are commonly employed3Melamine and cyanamide) post-treatment method to prepare the porous carbon material. The nitrogen-containing functional groups introduced by the post-treatment method are poor in distribution uniformity on the surface of the carbon material. And a large amount of toxic gas is used in the process of treating the carbon material, so that the preparation process is not environment-friendly. In addition, when a nitrogen-containing functional group is introduced to the surface of the carbon in a post-treatment mode, the original pore structure and morphology of the carbon material are damaged to a certain extent.
The nitrogen-containing heterocyclic compound represented by nicotinic acid is a common chemical raw material and is widely applied to the fields of food, medicine, industrial manufacturing, feed and the like. Meanwhile, the nitrogen-containing heterocyclic compound has abundant nitrogen-containing functional groups and is a pyridine ring structure. The nitrogen atom on the pyridine ring is different from the nitrogen atom on the amino group and is relatively stable, so that the nitrogen-doped carbon material is easily obtained after direct carbonization and cracking. But the directly prepared hierarchical porous carbon has small specific surface area and low porosity, and is not suitable for being used as a super capacitor electrode. Therefore, how to adopt a simple preparation process and utilize nitrogen-containing heterocyclic compounds such as nicotinic acid and the like to prepare the nitrogen-rich hierarchical pore carbon material with high specific surface area has important practical significance.
Disclosure of Invention
The invention aims to: provides a method for preparing a nitrogen-rich hierarchical pore carbon material with high specific surface area by a one-step carbonization method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a nitrogen-rich hierarchical pore carbon material with a high specific surface area by a one-step carbonization method comprises the following steps:
(1) grinding and mixing a nitrogen-containing heterocyclic compound serving as a precursor and an activating agent, and drying;
(2) adding a template agent into the product obtained in the step (1) for grinding and mixing;
(3) and (3) putting the product obtained in the step (2) into an inert atmosphere for carbonization treatment, and obtaining the nitrogen-rich hierarchical porous carbon material with high specific surface area after acid washing and water washing.
Preferably, the drying temperature in the step (1) is 75-85 ℃, and the drying time is 1.8-2.2 h.
Preferably, the nitrogen-containing heterocyclic compound is at least one of nicotinic acid, isonicotinic acid, 2-picolinic acid and dipicolinic acid; the template agent is at least one of magnesium acetate, magnesium oxide, magnesium hydroxide, magnesium chloride and magnesium citrate; the activating agent is KOH, NaOH or Na2CO3、K2CO3At least one of (1).
Preferably, the molar ratio of the activating agent to the nitrogen-containing heterocyclic compound is (0.25-2): 1, and the mass ratio of the template agent to the nitrogen-containing heterocyclic compound is (0.5-2): 1.
Preferably, the carbonization time is 1-3 h, the carbonization temperature is 500-1000 ℃, and the temperature rise rate of carbonization is controlled to be 1-10 ℃/min.
Preferably, the inert gas is one or two of nitrogen and argon.
Preferably, the acid used for acid washing is at least one acid selected from hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid.
An application of a one-step carbonization method in preparing a nitrogen-rich hierarchical pore carbon material with a high specific surface area can be used as an electrode material of a super capacitor.
The invention has the beneficial effects that:
1. the invention prepares the nitrogen-rich hierarchical pore carbon material with high specific surface area by a solid-phase one-step carbonization method, has simple synthesis process, and has higher carbon yield compared with the traditional two-step carbonization method. And the whole preparation process does not need to use any organic solvent, is easy to operate and has high safety.
2. The carbon precursor is used as a carbon source and a nitrogen source, and the prepared porous carbon material contains rich nitrogen-oxygen functional groups, so that one-step nitrogen doping functionalization of the carbon material is realized, and the method is simple and practical.
3. According to the invention, the morphology and the pore structure of the carbon material can be effectively regulated and controlled by simply regulating and controlling the proportion among the pyridine ring compound containing carboxylic acid, the activating agent and the template agent, so that the microporous-mesoporous-macroporous intercommunicated hierarchical pore carbon material is prepared, and has a high specific surface area (1200-3100 m)2g-1)。
4. The nitrogen-doped hierarchical porous carbon material synthesized by the method can be used as a supercapacitor electrode. Preparing an electrode by taking the prepared nitrogen-containing hierarchical porous carbon material as an active material, acetylene black as a conductive agent and polytetrafluoroethylene emulsion as a binder according to a mass ratio of 8:1:1, and measuring 1Ag in a three-electrode system with KOH as an electrolyte system-1The lower mass specific capacitance is 250-320 Fg–1. After 5000 cycles, the capacity retention was greater than 92%.
5. With 1-ethyl-3-methylimidazolium tetrafluoroborate ([ EMIm ]]BF4) Mixed solution (mass ratio is 1:1) of AN is used as electrolyte, andthe porous carbon material is assembled into a symmetrical button type two-electrode super capacitor. The obtained super capacitor has a wide voltage window (0-2.2V) and a power density of 250Wkg–1The corresponding energy density can reach 25 to 32Wh kg–1。
Drawings
FIG. 1 is a field emission scanning electron micrograph of nitrogen-rich porous carbon prepared according to example 1 of the present invention;
FIG. 2 is a nitrogen adsorption-desorption isotherm of the nitrogen-rich porous carbon prepared in example 1 of the present invention;
FIG. 3 is a CV plot of the nitrogen-rich porous carbon prepared in example 1 of the present invention at different scan rates (5mV/s to 200mV/s) in a three-electrode system;
FIG. 4 is a GCD plot of nitrogen-rich porous carbon prepared in example 1 of the present invention at different current densities (0.5A/g-20A/g);
FIG. 5 is a graph of the cycle stability at 10A/g for nitrogen-rich porous carbon prepared in example 1 of the present invention.
FIG. 6 is a graph of energy density and power density for nitrogen-enriched porous carbon assembled supercapacitors made according to example 1 of the present invention.
Detailed Description
Example 1
In this example 1, nicotinic acid is used as a carbon precursor, potassium hydroxide is used as an activating agent, and magnesium hydroxide is used as a template to prepare a nitrogen-rich hierarchical pore carbon material with a high specific surface area:
2.46 g of nicotinic acid and 1.12 g of potassium hydroxide (molar ratio of 1:1) are weighed out, mixed in a mortar, ground for 30min, dried in an 80-degree oven for 2 hours, and then 3.69 g of magnesium hydroxide is weighed out and added to the solid mixture and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Fig. 1 is a scanning electron microscope image of the field emission of the nitrogen-rich porous carbon material prepared in this example 1, and it can be seen from the image that the carbon material has a continuous macroporous 3D framework structure, and a sheet-like carbon wall structure. The carbon particles are not blocky carbon particles with different sizes, which indicates that the dosage of the activating agent is proper and the reaction is mild.
FIG. 2 is a nitrogen adsorption-desorption isotherm of the nitrogen-rich porous carbon prepared in example 1 of the present invention. The prepared nitrogen-rich carbon material is proved to have the pore structure characteristics of rich micropores, limited mesopores and certain macropores. The hierarchical pore structure can effectively improve the transmission rate of ions, thereby improving the rate capability of the carbon material. The porous carbon material has high specific surface area, and the BET specific surface area is 2608m2g–1。
FIG. 3 is a graph showing CV curves of the nitrogen-rich porous carbon prepared in example 1 of the present invention showing quasi-rectangular shapes even at 200mV s, at different scan rates (5mV/s to 200mV/s) in a three-electrode system–1At a high scan rate. This indicates that the sample has ideal capacitive characteristics and electrochemically reversible behavior.
FIG. 4 is a GCD plot of nitrogen-rich porous carbon prepared in example 1 of the present invention at different current densities (1A/g-20A/g). These GCD curves all appear in the shape of triangles, indicating that the major supercapacitive contribution of the sample is from the EDLC. As can be seen from the figure, the curve is-1 to 0V in the voltage window, and the current density is 1 A.g-1Specific capacitance of 278.3F g–1，20A·g-1The specific time capacitance is 188F g–1The capacity multiplying power performance reaches 67.6 percent.
FIG. 5 is a graph of the cycle stability at 10A/g for nitrogen-rich porous carbon prepared in example 1 of the present invention. As can be seen from the figure, the capacity retention rate of the nitrogen-rich porous carbon electrode is 93 percent after 5000 cycles. The nitrogen-rich porous carbon electrode is shown to have excellent cycling stability.
FIG. 6 is a graph of energy density and power density for nitrogen-enriched porous carbon assembled supercapacitors made according to example 1 of the present invention. The electrolyte is [ EMIm]BF4/AN (the mass ratio of the BF4 to the AN is 1:1) is assembled into the button cell. It is clear that the nitrogen-rich porous carbon electrode prepared in example 1 has superior characteristicsEnergy density and power density values. At a power density of 283W kg–1The corresponding energy density is 22.4Wh kg–1(ii) a When the power density is increased to 13400W kg–1The energy density was reduced to 8Wh kg–1. It was further confirmed that the nitrogen-rich porous carbon prepared in example 1 has excellent capacitance characteristics and potential for application in supercapacitors.
Example 2
In this example 2, a high specific surface area nitrogen-rich hierarchical pore carbon material is prepared by using nicotinic acid as a carbon precursor, sodium hydroxide as an activating agent, and magnesium hydroxide as a template agent:
2.46 g of nicotinic acid and 0.8 g of sodium hydroxide (molar ratio of both 1:1) were weighed out, mixed in a mortar, ground for 30min, dried in an 80 ℃ oven for 2 hours, and then 2.46 g of magnesium hydroxide was weighed out, added to the above solid mixture, and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 3
In this embodiment 3, a high-yield nitrogen-rich hierarchical pore carbon material is prepared by using nicotinic acid as a carbon precursor, sodium hydroxide and potassium hydroxide as activators, and magnesium hydroxide as a template:
2.46 g of nicotinic acid and 0.4 g of sodium hydroxide and 0.56 g of potassium hydroxide were weighed out, mixed by grinding in a mortar, and after grinding for 30min and drying in an 80 ℃ oven for 2 hours, 2.46 g of magnesium hydroxide was weighed out and added to the above solid mixture and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 4
In this example 4, a high specific surface area nitrogen-rich hierarchical pore carbon material is prepared by using nicotinic acid as a carbon precursor, potassium hydroxide as an activator, and magnesium acetate as a template agent:
2.46 g of nicotinic acid and 1.12 g of potassium hydroxide (molar ratio of 1:1) are weighed out, mixed in a mortar, ground for 30min, dried in an 80-degree oven for 2 hours, and then 2.46 g of magnesium acetate is weighed out, added to the solid mixture and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 5
In this example 5, nicotinic acid is used as a carbon precursor, Na2CO3Preparing the high specific surface area nitrogen-rich hierarchical pore carbon material by taking magnesium hydroxide as an activating agent:
2.46 g nicotinic acid and 1.06 g Na were weighed out2CO3(the molar ratio of the two is 2:1), grinding and mixing are carried out in a mortar, after grinding for 30min, 2.46 g of magnesium hydroxide is weighed and added into the solid mixture after drying in an oven with the temperature of 80 ℃ for 2h, and grinding is carried out for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 6
In this example 6, K is a carbon precursor of nicotinic acid2CO3Preparing the high specific surface area nitrogen-rich hierarchical pore carbon material by taking magnesium hydroxide as an activating agent:
2.46 g nicotinic acid and 1.38 g K are weighed out2CO3(molar ratio of the two is 2:1), grinding and mixing in a mortar, and grindingAfter 30min, after drying in an 80 degree oven for 2 hours, 2.46 g of magnesium hydroxide were weighed into the above solid mixture and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 7
In this embodiment 7, an isonicotinic acid is used as a carbon precursor, potassium hydroxide is used as an activating agent, and magnesium hydroxide is used as a template to prepare a nitrogen-rich hierarchical pore carbon material with a high specific surface area:
2.46 g of isonicotinic acid and 1.12 g of potassium hydroxide (molar ratio of the two is 1:1) are weighed out, mixed in a mortar, ground for 30min, dried in an 80-degree oven for 2h, and then 2.46 g of magnesium hydroxide is weighed out, added to the solid mixture and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 8
In this embodiment 8, an isonicotinic acid is used as a carbon precursor, sodium hydroxide is used as an activating agent, and magnesium hydroxide is used as a template to prepare a nitrogen-rich hierarchical pore carbon material with a high specific surface area:
2.46 g of nicotinic acid and 0.8 g of sodium hydroxide (molar ratio of both 1:1) were weighed out, mixed in a mortar, ground for 30min, dried in an 80 ℃ oven for 2 hours, and then 2.46 g of magnesium oxide was weighed out, added to the above solid mixture, and ground for 10 min. And (3) heating the solid mixture to 800 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 9
In this example 9, a high specific surface area nitrogen-rich hierarchical porous carbon material is prepared with a carbonization temperature of 700 ℃:
2.46 g of nicotinic acid and 0.8 g of sodium hydroxide (molar ratio of both 1:1) were weighed out, mixed in a mortar, ground for 30min, dried in an 80 ℃ oven for 2 hours, and then 2.46 g of magnesium hydroxide was weighed out, added to the above solid mixture, and ground for 10 min. And (3) heating the solid mixture to 700 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 2 hours. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Example 10
In this example 10, a high specific surface area nitrogen-rich hierarchical porous carbon material is prepared with a carbonization time of 1 hour:
2.46 g of nicotinic acid and 1.12 g of potassium hydroxide (molar ratio of 1:1) are weighed out, mixed in a mortar, ground for 30min, dried in an 80-degree oven for 2 hours, and then 2.46 g of magnesium hydroxide is weighed out, added to the solid mixture and ground for 10 min. And (3) heating the solid mixture to 700 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen atmosphere, and preserving the temperature for 1 hour. Then naturally cooling to room temperature, grinding the calcined product, and stirring for 6 hours at room temperature by using 1% hydrochloric acid to fully dissolve the metal oxide. Then filtering, washing with distilled water, and drying to obtain the invented high specific surface area nitrogen-enriched hierarchical porous carbon material.
Claims (6)
1. A method for preparing a nitrogen-rich hierarchical pore carbon material with a high specific surface area by a one-step carbonization method is characterized by comprising the following steps: the method comprises the following steps:
(1) grinding and mixing a nitrogen-containing heterocyclic compound serving as a precursor and an activating agent, and drying;
(2) adding a template agent into the product obtained in the step (1) for grinding and mixing;
(3) putting the product obtained in the step (2) into an inert atmosphere for carbonization treatment, and obtaining the nitrogen-rich hierarchical porous carbon material with high specific surface area after acid washing and water washing;
the nitrogen-containing heterocyclic compound is at least one of nicotinic acid, isonicotinic acid, 2-picolinic acid and pyridine dicarboxylic acid; the template agent is at least one of magnesium acetate, magnesium oxide, magnesium hydroxide, magnesium chloride and magnesium citrate; the activating agent is KOH, NaOH or Na2CO3、K2CO3At least one of (1).
2. The method for preparing the nitrogen-rich hierarchical pore carbon material with high specific surface area by the one-step carbonization method according to claim 1, is characterized in that: the drying temperature in the step (1) is 75-85 ℃, and the drying time is 1.8-2.2 h.
3. The method for preparing the nitrogen-rich hierarchical pore carbon material with high specific surface area by the one-step carbonization method according to claim 1, is characterized in that: the molar ratio of the activating agent to the nitrogen-containing heterocyclic compound is (0.25-2): 1, and the mass ratio of the template agent to the nitrogen-containing heterocyclic compound is (0.5-2): 1.
4. The method for preparing the nitrogen-rich hierarchical pore carbon material with high specific surface area by the one-step carbonization method according to claim 1, is characterized in that: the carbonization time is 1-3 h, the carbonization temperature is 500-1000 ℃, and the temperature rise rate of carbonization is controlled at 1-10 ℃/min.
5. The method for preparing the nitrogen-rich hierarchical pore carbon material with high specific surface area by the one-step carbonization method according to claim 1, is characterized in that: the inert atmosphere is one or two of nitrogen and argon.
6. The method for preparing the nitrogen-rich hierarchical pore carbon material with high specific surface area by the one-step carbonization method according to claim 1, is characterized in that: the acid used for acid cleaning is at least one acid of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid.
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