CN109911880B - Method for preparing nitrogen-containing carbon aerogel through normal-pressure drying in super-salt environment - Google Patents
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Abstract
The invention discloses a method for preparing nitrogen-containing carbon aerogel by normal pressure drying in an ultra-salt environment, and a productThe nitrogen-containing carbon aerogel is prepared by the following method: carrying out hydrothermal reaction on a mixture formed by formaldehyde, zinc chloride, a nitrogen source and phenol for a period of time, cooling to room temperature, and drying an obtained hydrothermal product; and then, preserving the heat for a period of time at a high temperature in an inert gas atmosphere, cooling to room temperature after the reaction is finished, soaking the obtained product in a hydrochloric acid solution, and then filtering, washing and drying by using deionized water to obtain the nitrogen-containing carbon aerogel. The nitrogen-containing carbon aerogel prepared by the invention has a hierarchical porous structure, and the maximum specific surface area can reach 1201.1m2The preparation process is simple, the synthesis period is short, the operation is easy, the cost is low, and the method is suitable for industrial production.
Description
(I) technical field
The invention relates to a method for preparing nitrogen-containing carbon aerogel by normal pressure drying in an ultra-salt environment.
(II) background of the invention
In recent years, carbon aerogel has attracted much attention due to its advantages such as high specific surface area and abundant three-dimensional pores. The carbon aerogel has high conductivity, larger specific surface area and wide pore distribution, and the characteristics make the carbon aerogel become a thermal application material in various fields, such as the sensing and detecting field and the energy storage field. And the carbon aerogel is easy to be functionally modified, so that the application of the carbon aerogel is more abundant, and the carbon aerogel also has the figure in the aspects of seawater desalination, waste oil adsorption and the like. In order to improve the hydrophobic state of the surface of the carbon aerogel, a method of introducing heteroatoms, such as nitrogen, boron and sulfur elements, into a carbon lattice is generally adopted, wherein the periodic table position of the nitrogen element is adjacent to carbon, and the nitrogen element can be effectively incorporated into a carbon skeleton. In the literature, the carbon aerogel needs activation and other steps after nitrogen doping, the preparation process is complicated, and the flow period is long.
On the other hand, the literature reports that the preparation method of the carbon aerogel comprises a sol-gel method, the polymerization and aging time is long, supercritical carbon dioxide drying is generally adopted, and the method is dangerous, high in cost and not suitable for industrial production.
Disclosure of the invention
The invention aims to provide a method for preparing nitrogen-containing carbon aerogel, which has simple process, environmental protection and low cost and is suitable for industrial production.
The technical scheme adopted by the invention is as follows:
a method for preparing a nitrogen-containing carbon aerogel by atmospheric drying in an ultra-salt environment, the method comprising:
(1) adding a nitrogen source, inorganic salt and phenol into formaldehyde under the ice-water bath condition, then carrying out hydrothermal reaction for 5-15 h at 100-180 ℃, and naturally cooling to room temperature; the formaldehyde: nitrogen source: inorganic salts: the ratio of the phenol dosage is 1-5 mL: 0.1-2.0 g: 1-8 g: 0.5-2.0 g;
(2) drying the hydrothermal product obtained in the step (1), preserving the heat for 1-5 hours in inert gas at the temperature of 600-1000 ℃, and cooling to room temperature;
(3) and (3) immersing the product obtained in the step (2) into 1-5M hydrochloric acid solution for 1-2 days, then carrying out suction filtration and washing by using deionized water until the pH value is not changed, and drying to obtain the nitrogen-containing carbon aerogel.
The nitrogen-containing carbon aerogel prepared in the super-salt environment has high mechanical strength and can be directly dried under normal pressure. And the nitrogen-containing carbon aerogel is obtained after carbonization, does not need subsequent treatment such as activation and the like, and is particularly suitable for the fields of supercapacitors, adsorption and the like.
The nitrogen source in the step (1) is one of the following or a mixture of more than two of the following: pyridine, pyrrole, ethylenediamine, polyaniline, m-phenylenediamine, urea, melamine, phenylethanolamine and polynaphthalene diamine. Preferably urea, melamine or ethylenediamine.
In the step (1), the inorganic salt is one of the following or a mixture of two or more of the following: sodium chloride, zinc chloride, calcium chloride, magnesium chloride and potassium chloride. Preferably zinc chloride.
In the step (2), the drying temperature is 80-150 ℃, and the drying time is 12-36 h.
And (3) in the step (2), the inert gas is nitrogen or argon.
The invention has the following beneficial effects:
(1) the invention provides a nitrogen-containing carbon aerogel which can be directly dried under normal pressure, long-time polymerization and aging are not needed, and a nitrogen-containing precursor is obtained after hydrothermal treatment;
(2) the invention provides the nitrogen-containing carbon aerogel which can be directly dried under normal pressure, the steps of drying by supercritical carbon dioxide and the like are not needed, the cost is low, and the equipment requirement is low;
(3) the prepared nitrogen-containing precursor is carbonized to obtain the nitrogen-containing carbon aerogel, a subsequent activation step is not needed, the safety and the high efficiency are realized, the preparation period is short, and the steps and the flows are few;
(4) the prepared nitrogen-containing carbon aerogel has larger specific surface area (reaching 1201.1 m)2(g), lower density;
(5) the preparation process is simple, the synthesis period is saved, the operation is easy, the cost is low, and the method is suitable for industrial production.
(IV) description of the drawings
FIG. 1 is an XRD spectrum of a sample of examples 1-3.
FIG. 2 is an XRD spectrum of a sample of example 4-6.
FIG. 3 is an XRD spectrum of the samples of examples 7-9.
FIG. 4 is a SEM image of a sample of example 2.
FIG. 5 is an adsorption isotherm plot of the sample of example 2.
FIG. 6 is a graph of the pore size distribution of the sample of example 2.
FIG. 7 is a SEM image of a sample of example 5.
FIG. 8 is an adsorption isotherm plot of the sample of example 5.
FIG. 9 is a graph of the pore size distribution of the sample of example 5.
FIG. 10 is a SEM image of a sample of example 9.
FIG. 11 adsorption isotherm plot of the example 9 sample.
FIG. 12 pore size distribution plot for example 9 sample.
Fig. 13 graph of constant current charge and discharge in a three electrode supercapacitor system for the sample of example 9.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of urea were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then N is added at 700 ℃ to2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 1, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 2:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of urea were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, at a temperature of 800 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
The sample prepared in this example had a specific surface area of 828.9m2(ii) in terms of/g. Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 1, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
The morphology of the sample was analyzed using a Hitachi S-4700 II field emission scanning electron microscope, as shown in FIG. 4. As can be seen, the sample had a porous structure.
The nitrogen adsorption/desorption isotherm of the nitrogen adsorption/desorption curve of the sample was measured using a Micromeritics ASAP 2460 instrument, and the adsorption isotherm of the sample is shown in fig. 5; as shown in fig. 6, the pore size distribution of the sample was centered at 1.77 nm.
Example 3:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of urea were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then at 900 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 1, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 4:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of melamine were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then N is added at 700 ℃ to2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 2, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 5:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of melamine were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, at a temperature of 800 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
The sample prepared in this example had a specific surface area of 729.6m2A density of about 0.09g/cm3. Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 2, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
The morphology of the sample was analyzed using a Hitachi S-4700 II field emission scanning electron microscope, as shown in FIG. 7. As can be seen, the sample had a porous structure.
The nitrogen adsorption/desorption isotherm of the nitrogen adsorption/desorption curve of the sample was measured using a Micromeritics ASAP 2460 instrument, and the adsorption isotherm of the sample is shown in fig. 8; as shown in fig. 9, the pore size distribution of the sample was centered at 0.98, 2.13, and 2.38 nm.
Example 6:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.25g of melamine were added to 1.5ml of formaldehyde to give a white viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then at 900 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
Phase analysis of sample was performed using an X-ray diffractometer (X' pertro). In fig. 2, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 7:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.2ml of ethylenediamine were added to 1.5ml of formaldehyde to obtain a pale yellow viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then N is added at 700 ℃ to2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
The sample prepared in this example had a specific surface area of 843.5m2(ii) in terms of/g. Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 3, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 8:
in an ice-water bath 6.5g ZnCl was added20.941g of phenol and 0.2ml of ethylenediamine were added to 1.5ml of formaldehyde to obtain a pale yellow viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, at a temperature of 800 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
The sample prepared in this example had a specific surface area of 921.5m2(ii) in terms of/g. Phase analysis of the sample an X-ray diffractometer (X' PertPRO) was used for phase analysis of the sample. In fig. 3, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
Example 9:
in an ice-water bath 6.5g ZnCl was added20.9g of phenol and 0.2ml of ethylenediamine were added to 1.5ml of formaldehyde to obtain a pale yellow viscous colloid, and the mixture was subjected to hydrothermal reaction at 160 ℃ for 8 hours; the black product obtained is then dried at 135 ℃ for 12 hours, and then at 900 ℃ under N2Preserving the temperature in the atmosphere for 2 hours, naturally cooling to room temperature, immersing the prepared sample in 1M HCl for 48 hours, repeatedly washing with deionized water until the pH value is not changed, and drying the washed product at 80 ℃ to obtain the final product.
The sample prepared in this example had a specific surface area of 1201.1m2A density of about 0.05g/cm3. Phase analysis of sample was performed using an X-ray diffractometer (X' pertro). In fig. 3, it is shown that two diffraction peaks are assigned to the (002) crystal plane and the (100) crystal plane of graphitic carbon.
The morphology of the sample was analyzed using a Hitachi S-4700 II field emission scanning electron microscope, as shown in FIG. 10. As can be seen, the sample had a porous structure.
The nitrogen adsorption/desorption isotherm of the nitrogen adsorption/desorption curve of the sample was measured using a Micromeritics ASAP 2460 instrument, and the adsorption isotherm of the sample is shown in fig. 11; as shown in fig. 12, the pore size distribution of the sample was concentrated at 1.05, 2.13, and 2.38 nm.
As shown in FIG. 13, the constant current charge and discharge curve of the sample in the three-electrode supercapacitor system shows that the specific capacitance of the sample is 426.1F/g at a current density of 1A/g.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for preparing a nitrogen-containing carbon aerogel by atmospheric drying in an ultra-salt environment, the method comprising:
(1) adding a nitrogen source, inorganic salt and phenol into formaldehyde under the ice-water bath condition, then carrying out hydrothermal reaction for 5-15 h at 100-180 ℃, and naturally cooling to room temperature; the formaldehyde: nitrogen source: inorganic salts: the ratio of the phenol dosage is 1-5 mL: 0.1-2.0 g: 1-8 g: 0.5-2.0 g; the inorganic salt is one of the following or a mixture of two or more of the following: sodium chloride, zinc chloride, calcium chloride, magnesium chloride, potassium chloride; the nitrogen source is urea, melamine or ethylenediamine;
(2) drying the hydrothermal product obtained in the step (1), preserving the heat for 1-5 hours in inert gas at the temperature of 600-1000 ℃, and cooling to room temperature;
(3) and (3) immersing the product obtained in the step (2) into 1-5M hydrochloric acid solution for 1-2 days, then carrying out suction filtration and washing by using deionized water until the pH value is not changed, and drying to obtain the nitrogen-containing carbon aerogel.
2. The method of claim 1, wherein in step (1) the inorganic salt is zinc chloride.
3. The method according to claim 1, wherein the drying temperature in step (2) is 80-150 ℃ for 12-36 h.
4. The method of claim 1, wherein the inert gas in step (2) is nitrogen or argon.
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