CN115010130A - Nitrogen-doped porous carbon material and preparation method and application thereof - Google Patents
Nitrogen-doped porous carbon material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a nitrogen-doped porous carbon material and a preparation method and application thereof, and relates to the technical field of porous carbon materials. The preparation method of the nitrogen-doped porous carbon material provided by the invention comprises the following steps: carbonizing the biomass material to obtain a carbon source; mixing the carbon source and the potassium oxamate aqueous solution, and drying to obtain a mixture; and carrying out heat treatment on the mixture under the protective atmosphere to obtain the nitrogen-doped porous carbon material. According to the invention, potassium oxamate is used as an activator, so that the method is safer compared with the traditional activators such as potassium hydroxide, and can be used for synchronously completing nitrogen doping in the activation process so as to directly prepare the nitrogen-doped porous carbon material.
Description
Technical Field
The invention relates to the technical field of porous carbon materials, in particular to a nitrogen-doped porous carbon material and a preparation method and application thereof.
Background
The porous carbon material is one of the most widely used adsorbent materials and is used for absorbing various gasesThe adjuvant is widely studied. Its CO 2 The adsorption characteristics are of greater interest to researchers throughout the world, primarily due to the potential of porous carbon materials for use in carbon capture and storage technologies. The adsorption performance of the porous carbon material on carbon dioxide at the pressure of 1bar is mainly determined by the number of active adsorption sites contained therein, namely, the micropores (<0.7nm) and the number of nitrogen-containing basic groups.
Chemical activation is the most common method for forming a developed porous structure in carbon materials. The main process of chemical activation is to carbonize different starting materials to serve as a carbon source, uniformly mix the carbon source and an activating agent, and then perform carbonization treatment at high temperature. Currently, the most widely used activators are potassium hydroxide, sodium hydroxide, phosphoric acid, zinc chloride, and the like. The activator has universality, but also has certain corrosiveness, and can corrode instrument and equipment to a certain extent at high temperature. To achieve nitrogen doping in carbon materials, there are two main approaches: firstly, organic matters containing nitrogen are used as nitrogen sources, but the number of the nitrogen sources is limited, and more requirements are provided for preparing carbon sources of carbon materials; secondly, the carbon material is post-treated by using nitrogen-containing substances under the high-temperature condition, and the method has the main defect of excessively complex process. Therefore, a safer and simpler method is developed to realize one-step preparation of the nitrogen-doped porous carbon material, and CO is prepared 2 Adsorption studies also have significant value.
Disclosure of Invention
The invention aims to provide a nitrogen-doped porous carbon material and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a nitrogen-doped porous carbon material, which comprises the following steps:
carbonizing the biomass material to obtain a carbon source;
mixing the carbon source and the potassium oxamate aqueous solution, and drying to obtain a mixture;
and carrying out heat treatment on the mixture under the protective atmosphere to obtain the nitrogen-doped porous carbon material.
Preferably, the biomass material comprises one or more of glucose, sucrose, starch, lignin and cellulose.
Preferably, the carbonization treatment is hydrothermal carbonization or high-temperature carbonization;
the temperature of the hydrothermal carbonization is 160-220 ℃, and the heat preservation time of the hydrothermal carbonization is 1-6 h;
the temperature of the high-temperature carbonization is 400-600 ℃, and the heat preservation time of the high-temperature carbonization is 1-2 h.
Preferably, the mass ratio of the carbon source to the potassium oxamate in the potassium oxamate aqueous solution is 1: 1-5.
Preferably, the temperature of the heat treatment is 600-900 ℃; the heat preservation time of the heat treatment is 1-2 h.
Preferably, the temperature rising rate from the room temperature to the heat treatment temperature is 1-15 ℃/min.
Preferably, after the heat treatment, the method further comprises washing and drying in sequence.
The invention provides the nitrogen-doped porous carbon material prepared by the preparation method in the technical scheme.
Preferably, the specific surface area of the nitrogen-doped porous carbon material is 600-1500 m 2 The nitrogen content is 2.00-3.50 wt%.
The invention provides the technical scheme that the nitrogen-doped porous carbon material adsorbs CO 2 The use of (1).
The invention provides a preparation method of a nitrogen-doped porous carbon material, which comprises the following steps: carbonizing the biomass material to obtain a carbon source; mixing the carbon source and the potassium oxamate aqueous solution, and drying to obtain a mixture; and carrying out heat treatment on the mixture under the protective atmosphere to obtain the nitrogen-doped porous carbon material. According to the invention, potassium oxamate is used as an activating agent, so that the method is safer compared with the traditional activating agents such as potassium hydroxide and the like, and can synchronously complete nitrogen doping in the activating process so as to directly prepare the nitrogen-doped porous carbon material.
Drawings
FIG. 1 is a Raman spectrum test result chart of the nitrogen-doped porous carbon material prepared in examples 1 to 3;
FIG. 2 is a graph showing XPS test results of nitrogen-doped porous carbon materials prepared in examples 1 to 3;
FIG. 3 is a TEM test photograph of the nitrogen-doped porous carbon material prepared in example 3;
FIG. 4 shows N at-196 ℃ for the nitrogen-doped porous carbon material prepared in examples 1 to 3 2 Adsorption and desorption curve graphs;
FIG. 5 shows CO at 0 ℃ and 25 ℃ for the nitrogen-doped porous carbon materials prepared in examples 1 to 3 2 Adsorption isotherms.
Detailed Description
The invention provides a preparation method of a nitrogen-doped porous carbon material, which comprises the following steps:
carbonizing the biomass material to obtain a carbon source;
mixing the carbon source and the potassium oxamate aqueous solution, and drying to obtain a mixture;
and carrying out heat treatment on the mixture under the protective atmosphere to obtain the nitrogen-doped porous carbon material.
In the present invention, all the raw materials are commercially available products well known in the art unless otherwise specified.
The invention carries out carbonization treatment on the biomass material to obtain the carbon source. In the present invention, the biomass material preferably comprises one or more of glucose, sucrose, starch, lignin and cellulose.
In the present invention, the carbonization treatment is preferably hydrothermal carbonization or high-temperature carbonization.
In the present invention, when the carbonization treatment is hydrothermal carbonization, the medium for the hydrothermal carbonization preferably includes water; the mass ratio of the water to the biomass material is preferably 100: 5-20, and more preferably 100: 10. In the invention, the temperature of the hydrothermal carbonization is preferably 160-220 ℃, and more preferably 180-210 ℃; the heat preservation time of the hydrothermal carbonization is preferably 1-6 h, and more preferably 2-4 h. In the hydrothermal carbonization process, the biomass material is subjected to polycondensation reaction to form a polymer with high carbon content as a carbon material activation precursor.
After the hydrothermal carbonization, the method preferably further comprises the steps of filtering, washing and drying the obtained hydrothermal carbonization liquid in sequence. The filtration is not particularly limited in the present invention, and may be performed by a method known to those skilled in the art. In the invention, the washing reagent is preferably deionized water, and the number of washing is preferably 2-3, and more preferably 3. In the invention, the drying temperature is preferably 100-120 ℃, and more preferably 100-110 ℃; the drying time is preferably 4-6 h, and more preferably 4 h. In the present invention, the drying may remove moisture doped in the washed product.
In the invention, when the carbonization treatment is high-temperature carbonization, the temperature of the high-temperature carbonization is preferably 400-600 ℃, and more preferably 500-600 ℃; the high-temperature carbonization time is preferably 1-2 h, and more preferably 1.5-2 h; in the present invention, the rate of temperature increase to the high-temperature carbonization temperature is 5 to 15 ℃/min, and more preferably 10 ℃/min. In the present invention, the high-temperature carbonization is preferably performed under a protective atmosphere, and the gas for providing the protective atmosphere is preferably nitrogen or argon. In the present invention, the high-temperature carbonization is preferably performed in a tube furnace. In the present invention, the high-temperature carbonization preferably includes: and (3) placing the biomass material in a tubular furnace, and continuously introducing gas for providing protective atmosphere to carry out high-temperature carbonization. In the present invention, the flow rate of the gas for providing the protective atmosphere into the tube furnace is preferably 60 mL/min.
In the high-temperature carbonization process, the biomass material is subjected to a high-temperature cracking reaction, so that the hydrogen and oxygen content is reduced, the carbon content is increased, and a carbon material activation precursor is formed.
After the carbon source is obtained, the carbon source and the potassium oxamate aqueous solution are mixed and dried to obtain a mixture. In the present invention, the method for preparing the potassium oxamate aqueous solution preferably comprises: dissolving potassium oxamate in water to obtain potassium oxamate water solution. In the present invention, the water is preferably deionized water; the mass ratio of the potassium oxamate to the water is preferably 1: 5-15, and more preferably 1: 5-10. In the invention, the mass ratio of the carbon source to the potassium oxamate is preferably 1: 1-5, and more preferably 1: 1-3. In the invention, the mixing temperature is preferably 20-30 ℃, and more preferably 25-30 ℃; the mixing is preferably carried out under stirring conditions; the mixing time is preferably 2 h. In the invention, the drying temperature is preferably 100-120 ℃, and more preferably 100-110 ℃; the drying time is preferably 4-5 h.
After the mixture is obtained, the mixture is subjected to heat treatment under a protective atmosphere to obtain the nitrogen-doped porous carbon material. In the invention, the heat treatment temperature is preferably 600-900 ℃, and more preferably 700-800 ℃; the heat preservation time of the heat treatment is preferably 1-2 h. In the present invention, the rate of temperature increase from room temperature to the temperature of the heat treatment is preferably 1 to 15 ℃/min, and more preferably 5 to 10 ℃/min. In the present invention, the heat treatment is preferably performed in a tube furnace. In the present invention, the protective atmosphere is preferably a nitrogen atmosphere or an argon atmosphere. In the present invention, the heat treatment preferably includes: a protective gas providing a protective atmosphere is continuously passed into the tube furnace. In the present invention, the flow rate of the shielding gas introduced into the tube furnace is preferably 60 mL/min.
In the heat treatment process, the carbon material activation precursor and potassium oxamate are subjected to activation reaction at high temperature, carbon is corroded to form a porous structure, and nitrogen doping is completed simultaneously to obtain the nitrogen-doped porous carbon material.
After the heat treatment, the present invention preferably further comprises washing and drying in this order. In the present invention, the washing preferably includes acid washing and water washing sequentially; the acid-washing reagent preferably comprises a strong acid aqueous solution; the strong acid aqueous solution preferably comprises hydrochloric acid aqueous solution; the concentration of the strong acid aqueous solution is preferably 5-20 wt%, and more preferably 10 wt%; in the present invention, the water is washed to pH 7.0.
In the invention, the drying temperature is preferably 100-120 ℃, and more preferably 100-110 ℃; the drying time is preferably 4-5 h, and more preferably 4 h.
The invention provides the nitrogen-doped porous carbon material prepared by the preparation method in the technical scheme. In the invention, the nitrogen-doped porous carbon material is mainly of a microporous structure and simultaneously comprises mesopores.
In the invention, the specific surface area of the nitrogen-doped porous carbon material is preferably 600-1500 m 2 Per g, more preferably 664 to 1497m 2 (ii)/g; the nitrogen content is preferably 2.00 to 3.50 wt%, more preferably 2.25 to 2.52 wt%.
The invention provides the technical scheme that the nitrogen-doped porous carbon material adsorbs CO 2 The use of (1).
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Dissolving 5.0g of sucrose in 50mL of water to form a transparent solution, placing the transparent solution in a stainless steel hydrothermal reaction kettle, and carrying out hydrothermal carbonization treatment for 6 hours at 200 ℃; filtering the obtained hydrothermal carbonization liquid, repeatedly washing with deionized water, and finally drying at 100 ℃ for 4h to obtain a carbon source;
dissolving 2.0g of potassium oxamate in 15mL of deionized water to form a transparent solution, adding 1.0g of the carbon source, stirring at room temperature for 2 hours, and drying at 100 ℃ for 5 hours to obtain a mixture;
placing the mixture in a tubular furnace, and introducing nitrogen for protection, wherein the flow rate of the nitrogen is 60 mL/min; raising the temperature of the tubular furnace from room temperature to 700 ℃ at the speed of 10 ℃/min, and carrying out heat treatment for 2h at 700 ℃; and after natural cooling, washing the product by using a 10 wt% hydrochloric acid aqueous solution, repeatedly washing by using deionized water until the pH of the washing solution is 7.0, and drying at 100 ℃ for 4 hours to obtain the nitrogen-doped porous carbon material.
Example 2
Putting lignin in a tube furnace, heating the furnace temperature to 500 ℃ at the speed of 10 ℃/min under the protection of nitrogen (60mL/min), carbonizing the lignin at high temperature for 2h, and naturally cooling the lignin to room temperature to obtain a carbon source;
dissolving 2.0g of potassium oxamate in 15mL of deionized water to form a transparent solution, adding 1.0g of the carbon source, stirring for 2 hours at room temperature, and drying for 5 hours at 100 ℃ to obtain a mixture;
placing the mixture in a tubular furnace, and introducing nitrogen for protection, wherein the flow rate of the nitrogen is 60 mL/min; the furnace temperature of the tubular furnace is increased from room temperature to 800 ℃ at the speed of 10 ℃/min, and heat treatment is carried out for 2h at 800 ℃; and after natural cooling, washing the product by using a 10 wt% hydrochloric acid aqueous solution, repeatedly washing by using deionized water until the pH value of the washing solution is 7.0, and drying at 100 ℃ for 4h to obtain the nitrogen-doped porous carbon material.
Example 3
Putting lignin in a tube furnace, heating the furnace temperature to 500 ℃ at the speed of 10 ℃/min under the protection of nitrogen (60mL/min), carbonizing the lignin at high temperature for 2h, and naturally cooling the lignin to room temperature to obtain a carbon source;
dissolving 3.0g of potassium oxamate in 15mL of deionized water to form a transparent solution, adding 1.0g of the carbon source, stirring at room temperature for 2 hours, and drying at 100 ℃ for 5 hours to obtain a mixture;
placing the mixture in a tubular furnace, and introducing nitrogen for protection, wherein the flow rate of the nitrogen is 60 mL/min; raising the temperature of the tubular furnace from room temperature to 800 ℃ at the speed of 10 ℃/min, and carrying out heat treatment for 2h at 800 ℃; and after natural cooling, washing the product by using a 10 wt% hydrochloric acid aqueous solution, repeatedly washing by using deionized water until the pH value of the washing solution is 7.0, and drying at 100 ℃ for 4h to obtain the nitrogen-doped porous carbon material.
Test example
Raman spectrum tests are carried out on the nitrogen-doped porous carbon materials prepared in examples 1-3, and the test results are shown in figure 1. As can be seen from FIG. 1, the nitrogen-doped porous carbon material I prepared in examples 1 to 3 D /I G The values are 1.15, 1.32, 1.22, respectively. Higher I D /I G The values show that the nitrogen-doped porous carbon material prepared in examples 1-3 has a structure mainly amorphous and has a large number of defects.
XPS test was performed on the nitrogen-doped porous carbon material prepared in examples 1 to 3, and the test results are shown in FIG. 2. FIG. 2 shows that nitrogen doping was successfully achieved in the carbon material after potassium oxamate activation treatment. The nitrogen-doped porous carbon materials prepared in examples 1 to 3 had nitrogen contents of 2.52 wt%, 2.25 wt%, and 2.36 wt%, respectively. It can be seen that the nitrogen content in the nitrogen-doped porous carbon materials prepared in examples 2 to 3 was reduced compared to that in example 1 due to the increase in activation temperature (heat treatment temperature).
Fig. 3 is a TEM test photograph of the nitrogen-doped porous carbon material prepared in example 3. FIG. 3 shows that a uniform and developed porous structure is formed in the prepared nitrogen-doped porous carbon material, and potassium oxamate is proved to be capable of effectively forming the porous structure in the carbon material under the high-temperature condition. Meanwhile, the amorphous structure characteristic of the nitrogen-doped porous carbon material is also shown in FIG. 3, and the result is consistent with the test result in FIG. 1.
The nitrogen gas adsorption and desorption test was performed on the nitrogen-doped porous carbon material prepared in examples 1 to 3, the test method was a static volume method adsorption test, and the test results are shown in fig. 4. As can be seen from fig. 4, after the potassium oxamate activation treatment, developed porous structures are formed in the nitrogen-doped porous carbon materials prepared from different biomass materials, which are consistent with the characteristics shown in the TEM photograph in fig. 3. The specific surface area of the nitrogen-doped porous carbon material prepared in example 1 is 664m 2 (ii) in terms of/g. Specific surface area of nitrogen-doped porous carbon material prepared in example 2 was 948m 2 The specific surface area of the nitrogen-doped porous carbon material is obviously improved. The specific surface area of the nitrogen-doped porous carbon material prepared in example 3 is 1497m 2 And/g, the specific surface area of the nitrogen-doped porous carbon material is further improved along with the increase of the using amount of potassium oxamate.
The nitrogen-doped porous carbon material prepared in the embodiment 1-3 is subjected to a carbon dioxide adsorption characteristic test, which comprises the following steps:
adding 100mg of nitrogen-doped porous carbon material into a test sample chamber, heating to 250 ℃, and carrying out vacuum degassing treatment for 3 h;
setting the environment temperature of the test sample chamber, gradually increasing the carbon dioxide pressure from a vacuum state, and measuring the adsorption capacity under each equilibrium pressure until the equilibrium pressure reaches 1.0-1.1 bar, so as to obtain a complete carbon dioxide adsorption isotherm;
after the carbon dioxide adsorption test is finished, the sample chamber is heated to 100 ℃ for vacuum treatment, and carbon dioxide desorption is finished.
CO 2 The results of the adsorption tests are shown in FIG. 5. from FIG. 5, it can be seen that the CO of examples 1-3 was obtained at 25 ℃ and 1bar pressure 2 The adsorption capacity is respectively 3.15mmol/g, 3.78mmol/g and 3.91 mmol/g; when the test temperature is 0 ℃, the corresponding CO 2 The adsorption amounts were 4.25mmol/g, 5.49mmol/g, and 6.00mmol/g, respectively. Especially the nitrogen doped porous carbon material of example 3 exhibited a higher adsorption capacity. The test results show that potassium oxamate is used as an activator, and a biomass material is used as a carbon source, so that excellent CO can be conveniently synthesized 2 Nitrogen with adsorption capacity is doped into the porous carbon material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a nitrogen-doped porous carbon material is characterized by comprising the following steps:
carbonizing the biomass material to obtain a carbon source;
mixing the carbon source and the potassium oxamate aqueous solution, and drying to obtain a mixture;
and carrying out heat treatment on the mixture under the protective atmosphere to obtain the nitrogen-doped porous carbon material.
2. The method of claim 1, wherein the biomass material comprises one or more of glucose, sucrose, starch, lignin, and cellulose.
3. The production method according to claim 1 or 2, characterized in that the carbonization treatment is hydrothermal carbonization or high-temperature carbonization;
the temperature of the hydrothermal carbonization is 160-220 ℃, and the heat preservation time of the hydrothermal carbonization is 1-6 h;
the temperature of the high-temperature carbonization is 400-600 ℃, and the heat preservation time of the high-temperature carbonization is 1-2 h.
4. The preparation method according to claim 1, wherein the mass ratio of the carbon source to the potassium oxamate in the potassium oxamate aqueous solution is 1: 1-5.
5. The method according to claim 1, wherein the heat treatment temperature is 600 to 900 ℃; the heat preservation time of the heat treatment is 1-2 h.
6. The method according to claim 1 or 5, wherein a temperature rise rate from room temperature to the temperature of the heat treatment is 1 to 15 ℃/min.
7. The method according to claim 1, wherein the heat treatment further comprises washing and drying in this order.
8. The nitrogen-doped porous carbon material prepared by the preparation method of any one of claims 1 to 7.
9. The nitrogen-doped porous carbon material according to claim 8, wherein the specific surface area of the nitrogen-doped porous carbon material is 600-1500 m 2 The nitrogen content is 2.00-3.50 wt%.
10. Use of the nitrogen-doped porous carbon material according to any one of claims 8 to 9 for adsorbing CO 2 The use of (1).
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Cited By (2)
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| CN115518618A (en) * | 2022-11-02 | 2022-12-27 | 江西省科学院应用化学研究所 | Nitrogen-doped porous carbon material and preparation method and application thereof |
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