CN110577223A - Preparation process of porous carbon nanosphere - Google Patents
Preparation process of porous carbon nanosphere Download PDFInfo
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- CN110577223A CN110577223A CN201911029139.8A CN201911029139A CN110577223A CN 110577223 A CN110577223 A CN 110577223A CN 201911029139 A CN201911029139 A CN 201911029139A CN 110577223 A CN110577223 A CN 110577223A
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- diaminopyridine
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
The invention discloses a preparation process of porous carbon nanospheres, which comprises the following steps: s1 preparation of ZnCl2A solution; s2, ZnCl2Adding 2, 6-diaminopyridine into the solution, and stirring until the 2, 6-diaminopyridine is completely dissolved; s3, adding formaldehyde into the solution prepared in the S2 until the reaction is completed to obtain a solution A; s4, centrifuging the solution A, and drying the centrifugal precipitate to obtain the polytriazine; s5, calcining the polytriazine to obtain a carbonized product B; s6, washing and drying the carbonized product B to obtain a porous carbon nanosphere; wherein: ZnCl2The concentration of the solution is more than 0.5mg/mL and less than 4 mg/mL. The invention is realized by ZnCl with lower concentration2the solution is polymerized with 2, 6-diaminopyridine and formaldehyde to form the polytriazine nanosphereAs a carbon precursor, a carbon precursor containing ZnCl2The polytriazine is carbonized, the carbonization and the foaming process are carried out simultaneously, the polytriazine is converted into the porous carbon nanosphere C-PFZ, the formed C-PFZ has the advantages of no surface collapse, good overall appearance and excellent electrochemical performance as an EDLC electrode.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation process of a porous carbon nanosphere.
background
With the change of electronic information technology, the update speed of digital electronic products is faster and faster, and the growth of capacitor industry is also driven.
the global supercapacitor market has been growing rapidly over the past decade. The activated carbon has low cost, good electrochemical stability, good electronic conductivity and large surface area, and is widely applied to super capacitors. In this case, Porous Carbon Spheres (PCS) combine the advantages of carbon materials with spherical colloids, which gives them some unique functions such as regular geometry, good flowability and adjustable porosity and controllable particle size distribution. A great deal of effort has therefore been invested throughout the electrochemical community in the synthesis of porous carbon nanomaterials for Electric Double Layer Capacitors (EDLCs). It is common to perform chemical activation of porous carbon, which generally refers to the use of ZnCl2And KOH and the like are used for adjusting the pore diameter and the specific surface area of the porous carbon. And ZnCl2The salt template has low cost and less corrosion, and is widely selected as an activator of porous carbon.
In recent years, ZnCl has been used for the preparation of porous materials2The salt template approach includes two strategies: one is by contacting the polymer precursor with supersaturated ZnCl2The solution is mixed to prepare a high-salt solution, the method can play the roles of dehydration, foaming and pore-forming agent, but the overall appearance in the polymerization process has great influence; another method is ZnCl2activation of different carbon precursors of synthetic polymers, biomass or waste, with a small proportion of ZnCl2Acting as a blowing agent and stabilizer during carbonization to induce 3D structure formation, but this method is only applicable to polymer products. For polymer precursors, high salt ZnCl2Conditions which, although giving it greater mechanical strength and avoiding special drying processes, use large amounts of ZnCl2Not only is not beneficial to the large-scale production of porous carbon, but also is easy to damage the integral appearance of the carbon precursor self-assembly, and simultaneously brings serious environmental pollution.
Disclosure of Invention
aiming at the defects of the prior art, the invention aims to provide a preparation process of porous carbon nanospheres, which solves the problem that the porous carbon nanospheres are prepared under the condition of high salt in the prior artlarge amount of ZnCl2Leading to the large scale of porous carbon which easily destroys the integral appearance of the carbon precursor self-assembly and brings serious environmental pollution.
the purpose of the invention can be realized by the following technical scheme:
a preparation process of a porous carbon nanosphere comprises the following steps:
S1, taking ZnCl2Dissolving the solid in deionized water to obtain ZnCl with the concentration of more than 0.5mg/mL and less than 4mg/mL2A solution;
S2, ZnCl2Adding 2, 6-diaminopyridine into the solution, and stirring until the 2, 6-diaminopyridine is completely dissolved;
S3, adding formaldehyde with the mass percent concentration of 37-40% into the solution obtained in the step S2, and stirring at room temperature for 18 hours until the reaction is complete to obtain a solution A;
S4, centrifuging the solution A to obtain a centrifugal precipitate, and drying the centrifugal precipitate to obtain the polytriazine;
S5, calcining the polytriazine at the ambient temperature of 600 ℃ for 5 hours, then heating to 900 ℃ and continuing calcining for 2 hours to obtain a carbonized product B;
and S6, washing and drying the carbonized product B, and then performing Soxhlet extraction for 2d and drying to obtain the porous carbon nanosphere.
Further, ZnCl in the S22the mass ratio of the solid to the 2, 6-diaminopyridine is 1-8: 1.
furthermore, the dosage of the formaldehyde in the S3 is 1.5 multiplied by 10 of the mass of the 2, 6-diaminopyridine-3And (4) doubling.
further, the temperature of the drying in S4 is 60 ℃.
Further, the polytriazine in the S5 is calcined in a nitrogen protection environment.
Further, the temperature increase rate in S5 is 5 ℃/min.
further, the washing of the carbonized product B in S6 is performed by using 1mol/L HCl solution.
Further, the drying temperature of the carbonized product B in the S6 is 80 ℃.
Further, the solvent used in the soxhlet extraction in S6 is water.
the invention has the beneficial effects that:
1. The invention is realized by ZnCl with lower concentration2The solution is polymerized with 2, 6-diaminopyridine and formaldehyde into polytriazine nanospheres as the carbon precursor. Then adding the solution containing ZnCl2the PF (poly-triazine) is carbonized and the carbonization and the foaming process are carried out simultaneously, the PF (poly-triazine) is converted into the porous carbon nanosphere C-PFZ, the surface of the formed C-PFZ is free from collapse, the overall appearance is good, and the formed C-PFZ is used as an EDLC electrode and has excellent electrochemical performance.
2. compared with other salt templates, the method reduces the use amount of inorganic salt, lowers the synthesis cost, and can reduce the pollution to the environment in the synthesis process.
3. Compared with other salt templates, the method can adjust ZnCl under the condition of low salt2Of equivalent concentration of (C) or ZnCl2The mass ratio of the nano-sphere to the 2, 6-diaminopyridine is used for regulating and controlling the shape integrity, the pore structure and the specific surface area of the polymer nano-sphere.
4. the preparation process adopted by the invention has simple procedures, is easy to reproduce and is convenient for industrial production.
Drawings
in order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a high resolution projection electron microscope (HR-Tem) image of various embodiments of the present invention;
FIG. 2 is a graph of adsorption and desorption curves for various embodiments of the present invention;
FIG. 3 is a porous carbon nanosphere pore size distribution plot of embodiments of the present invention;
FIG. 4 is a schematic representation of the specific surface area of various embodiments of the present invention;
FIG. 5 is a process flow diagram of an embodiment of the invention.
Detailed Description
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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:
the embodiment of the invention provides a preparation process of a porous carbon nanosphere, which comprises the following steps:
s1, taking 150mg ZnCl2The solid is dissolved in 300mL of deionized water to obtain ZnCl with the concentration of 0.5mg/mL2A solution;
S2, ZnCl2150mg of 2, 6-diaminopyridine are added to the solution and stirred until completely dissolved (ZnCl)2The mass ratio of the solid to the 2, 6-diaminopyridine is 1: 1);
S3, adding 225uL of formaldehyde with the mass percentage concentration of 37-40% into the solution obtained in the step S2, and stirring at room temperature for 18h until the reaction is complete to obtain a solution A;
s4, centrifuging the solution A to obtain a centrifugal precipitate, collecting the centrifugal precipitate, and drying the centrifugal precipitate in an oven at the temperature of 60 ℃ to obtain the polytriazine;
s5, placing polytriazine in a tube furnace, calcining for 5h at 600 ℃ in a nitrogen environment atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min, continuing calcining for 2h, and carbonizing to obtain a carbonized product B;
s6, washing the carbonized product B by adopting 1mol/L HCl solution, then putting the washed carbonized product B into an oven to be dried at the temperature of 80 ℃, and finally, taking water as a solvent, and carrying out Soxhlet extraction for 2d and then drying to obtain the porous carbon nanosphere.
Example 2:
The embodiment of the invention provides a preparation process of a porous carbon nanosphere, which comprises the following steps:
S1, collecting 300mg ZnCl2The solid is dissolved in 300mL of deionized water to obtain ZnCl with the concentration of 1mg/mL2A solution;
s2, ZnCl2150mg of 2, 6-diaminopyridine are added to the solution and stirred until completely dissolved (ZnCl)2The mass ratio of the solid to the 2, 6-diaminopyridine is 2: 1);
S3, adding 225uL of formaldehyde with the mass percentage concentration of 37-40% into the solution obtained in the step S2, and stirring at room temperature for 18h until the reaction is complete to obtain a solution A;
S4, centrifuging the solution A to obtain a centrifugal precipitate, collecting the centrifugal precipitate, and drying the centrifugal precipitate in an oven at the temperature of 60 ℃ to obtain the polytriazine;
s5, placing polytriazine in a tube furnace, calcining for 5h at 600 ℃ in a nitrogen environment atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min, continuing calcining for 2h, and carbonizing to obtain a carbonized product B;
S6, washing the carbonized product B by adopting 1mol/L HCl solution, then putting the washed carbonized product B into an oven to be dried at the temperature of 80 ℃, and finally, taking water as a solvent, and carrying out Soxhlet extraction for 2d and then drying to obtain the porous carbon nanosphere.
Example 3:
The embodiment of the invention provides a preparation process of a porous carbon nanosphere, which comprises the following steps:
s1, taking 600mg ZnCl2The solid is dissolved in 300mL of deionized water to obtain ZnCl with the concentration of 2mg/mL2A solution;
S2, ZnCl2150mg of 2, 6-diaminopyridine was added to the solution and stirred until completely dissolved (ZnCl)2The mass ratio of the solid to the 2, 6-diaminopyridine is 4: 1);
S3, adding 225uL of formaldehyde with the mass percentage concentration of 37-40% into the solution obtained in the step S2, and stirring at room temperature for 18h until the reaction is complete to obtain a solution A;
S4, centrifuging the solution A to obtain a centrifugal precipitate, collecting the centrifugal precipitate, and drying the centrifugal precipitate in an oven at 60 ℃ to obtain the polytriazine;
s5, placing polytriazine in a tube furnace, calcining for 5h at 600 ℃ in a nitrogen environment atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min, continuing calcining for 2h, and carbonizing to obtain a carbonized product B;
S6, washing the carbonized product B with 1mol/L HCl solution, then drying in an oven at 80 ℃, finally drying by taking water as a solvent and performing Soxhlet extraction for 2d to obtain the porous carbon nanosphere, wherein the projection electron microscope image of the porous carbon nanosphere is shown in figure 1a, and the porous carbon nanosphere has good surface overall appearance and no obvious collapse.
Example 4:
the embodiment of the invention provides a preparation process of a porous carbon nanosphere, which comprises the following steps:
s1, taking 400mg ZnCl2the solid is dissolved in 200mL of deionized water to obtain ZnCl with the concentration of 2mg/mL2a solution;
S2, ZnCl2100mg of 2, 6-diaminopyridine was added to the solution and stirred until completely dissolved (ZnCl)2The mass ratio of the solid to the 2, 6-diaminopyridine is 4: 1);
S3, adding 150uL of formaldehyde with the mass percentage concentration of 37-40% into the solution obtained in the step S2, stirring uniformly, immediately transferring into a high-pressure reaction kettle, placing in a 60 ℃ oven, and reacting for 12 hours until the reaction is complete to obtain a solution A;
S4, centrifuging the solution A to obtain a centrifugal precipitate, collecting the centrifugal precipitate, and drying the centrifugal precipitate in an oven at the temperature of 60 ℃ to obtain the polytriazine;
s5, placing polytriazine in a tube furnace, calcining for 5h at 600 ℃ in a nitrogen environment atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min, continuing calcining for 2h, and carbonizing to obtain a carbonized product B;
S6, washing the carbonized product B with 1mol/L HCl solution, then drying in an oven at 80 ℃, finally drying by taking water as a solvent and performing Soxhlet extraction for 2d to obtain the porous carbon nanosphere, wherein the projection electron microscope image of the porous carbon nanosphere is shown in figure 1B, and the porous carbon nanosphere has good surface overall appearance and no obvious collapse.
Example 5:
The embodiment of the invention provides a preparation process of a porous carbon nanosphere, which comprises the following steps:
s1, taking 1200mg ZnCl2The solid is dissolved in 300mL of deionized water to obtain ZnCl with the concentration of 4mg/mL2a solution;
S2, ZnCl2150mg of 2, 6-diaminopyridine was added to the solution and stirred until completely dissolved (ZnCl)2the mass ratio of the solid to the 2, 6-diaminopyridine is 8: 1);
S3, adding 225uL of formaldehyde into the solution obtained in the S2, and stirring at room temperature for 18h until the reaction is complete to obtain a solution A;
S4, centrifuging the solution A to obtain a centrifugal precipitate, collecting the centrifugal precipitate, and drying the centrifugal precipitate in an oven at the temperature of 60 ℃ to obtain the polytriazine;
S5, placing polytriazine in a tube furnace, calcining for 5 hours at 600 ℃ in a nitrogen environment atmosphere, and then calcining for 2 hours when the temperature is raised to 900 ℃ at the rate of 5 ℃/min for carbonization to obtain a carbonized product B;
S6, washing the carbonized product B with 1mol/L HCl solution, then putting the carbonized product B into an oven to be dried at 80 ℃, finally, taking water as a solvent, and carrying out Soxhlet extraction for 2d and then drying to obtain the porous carbon nanosphere, wherein the projection electron microscopy image of the porous carbon nanosphere is shown in figure 1c, and the surface of the porous carbon nanosphere is obviously collapsed.
as shown in fig. 1, a high resolution projection electron microscope (HR-Tem) image of the porous carbon nanosphere obtained in each of the above examples shows that: a. in the b picture, the porous carbon spheres directly carbonized have no surface collapse and have adjustable surface area and reasonable pore structure; and c, the surface of the carbonized porous carbon sphere in the graph has more collapse and poor integral appearance.
as shown in fig. 2, the adsorption/desorption curves of the porous carbon nanospheres of the above examples show that: selected isothermal curves of C-PFZ are shown at P/P0<when the adsorption rate was 0.05, the adsorption was increased stepwise, and the adsorbate was coagulated by capillary action, and the isotherm was rapidly raised.
As shown in fig. 3, the pore size distribution of the porous carbon nanospheres of the above embodiments is shown in the figure: the pore size distribution of C-PFZ confirms the presence of a large number of mesopores (4-40 nm). Introduced ZnCl2the higher the ratio, the more mesopores are produced.
As shown in fig. 4, the pore size distribution of the porous carbon nanospheres of the above embodiments is shown in the figure: can be adjusted by ZnCl2Phase ofWhen concentration is ZnCl2the mass ratio to 2, 6-diaminopyridine is adjusted with ZnCl2The specific surface area of the porous carbon nanoball becomes significantly large as the ratio increases.
In summary, the preparation process of the porous carbon nanosphere provided by the invention is shown in fig. 5, and ZnCl with lower concentration is used2the solution is polymerized with 2, 6-diaminopyridine and formaldehyde into polytriazine nanospheres as the carbon precursor. Then adding the solution containing ZnCl2the PF (polytriazine) is carbonized, the PF can be converted into the porous carbon nanosphere C-PFZ through a direct high-temperature process, the surface of the C-PFZ does not collapse, the overall appearance of the carbon precursor self-assembly is well maintained, and the electrode serving as the EDLC shows excellent electrochemical performance. Compared with other salt templates, the use amount of inorganic salt is reduced, the synthesis cost is reduced, and the pollution to the environment is reduced.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (9)
1. A preparation process of a porous carbon nanosphere is characterized by comprising the following steps:
S1, taking ZnCl2Dissolving the solid in deionized water to obtain a solution with a mass concentration of more than 0.5mg/mL and less than4mg/mL ZnCl2A solution;
S2, ZnCl2adding 2, 6-diaminopyridine into the solution, and stirring until the 2, 6-diaminopyridine is completely dissolved;
s3, adding formaldehyde with the mass percent concentration of 37-40% into the solution obtained in the step S2, and stirring at room temperature for 18 hours until the reaction is complete to obtain a solution A;
s4, centrifuging the solution A to obtain a centrifugal precipitate, and drying the centrifugal precipitate to obtain the polytriazine;
s5, calcining the polytriazine at the ambient temperature of 600 ℃ for 5 hours, and then heating to 900 ℃ to calcine for 2 hours to obtain a carbonized product B;
And S6, washing and drying the carbonized product B, and then performing Soxhlet extraction for 2d and drying to obtain the porous carbon nanosphere.
2. The process for preparing porous carbon nanospheres according to claim 1, wherein ZnCl is present in S22The mass ratio of the solid to the 2, 6-diaminopyridine is 1-8: 1.
3. The process for preparing porous carbon nanospheres according to claim 1, wherein the amount of formaldehyde in S3 is 1.5 x 10 based on the mass of 2, 6-diaminopyridine-3And (4) doubling.
4. the process for preparing a porous carbon nanosphere according to claim 1, wherein the temperature of drying in S4 is 60 ℃.
5. The process for preparing porous carbon nanospheres according to claim 1, wherein the polytriazine in S5 is calcined under a nitrogen atmosphere.
6. The process for preparing a porous carbon nanosphere according to claim 5 wherein the temperature increase rate in S5 is 5 ℃/min.
7. The process for preparing a porous carbon nanosphere according to claim 1, wherein the washing of the carbonized product B in S6 is performed with 1mol/L HCl solution.
8. The process for preparing a porous carbon nanoball according to claim 7, wherein the drying temperature of the carbonized product B in S6 is 80 ℃.
9. The process for preparing a porous carbon nanosphere according to claim 7, wherein the solvent used in the Soxhlet extraction in S6 is water.
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| CN114887397A (en) * | 2022-05-16 | 2022-08-12 | 江苏博同环保科技有限公司 | Durable filter cloth filtering plate capable of being recycled |
| CN115285950A (en) * | 2022-06-14 | 2022-11-04 | 安徽理工大学 | Poly-triazine carbon material and preparation method and application thereof |
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