CN109292774B - Preparation method and application of pomegranate-shaped porous carbon microsphere material - Google Patents
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method and application of a pomegranate-shaped porous carbon microsphere material, and relates to the technical field of nano materials and electrochemical devices. The synthesized polymer resin spheres are self-assembled into pomegranate-shaped micro spheres under the promotion of capillary force through a spray drying process, and the pomegranate-shaped porous micro carbon spheres with high specific surface area are obtained through later carbonization and activation, so that the pomegranate-shaped porous micro carbon spheres have high energy density performance, the capacitance is greatly improved, and in 6M KOH solution, 1A g‑1At a current density of 382F g‑1Specific mass capacity of 312F cm‑3Volume to capacity of (a). At a temperature of up to 50A g‑1Can be maintained even at 298F g‑1Has a specific mass capacity of 228F cm‑3Volume to capacity of (a). The method has the advantages of simple and efficient preparation, short time consumption, effective reduction of production cost and suitability for large-scale production.
Description
Technical Field
The invention relates to the technical field of nano materials and electrochemical devices, in particular to a preparation method and application of a pomegranate-shaped porous carbon microsphere material.
Background
Carbon spheres are widely studied because of their excellent structural stability, regular geometric configuration, and simple production process. At present, in commercial supercapacitor preparation, a carbon material is used as an electrode material in 80 percent, and nanocrystallization research and production are focused, but the problem of agglomeration of the material caused by a nanometer effect is particularly serious, and the application of the carbon material in the supercapacitor is directly restricted by the problems that the specific capacity is influenced by the violent reduction of tap density caused by size reduction and the like.
Chinese patent (application publication No. CN107731557A) discloses a preparation method and application of an electrode nitrogen-oxygen co-doped porous carbon and ferroferric oxide composite material for a supercapacitor. The composite material contains four elements of Fe, N, C and O, cyclopentadienyl iron, iron powder, hexachlorobutadiene and pyridine are weighed and added into a high-temperature reaction kettle, the high-temperature reaction kettle is placed into an oven to react for 4 to 20 hours, a dried semi-finished product is placed into a liner of a polytetrafluoroethylene reaction kettle, a saturated urea solution is added into the dried semi-finished product, the high-temperature reaction kettle is placed into the oven to react for 6 to 20 hours after being sealed, the high-temperature reaction kettle is naturally cooled, centrifugally separated, dried and then taken outMeasuring the prepared sample into a porcelain boat, placing the porcelain boat in the middle part of a quartz tube of a tube furnace, introducing argon for 30min, carrying out heating reaction, and maintaining for about 60-12min to obtain the nitrogen-oxygen co-doped porous carbon/ferroferric oxide composite material for the electrode of the supercapacitor, wherein the specific surface area of the treated sample is 814.1m at most2The capacitance value is 201.3F/g at most. The preparation method is complex and takes long time, and the specific surface area and the capacitance value of the obtained product are low, so that the requirement of excellent electrode performance of the super capacitor cannot be met.
Therefore, the nano porous carbon material with high electrical property is prepared by a method with relatively simple and efficient process, and has good application prospect in the aspects of super capacitors and the like.
Disclosure of Invention
The invention provides a preparation method of a pomegranate-shaped porous carbon microsphere material, wherein a spray drying process is adopted to self-assemble synthesized polymer resin spheres into pomegranate-shaped microspheres under the promotion of capillary force, and the pomegranate-shaped porous carbon microspheres with high specific surface area are obtained through later carbonization and activation, so that the pomegranate-shaped porous carbon microsphere material has high energy density performance, greatly improves capacitance, is simple and efficient to prepare, can effectively reduce production cost, and can be prepared in large quantities.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a pomegranate-shaped porous carbon microsphere material comprises the following steps:
(1) dissolving m-aminophenol in deionized water, adding a formaldehyde solution, mixing and stirring to form a milky white solution;
(2) feeding the solution obtained in the step (1) into a pressure spray dryer, and performing spray drying to obtain a powder sample;
(3) sintering and carbonizing the powder sample obtained in the step (2) in an inert atmosphere to obtain a precursor;
(4) mixing the precursor obtained in the step (3) with potassium hydroxide, and activating in an inert atmosphere;
(5) and (4) centrifugally washing and drying the mixture obtained in the step (4) to obtain the pomegranate-shaped porous carbon microsphere material.
According to the scheme, the mass concentration of the formaldehyde solution in the step (1) is 37%, the using amount is 0.5-3.5ml, the amount of m-aminophenol is 0.5-2.5g, and the amount of deionized water is 50-250 ml.
According to the scheme, the sample injection rate in the step (2) is 1-2ml/min, and the drying temperature is 120-150 ℃.
According to the scheme, the spraying pressure in the step (2) is 5-16 MPa.
According to the scheme, the sintering carbonization temperature in the step (3) is 500 ℃, and the sintering carbonization time is 2 hours.
According to the scheme, the mass ratio of the precursor to the potassium hydroxide in the step (4) is 1: 3.
according to the above scheme, the activation temperature in the step (4) is 700 ℃ and the activation time is 2 hours.
According to the scheme, the pomegranate-shaped porous carbon microspheres are formed by agglomeration of porous carbon microspheres, the diameters of the porous carbon microspheres are 200nm, and the diameters of the pomegranate-shaped porous carbon microspheres are 1-10 μm.
The method for preparing the super-capacitor electrode by using the pomegranate-shaped porous carbon microsphere material comprises the following steps:
(1) weighing a pomegranate-shaped porous carbon material for a super capacitor electrode and acetylene black: the mass ratio of the polytetrafluoroethylene is as follows: 8.8:1:0.2, putting into a mortar, adding ethanol, and uniformly mixing.
(2) And (2) drying the mixture obtained in the step (1) at 100 ℃ for 15min, tabletting for 1min under the pressure of 10MPa, and weighing to obtain the super-capacitor electrode.
The action mechanism of the invention is as follows:
the invention forms phenolic resin balls by condensation reaction of m-aminophenol and formaldehyde, because m-aminophenol has an amino radical ion group, the invention has catalytic acceleration effect, the reaction can be completed in about 10 minutes, and nitrogen atoms are introduced into the raw materials, because the electron affinity of the nitrogen atoms is stronger, the polarity of the porous carbon material can be changed, meanwhile, the lone pair electron pair of the nitrogen atoms can be conjugated with the carbon material to obtain a large pi bond, and then the electrochemistry and the catalytic performance of the porous carbon material are improved; the reaction system does not need additional ammonia water additives, ethanol and other organic solvents, and greatly simplifies the reaction process.
Spray drying is carried out to the phenolic resin bobble that will obtain, the resin bobble is self-assembling under the promotion of capillary force, form a size discrepancy but the very high pomegranate form structure spheroid of sphericity, obtain pomegranate form carbon ball precursor through sintering carbonization again, add potassium hydroxide and precursor mixed activation, under the activation, pomegranate form structure carbon ball produces a large amount of micropores, the reunion of earlier stage is piled up simultaneously and has also formed a large amount of holes of piling up, both combine to form a pomegranate form porous carbon ball structure that has high specific surface area, a large amount of pore structure effectively promote the quick transmission of electrolyte ion, promote electrochemical reaction rate greatly.
The phenolic polymer formed in the phenolic reaction contains three elements of carbon, oxygen and nitrogen, in the later carbonization and activation process, a functional group containing hydrogen is removed, the nitrogen and the oxygen are doped between carbon-carbon bonds of the formed porous carbon material in the form of heteroatoms, in addition, the activation of potassium hydroxide is to etch part of the carbon elements through oxidation to achieve the purpose of pore-forming, in the process, part of the oxygen of the potassium hydroxide is doped in a carbon material skeleton, and the uniform distribution of the three elements of carbon, nitrogen and oxygen in the whole sphere can be seen from an electronic energy spectrum, so that the porous carbon material has more active sites and higher conductivity, is combined with a rich microporous structure, and has outstanding electrical properties.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the synthesized polymer nanospheres are self-assembled into pomegranate-shaped microspheres under the promotion of capillary force by a spray drying process, so that the problem of long preparation time of ball milling and other processes commonly used in the prior art is solved, the obtained carbon material has smaller size, and a large number of microporous pomegranate-shaped microsphere structures obtained by agglomeration have stronger conductivity.
(2) The material prepared by the invention has high specific surface area and abundant micropore structures, carbon, nitrogen and oxygen active molecules are uniformly distributed on the sphere, the electrochemical performance is outstanding, the unit energy density can be effectively improved, and the capacitance is greatly improved.
(3) The invention has the advantages of simple raw material preparation, greatly simplified process, short time consumption and low cost, and is suitable for large-scale production.
(4) The process product has wide application, can be used for developing a super capacitor, and can be used for synthesizing other various types of materials with macroporous hollow structures by mixing other materials to serve as a soft template for pore forming.
Drawings
Fig. 1 is a diagram showing a mechanism of forming a porous carbon sphere having a pomegranate-like structure according to example 1 of the present invention;
fig. 2 is an SEM image of a pomegranate-structured porous carbon sphere precursor according to example 1 of the present invention;
FIG. 3 is SEM, TEM and EDS images of pomegranate-structured porous carbon spheres of example 1 of the present invention;
fig. 4 is a raman and XRD pattern of the pomegranate-structured porous carbon spheres of example 1 of the present invention;
FIG. 5 is a drawing showing nitrogen desorption and a pore size distribution of the pomegranate-shaped porous carbon spheres of example 1 of the present invention;
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
(1) weighing 1.5g of m-aminophenol, adding 1.52m l of 37 wt% formaldehyde solution and 150ml of deionized water, mixing and stirring for ten minutes to form milky white solution;
(2) carrying out sample injection on the solution obtained in the step (1) through a peristaltic pump to start spray drying to obtain a powder sample, wherein the sample injection rate of the peristaltic pump is 1.5ml/min, and the drying temperature is 120 ℃;
(3) sintering and carbonizing the powder sample obtained in the step (2) for 2 hours in an inert atmosphere to obtain a precursor, wherein the sintering temperature is 500 ℃;
(4) mixing the precursor obtained in the step (3) with potassium hydroxide, and activating for 2 hours in an inert atmosphere, wherein the mass ratio of the precursor potassium hydroxide is 1:3, and the activation temperature is 700 ℃;
(5) and (4) centrifugally washing and drying the mixture obtained in the step (4) to obtain the pomegranate-shaped porous carbon microsphere material.
As shown in the process schematic diagram of fig. 1, m-aminophenol and formaldehyde are subjected to a phenolic condensation reaction to obtain a plurality of small-size phenolic resin spheres, the small-size phenolic resin spheres are subjected to spray drying and agglomeration to form pomegranate-shaped spheres, and then the pomegranate-shaped spheres are carbonized to obtain a pomegranate-shaped carbon sphere precursor, and the pomegranate-shaped porous carbon microspheres are formed through activation.
As shown in figure 2, the SEM image of the spray dried polymer, the spray dried agglomerate spheres were pomegranate shaped spheres of varying sizes but with particularly high sphericity.
As shown in fig. 3, which is a structural and elemental characterization diagram after carbonization and activation treatment, wherein SEM images a and b show that the polymer has a tendency to shrink in size during carbonization, so that the obtained pomegranate-shaped microspheres collapse to some extent, but still maintain an intact morphology; as seen in a TEM perspective view C, the solid sphere is a solid sphere with accumulation holes, and the accumulation holes are abundant, so that the rapid transmission of electrolyte ions is facilitated, and the electrochemical reaction rate is greatly improved; as can be seen in an EDS electron energy spectrum d, the three elements of carbon, nitrogen and oxygen are uniformly distributed in the whole sphere and have rich active sites.
As shown in a Raman analysis spectrogram of FIG. 4a, the material of the invention obtains relatively obvious D peak and G peak, the peak intensity ratio is about 1, which indicates that the material is a carbon material with more defects, can expose more active sites and is beneficial to improving the specific capacity. As shown in the XRD pattern of fig. 4b, two broadened diffraction peaks appeared at the 002 and 100 crystal planes in the X-ray diffraction test, indicating that the degree of crystallinity of carbon is low, and it is amorphous carbon.
As shown in fig. 5, this is a nitrogen desorption diagram and a pore size distribution diagram of a porous carbon sphere with a pomegranate-like structure, wherein a low-temperature nitrogen desorption test is performed on the carbon sphere to obtain a type i desorption curve, which is a typical microporous porous carbon material, and has a specific surface area of up to 1400 square meters per gram, and the fitted pore size distribution also verifies the guess of the existence of a large number of micropores.
Example 2:
(1) weighing 2.5g of m-aminophenol, adding 3.3m l of 37 wt% formaldehyde solution and 250m l of deionized water, mixing and stirring for ten minutes to form milky white solution;
(2) carrying out sample injection on the solution obtained in the step (1) through a peristaltic pump to start spray drying to obtain a powder sample, wherein the sample injection rate of the peristaltic pump is 2ml/min, and the drying temperature is 140 ℃;
(3) sintering and carbonizing the powder sample obtained in the step (2) for 2 hours in an inert atmosphere to obtain a precursor, wherein the sintering temperature is 500 ℃;
(4) mixing the precursor obtained in the step (3) with potassium hydroxide, and activating for 2 hours in an inert atmosphere, wherein the mass ratio of the precursor potassium hydroxide is 1:3, and the activation temperature is 700 ℃;
(5) and (4) centrifugally washing and drying the mixture obtained in the step (4) to obtain the pomegranate-shaped porous carbon microsphere material.
Example 3:
(1) weighing m-aminophenol, weighing 0.5g, adding 0.8ml of 37 wt% formaldehyde solution and 60ml of deionized water, mixing and stirring for ten minutes to form milky white solution;
(2) carrying out sample injection on the solution obtained in the step (1) through a peristaltic pump to start spray drying to obtain a powder sample, wherein the sample injection rate of the peristaltic pump is 1ml/min, and the drying temperature is 130 ℃;
(3) sintering and carbonizing the powder sample obtained in the step (2) for 2 hours in an inert atmosphere to obtain a precursor, wherein the sintering temperature is 500 ℃;
(4) mixing the precursor obtained in the step (3) with potassium hydroxide, and activating for 2 hours in an inert atmosphere, wherein the mass ratio of the precursor potassium hydroxide is 1:3, and the activation temperature is 700 ℃;
(5) and (4) centrifugally washing and drying the mixture obtained in the step (4) to obtain the pomegranate-shaped porous carbon microsphere material.
Comparative example 1:
this comparative example was prepared according to the process steps of example 1, except that the solution described in step (2) was not spray dried but only dried at 120 ℃ for 1 hour and ball milled to obtain a solid sample, and the remaining process steps were carried out sequentially. The electrochemical performance (electrolyte is 6M KOH) test is shown in tables 1 and 2.
Comparative example 2:
the comparative example is prepared according to the process steps of example 1, but the precursor in the step (3) is not subjected to potassium hydroxide mixing activation treatment, and is directly subjected to centrifugal washing and drying to prepare the pomegranate-shaped carbon material. The electrochemical performance (electrolyte is 6M KOH) test is shown in tables 1 and 2.
Comparative example 3:
4.4g of ethylenediamine, 10.8g of carbon tetrachloride and 1.0g of mesoporous silica SBA-15 template are added and mixed, the mixture is magnetically stirred for two hours, the temperature is raised to 90 ℃, and the mixture is stirred and refluxed for 6 hours. Drying the obtained sample at 100 ℃, then putting the sample into a tubular furnace, heating the sample to 600 ℃ at the heating rate of 5K/min under the nitrogen atmosphere, preserving the heat for 6 hours, cooling and taking out the sample. After the template is removed by 8 percent HF acid, the template is washed by ethanol and water for a plurality of times and filtered and separated. And finally drying in the air at 100 ℃ to obtain the ordered mesoporous carbonitride. Mixing the prepared ordered mesoporous carbon nitrogen material with potassium hydroxide according to the mass ratio of 1:3, fully stirring and uniformly mixing in an aqueous solution, drying, then placing a sample in a tubular furnace, heating to 750 ℃ at the speed of 10K/min under the Ar atmosphere, preserving heat for one hour, and naturally cooling to room temperature to obtain the required porous carbon nitrogen material. The electrochemical performance (electrolyte is 6M KOH) test is shown in tables 1 and 2.
The products obtained in examples 1-3 and comparative examples 1-3 were tested for relevant electrical properties, and the prepared materials were mixed with acetylene black: the mass ratio of the polytetrafluoroethylene is as follows: mixing at the ratio of 8.8:1:0.2, adding ethanol into a mortar, uniformly mixing, drying the obtained mixture at 100 ℃ for 15min, tabletting for 1min under the pressure of 10MPa, cutting and selecting the size of 2cm multiplied by 3cm for each material, pressing the material on foamed nickel to obtain a super capacitor electrode plate, soaking the super capacitor electrode plate in 6M KOH solution for 24 hours to perform electrochemical performance test, wherein a working electrode is the prepared electrode plate, a counter electrode is a platinum wire electrode, a reference electrode is a calomel electrode, and the 6M KOH solution is used as electrolyte solution to perform constant current charge and discharge test under different current densities.
TABLE 1.1Ag-1Electrical properties of the electrode material at a current density of
TABLE 2.50Ag-1Electrical properties of the electrode material at a current density of
From the figure, compared with the sample which is not subjected to spray drying in the comparative example 1, the sample which is not subjected to activation treatment in the comparative example 2, the raw material in the comparative example 3 and the sample with different preparation methods, the product has outstanding specific mass capacity and specific volume capacity performance which are higher than those of the comparative example product, and fully shows that the product effectively improves the capacitance performance of the super capacitor and shows good cycling stability.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (10)
1. The preparation method of the pomegranate-shaped porous carbon microsphere material is characterized by comprising the following steps of:
(1) dissolving m-aminophenol in deionized water, adding a formaldehyde solution, mixing and stirring to form a milky white solution, and performing condensation reaction on the m-aminophenol and formaldehyde to form phenolic resin pellets;
(2) feeding the solution obtained in the step (1) into a pressure spray dryer, and performing spray drying to obtain a powder sample;
(3) sintering and carbonizing the powder sample obtained in the step (2) in an inert atmosphere to obtain a precursor;
(4) mixing the precursor obtained in the step (3) with potassium hydroxide, and activating in an inert atmosphere;
(5) and (4) centrifugally washing and drying the mixture obtained in the step (4) to obtain the pomegranate-shaped porous carbon microsphere material.
2. The method for preparing the pomegranate-shaped porous carbon microsphere material according to claim 1, wherein the formaldehyde solution in the step (1) has a mass concentration of 37% and is used in an amount of 0.5-3.5ml, the m-aminophenol is used in an amount of 0.5-2.5g, and the deionized water is used in an amount of 50-250 ml.
3. The method for preparing the pomegranate-shaped porous carbon micron sphere material according to claim 1, wherein the mixing and stirring time in the step (1) is 10 minutes.
4. The method as claimed in claim 1, wherein the sample injection rate in step (2) is 1-2ml/min, and the drying temperature is 120-150 ℃.
5. The method for preparing the pomegranate-shaped porous carbon micron sphere material according to claim 1, wherein the spraying pressure in the step (2) is 0.5 to 1.6 MPa.
6. The method for preparing the pomegranate-shaped porous carbon micron sphere material according to claim 1, wherein the sintering and carbonizing temperature in the step (3) is 500 ℃ and the sintering and carbonizing time is 2 hours.
7. The preparation method of the pomegranate-shaped porous carbon microsphere material according to claim 1, wherein the mass ratio of the precursor to the potassium hydroxide in the step (4) is 1: 3.
8. the method for preparing the pomegranate-shaped porous carbon micron sphere material according to claim 1, wherein the activation temperature in the step (4) is 700 ℃ and the activation time is 2 hours.
9. The method for preparing the pomegranate-shaped porous carbon microsphere material according to claim 1, wherein the pomegranate-shaped porous carbon microsphere is formed by agglomerating porous carbon microspheres, the diameter of the porous carbon microspheres is 200nm, and the diameter of the pomegranate-shaped porous carbon microsphere is 1-10 μm.
10. A preparation method of a super capacitor electrode, which is the pomegranate-shaped porous carbon microsphere material obtained by the preparation method of the pomegranate-shaped porous carbon microsphere material in claim 1, and is characterized by comprising the following steps:
(1) weighing a pomegranate-shaped porous carbon material for a super capacitor electrode and acetylene black: the mass ratio of the polytetrafluoroethylene is as follows: 8.8:1:0.2, putting into a mortar, adding a proper amount of ethanol, and uniformly mixing;
(2) and (2) drying the mixture obtained in the step (1) at 100 ℃ for 15min, tabletting for 1min under the pressure of 10MPa, and weighing to obtain the super-capacitor electrode.
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