CN109665525B - Preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon - Google Patents
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Abstract
The invention provides a preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon, which comprises the steps of preparing a hydrothermal carbon sample by taking a carbon source, an iron-nitrogen dopant and a surfactant as raw materials; and then carrying out high-temperature carbonization treatment and chemical activation treatment in the protective gas atmosphere to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon. The dumbbell-shaped iron-nitrogen double-doped porous carbon prepared by the method has the advantages of high conductivity, adjustable specific surface area and pore volume, controllable iron-nitrogen content and the like, and is beneficial to realizing optimization of physical and chemical properties by regulating and controlling the structure of the dumbbell-shaped iron-nitrogen double-doped porous carbon. The dumbbell-shaped iron-nitrogen double-doped porous carbon prepared by the method has potential application values in the fields of electrode materials, separation, adsorption, sensing, catalyst carriers, gas storage and the like, and can greatly promote the rapid development of novel carbon nano materials in China.
Description
Technical Field
The invention relates to the field of carbon material preparation, and particularly relates to a preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon.
Background
The porous carbon material has the characteristics of low cost, large specific surface area, developed pore structure, acid and alkali resistance, corrosion resistance, good stability, excellent conductivity, adjustable pore diameter and the like, and is widely applied to the aspects of macromolecule separation, adsorption, photoelectric micro-devices and the like. In addition to the above properties, porous carbon materials also show attractive prospects in the fields of supercapacitors, lithium ion batteries, lithium sulfur batteries, fuel cells and the like.
At present, methods for synthesizing porous carbon materials mainly include a hard template method, an assembly method, a hydrothermal method, and the like. The hard template method generally adopts a method of coating a hard template (such as silicon oxide, magnesium oxide and the like) with a carbon source and removing the hard template after carbonization to prepare the porous carbon material, but the method has complex process, higher cost, long manufacturing period and difficult large-scale production, and the hard template method has higher requirements on a precursor and the template. The method for preparing the porous carbon material by the assembly method is a method for synthesizing the porous carbon material by guiding a soluble pore-forming agent. The method saves the step of preparing the hard template, is more economic and reasonable, and is green and environment-friendly. At present, the method mainly takes resin formed by catalytic reaction of phenol and formaldehyde as a precursor, and obtains the porous carbon material through subsequent heat treatment. At present, most of monocyclic phenol and synthetic resin thereof are used as pore-forming agents, so that various properties of the prepared material are greatly limited, and the properties of the obtained carbon material cannot meet the application requirements easily. The hydrothermal method is a method of adding water to a sealed container under high temperature and high pressure to cause the reactants to chemically react therein to obtain a carbon material. Compared with the traditional preparation method, the hydrothermal method is green, environment-friendly, mild and fast, and the preparation process of the method reflects the ideas of green, environment-friendly and sustainable development of chemical preparation materials.
Researches show that the activation and doping modification of the carbon material can further improve the performance of the carbon material in various aspects. Methods for activating carbon materials are mainly divided into two main categories: physical activation methods and chemical activation methods. The physical activation is to utilize oxidizing gases such as air, carbon dioxide, water vapor and the like to react with carbon atoms in the carbon material at high temperature; chemical activation is by chemical agents such as ZnCl2、KOH、H3PO4And NH4NO3And the carbon material are subjected to a series of crosslinking or polycondensation reactions, so that rich pores are created. The water vapor activation speed is high, but the high specific surface area activated carbon is difficult to obtain; activated carbon with high specific surface area can be obtained by adopting carbon dioxide activation, but the activation temperature is high, the activation speed is low, so that the energy consumption is very high, and the activation time usually needs tens of hours or even hundreds of hours. The chemical activation has the advantages of short activation time, low activation temperature and favorable obtainment of specific surface areaHigher carbon materials; in particular ammonium salts (e.g. NH)4NO3Etc.) can be completely decomposed without impurity removal, the pore size of the carbon material can be effectively controlled, the reaction temperature can be reduced, the electric energy can be saved, and the safety can be improved. The carbon skeleton is doped with the hetero element (such as N, P, S, B, Fe) so as to obviously improve the surface properties of the carbon material, such as improving the wettability, the conductivity, the electrocatalytic performance and the like, and the carbon skeleton can also be used as an active site of reaction in electrochemistry. Moreover, compared with single-element doping, multi-element doping has more remarkable advantages in the aspect of improving the performance of the porous carbon material in recent years.
In addition, the most important problem faced in the field of porous carbon materials is how to meet the large-scale industrialization requirement, and on the other hand, as a novel material, the material plays an important role in the field of catalysis and plays an important role in realizing green production in industry.
Disclosure of Invention
The invention provides a preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon, which is simple in method and low in cost and can realize industrial production.
The technical scheme for realizing the invention is as follows:
a preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon comprises the following steps:
(1) dissolving a carbon source, an iron nitrogen dopant and a surfactant with deionized water, stirring, putting into an ultrasonic cleaner for ultrasonic treatment, transferring into a hydrothermal reaction kettle for hydrothermal reaction, cooling to room temperature, filtering and washing the obtained material with deionized water to be neutral, and putting into a drying oven for drying to obtain a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment in a protective gas atmosphere to obtain an iron-nitrogen double-doped carbon sample;
(3) and (3) uniformly mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with an activating agent, adding alcohol and water with the same volume, dissolving, putting into an oven for drying, calcining the dried product in a nitrogen gas atmosphere, taking out, washing with deionized water, and drying in the oven to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
In the step (1), the carbon source is glucose, sucrose, glycogen or cellulose, the iron-nitrogen dopant is ammonium ferrous sulfate hexahydrate, and the surfactant is sodium dodecyl benzene sulfonate or sodium dodecyl sulfate; the mass ratio of the carbon source, the iron-nitrogen dopant and the surfactant is (20-30): (1-3): 1.
the stirring time in the step (1) is 10-30min, the stirring speed is 100-; the hydrothermal reaction temperature is 160-190 ℃, the hydrothermal time is 10-15h, the drying temperature is 105 ℃, and the drying time is 6-10 h.
In the step (2), the protective gas is any one of nitrogen, argon or helium with a mass fraction of 99.99%, and the gas inlet flow rate of the protective gas is 100-.
The high-temperature carbonization temperature in the step (2) is 700-900 ℃, the carbonization time is 2-4h, and the temperature rise speed is 3-6 ℃/min.
The mass ratio of the iron-nitrogen double-doped carbon sample to the activating agent in the step (3) is 1: (1-3), the activating agent is ammonium nitrate, ammonium carbonate or ammonium bicarbonate.
In the step (3), the drying temperature is 80-120 ℃, and the drying time is 12-24 h; the calcination temperature is 250-350 ℃, the calcination time is 1-3h, and the temperature rise speed is 2-5 ℃/min.
The invention has the beneficial effects that:
(1) the carbon source, the iron-nitrogen dopant and the surfactant adopted for preparing the dumbbell-shaped iron-nitrogen double-doped porous carbon are easy to obtain, the price is low, and the large-scale production is facilitated;
(2) the preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon has the advantages that the dumbbell-shaped iron-nitrogen double-doped porous carbon is prepared by combining a hydrothermal method, a carbonization method and an activation method, the process and the flow are simple and convenient, the control is easy, the sustainability is high, no acid, alkali and other pollutants are generated in the operation process, and the quality of the obtained product is good;
(3) the dumbbell-shaped iron-nitrogen double-doped porous carbon prepared by the method has the advantages of high conductivity, adjustable specific surface area and pore volume, controllable iron-nitrogen content and the like, and is beneficial to realizing the optimization of physical and chemical properties by regulating and controlling the structure of the dumbbell-shaped iron-nitrogen double-doped porous carbon;
(4) the dumbbell-shaped iron-nitrogen double-doped porous carbon prepared by the method has potential application values in the fields of electrode materials, separation, adsorption, sensing, catalyst carriers, gas storage and the like, and can greatly promote the rapid development of novel carbon nano materials in China.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of "dumbbell" type iron-nitrogen double doped porous carbon obtained in example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of "dumbbell" type iron-nitrogen double doped porous carbon obtained in example 1 of the present invention;
FIG. 3 is an XRD pattern of "dumbbell" type iron-nitrogen double doped porous carbon obtained in example 1 of the present invention;
FIG. 4 is a Raman spectrum of "dumbbell" type Fe-N double doped porous carbon obtained in example 1 of the present invention;
FIG. 5 is an XPS plot of "dumbbell" type Fe-N double doped porous carbon obtained in example 1 of the present invention;
FIG. 6 is a high resolution XPS plot of Fe 2p of "dumbbell" type Fe-N double doped porous carbon obtained in example 1 of the present invention;
fig. 7 is a high resolution XPS plot of N1 s from "dumbbell" fe-N double doped porous carbon obtained in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon comprises the following steps:
(1) and (2) mixing the following components in percentage by mass: 1: dissolving glucose, ammonium ferrous sulfate hexahydrate and sodium dodecyl benzene sulfonate of 1 in deionized water, stirring on a magnetic stirrer for 10min at a stirring speed of 200r/min, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for 1h at an ultrasonic power of 100W, transferring the mixture into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at a hydrothermal reaction temperature of 180 ℃ for 15h, cooling to room temperature, filtering and washing the obtained material to be neutral by using deionized water, putting the obtained material into an oven for drying at a drying temperature of 105 ℃ for 6h, and obtaining a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample obtained in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment in nitrogen with the mass fraction of 99.99%, wherein the gas inflow is 100sccm, the carbonization temperature is 800 ℃, the carbonization time is 4h, and the temperature rise speed is 3 ℃/min to obtain an iron-nitrogen double-doped carbon sample;
(3) mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with ammonium nitrate according to the mass ratio of 1: 1, adding alcohol and water with the same volume, dissolving, then placing the mixture into an oven for drying at the drying temperature of 80 ℃ for 24 hours, then calcining the dried product in a nitrogen gas atmosphere at the calcining temperature of 250 ℃ for 3 hours at the heating speed of 2 ℃/min, taking out the calcined product, washing the calcined product with deionized water, and drying the calcined product in the oven for 12 hours at the temperature of 120 ℃ to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
Fig. 1 and 2 are scanning electron microscope images and transmission electron microscope images of the prepared "dumbbell" type iron-nitrogen double doped porous carbon, and we can clearly see that the obtained sample is a typical "dumbbell" type structure carbon sphere, and the diameter of the sphere is about hundreds of nanometers. Two less obvious diffraction peaks can be seen in the XRD chart of fig. 3, corresponding to the (002) and (100) crystal planes of graphite respectively, which illustrates that the sample is mainly amorphous structure and has a low graphitization degree; the existence of the D peak in fig. 4 indicates that the obtained "dumbbell-shaped" iron-nitrogen double-doped porous carbon has some defects on the surface, which may be caused by the pores and functional groups on the surface of the carbon material; the existence of the G peak indicates that the obtained dumbbell-shaped iron-nitrogen double-doped porous carbon has good conductivity, and the peak value of the G peak is larger than the D peak, which indicates that the dumbbell-shaped iron-nitrogen double-doped porous carbon has a certain graphitization degree. Fig. 5 is an XPS plot of the resulting "dumbbell" iron-nitrogen double doped porous carbon, fig. 6 and 7 are high resolution XPS plots of the corresponding Fe 2p and N1 s, respectively, indicating that we doped iron and nitrogen elements into the carbon sample and measured atomic percentages of C, O, Fe, N as 80.92, 18.01, 0.15 and 0.91at%, respectively. In conclusion, the dumbbell-shaped iron-nitrogen double-doped porous carbon material is successfully prepared.
Example 2
A preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon comprises the following steps:
(1) and (2) mixing the components in a mass ratio of 25: 2: dissolving sucrose, ammonium ferrous sulfate hexahydrate and sodium dodecyl sulfate of 1 in deionized water, stirring on a magnetic stirrer for 20min at a stirring speed of 150r/min, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for 2h at an ultrasonic power of 150W, transferring the mixture into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at a hydrothermal reaction temperature of 180 ℃ for 13h, cooling to room temperature, filtering and washing the obtained material to be neutral by using deionized water, drying in an oven at a drying temperature of 105 ℃ for 8h to obtain a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample obtained in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment on 99.99% helium gas by mass, wherein the gas inflow is 200sccm, the carbonization temperature is 800 ℃, the carbonization time is 3h, and the temperature rise speed is 5 ℃/min to obtain an iron-nitrogen double-doped carbon sample;
(3) mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with ammonium carbonate according to the mass ratio of 1: 2, uniformly mixing, adding alcohol and water with the same volume, dissolving, then placing into an oven for drying at the drying temperature of 100 ℃ for 18h, then calcining the dried product in the nitrogen atmosphere at the calcining temperature of 300 ℃ for 2h at the heating speed of 3 ℃/min, taking out, washing with deionized water, and drying in the oven at the temperature of 100 ℃ for 16h to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
Example 3
A preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon comprises the following steps:
(1) and (3) mixing the following components in percentage by mass: 3: 1, dissolving glycogen, ammonium ferrous sulfate hexahydrate and sodium dodecyl sulfate by using deionized water, stirring on a magnetic stirrer for 30min at the stirring speed of 100r/min, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for 3h at the ultrasonic power of 300W, transferring the mixture into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the hydrothermal reaction temperature of 190 ℃ for 10h, cooling to room temperature, filtering and washing the obtained material to be neutral by using the deionized water, drying in an oven at the drying temperature of 105 ℃ for 10h to obtain a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample obtained in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment in argon with the mass fraction of 99.99%, wherein the gas inflow is 400sccm, the carbonization temperature is 900 ℃, the carbonization time is 2h, and the temperature rise speed is 6 ℃/min to obtain an iron-nitrogen double-doped carbon sample;
(3) mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with ammonium bicarbonate according to a mass ratio of 1: 3, uniformly mixing, adding alcohol and water with the same volume, dissolving, then placing into an oven for drying at the drying temperature of 120 ℃ for 12h, then calcining the dried product in the nitrogen atmosphere at the calcining temperature of 350 ℃ for 1h at the heating speed of 5 ℃/min, taking out, washing with deionized water, and drying in the oven for 24h at the temperature of 80 ℃ to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
Example 4
A preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon comprises the following steps:
(1) and (2) mixing the components in a mass ratio of 25: 2: dissolving cellulose, ammonium ferrous sulfate hexahydrate and sodium dodecyl sulfate of 1 in deionized water, stirring on a magnetic stirrer for 25min at a stirring speed of 150r/min, putting the mixture into an ultrasonic cleaner for ultrasonic treatment for 2h at an ultrasonic power of 200W, transferring the mixture into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at a hydrothermal reaction temperature of 160 ℃ for 14h, cooling to room temperature, filtering and washing the obtained material to be neutral by using deionized water, putting the obtained material into an oven for drying at a drying temperature of 105 ℃ for 8h, and obtaining a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample obtained in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment in nitrogen with the mass fraction of 99.99%, wherein the gas inflow is 200sccm, the carbonization temperature is 700 ℃, the carbonization time is 3h, and the temperature rise speed is 4 ℃/min to obtain an iron-nitrogen double-doped carbon sample;
(3) mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with ammonium carbonate according to the mass ratio of 1: 2, uniformly mixing, adding alcohol and water with the same volume, dissolving, then placing into an oven for drying at the drying temperature of 100 ℃ for 18h, then calcining the dried product in a nitrogen gas atmosphere at the calcining temperature of 300 ℃ for 2h at the heating speed of 4 ℃/min, taking out, washing with deionized water, and drying in the oven at the temperature of 120 ℃ for 12h to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon is characterized by comprising the following steps:
(1) dissolving a carbon source, an iron nitrogen dopant and a surfactant in deionized water, wherein the iron nitrogen dopant is ammonium ferrous sulfate hexahydrate, stirring, putting into an ultrasonic cleaner for ultrasonic treatment, transferring into a hydrothermal reaction kettle for hydrothermal reaction, cooling to room temperature, filtering and washing the obtained material to be neutral by using deionized water, putting into an oven for drying, and obtaining a hydrothermal carbon sample;
(2) putting the hydrothermal carbon sample in the step (1) into a tubular furnace, and carrying out high-temperature carbonization treatment in a protective gas atmosphere to obtain an iron-nitrogen double-doped carbon sample;
(3) and (3) uniformly mixing the iron-nitrogen double-doped carbon sample obtained in the step (2) with an activating agent, adding alcohol and water with the same volume, dissolving, putting into an oven for drying, calcining the dried product in a nitrogen gas atmosphere, taking out, washing with deionized water, and drying in the oven to obtain the dumbbell-shaped iron-nitrogen double-doped porous carbon.
2. The preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: in the step (1), the carbon source is glucose, sucrose, glycogen or cellulose, and the surfactant is sodium dodecyl benzene sulfonate or sodium dodecyl sulfonate; the mass ratio of the carbon source, the iron-nitrogen dopant and the surfactant is (20-30): (1-3): 1.
3. the preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: the stirring time in the step (1) is 10-30min, the stirring speed is 100-; the hydrothermal reaction temperature is 160-190 ℃, the hydrothermal time is 10-15h, the drying temperature is 105 ℃, and the drying time is 6-10 h.
4. The preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: in the step (2), the protective gas is any one of nitrogen, argon or helium with a mass fraction of 99.99%, and the gas inlet flow rate of the protective gas is 100-.
5. The preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: the high-temperature carbonization temperature in the step (2) is 700-900 ℃, the carbonization time is 2-4h, and the temperature rise speed is 3-6 ℃/min.
6. The preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: the mass ratio of the iron-nitrogen double-doped carbon sample to the activating agent in the step (3) is 1: (1-3), the activating agent is ammonium nitrate, ammonium carbonate or ammonium bicarbonate.
7. The preparation method of the dumbbell-shaped iron-nitrogen double-doped porous carbon according to claim 1, which is characterized in that: in the step (3), the drying temperature is 80-120 ℃, and the drying time is 12-24 h; the calcination temperature is 250-350 ℃, the calcination time is 1-3h, and the temperature rise speed is 2-5 ℃/min.
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