CN112158837A - High internal phase emulsion template method for preparing and regulating nitrogen/sulfur co-doped porous carbon - Google Patents
High internal phase emulsion template method for preparing and regulating nitrogen/sulfur co-doped porous carbon Download PDFInfo
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- CN112158837A CN112158837A CN202011093560.8A CN202011093560A CN112158837A CN 112158837 A CN112158837 A CN 112158837A CN 202011093560 A CN202011093560 A CN 202011093560A CN 112158837 A CN112158837 A CN 112158837A
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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
- C01B32/318—Preparation characterised by the starting materials
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a method for preparing and regulating a high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon. Firstly, dissolving a surfactant, a monomer and a catalyst in deionized water to obtain a water phase, slowly dropwise adding an oil phase into the water phase under the condition of mechanical stirring to obtain an oil-in-water type high internal phase emulsion, and then carrying out polymerization reaction to obtain a solid massive crude product. Removing the inner phase by Soxhlet extraction and vacuum drying to obtain a porous polymer precursor, and carbonizing and activating to obtain the nitrogen/sulfur co-doped porous carbon material. The invention can effectively regulate and control the porous carbon pore structure and the nitrogen/sulfur content by changing the molar ratio of the melamine to the thiourea. Along with the increase of the content of thiourea, the specific surface area of the prepared porous carbon material is gradually increased, and the specific capacitance of a super container prepared by taking the porous carbon material as an electrode material is also obviously increased. The supercapacitor prepared by taking the prepared nitrogen/sulfur co-doped porous carbon as an electrode material shows good electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of preparation of high polymer materials, and particularly relates to a high internal phase emulsion template method for preparing and regulating nitrogen/sulfur co-doped porous carbon.
Background
The super capacitor is a novel energy storage device with the characteristics of both an electrostatic capacitor and a battery. Compared with conventional energy storage devices, supercapacitors have higher safety, longer cycle life, faster charging/discharging capability and higher power density, and thus have great potential in energy storage devices. The part of the super capacitor which plays a core role is an electrode, and various electrode materials applied to the super capacitor comprise carbon materials, conductive polymers, metal oxides and composite materials thereof. Porous carbon is generally selected as an electrode material because of its wide source, easy availability of high specific surface area and excellent electrical conductivity. However, the electrode material as an electric double layer capacitor cannot satisfy the requirements of high energy and high power density. One of the successful approaches to overcome the disadvantages is to incorporate some heteroatoms into the carbon backbone, which can enhance conductivity. Additional contributions may be generated from the faraday charge transfer reaction that occurs between the heteroatom and the electrolyte. The doping of nitrogen, boron, phosphorus, sulfur and other heteroatoms can improve the electrochemical performance of the carbon material. In addition, co-doping strategies have been further applied to increase the specific capacitance of the material.
Patent CN110538635A discloses the preparation of a nitrogen-sulfur co-doped porous magnetic carbon material, which mainly comprises the following steps: 1) weighing resorcinol and formaldehyde, dissolving in distilled water, stirring the mixed solution at 40-50 deg.C for more than 1h, weighing melamine, adding into the solution, heating to 80 deg.C, and stirring vigorously to obtain solution; (2) weighing ferric nitrate nonahydrate and thiourea, respectively and slowly adding into the solution, stirring, then transferring the mixed solution into a high-pressure kettle, and keeping the temperature at 180 ℃ for static reaction for 24 hours; (3) and after the reaction is finished, carrying out suction filtration by using a Buchner funnel to collect reaction precipitates, and then rinsing by using distilled water to obtain the wet nitrogen-sulfur co-doped porous magnetic carbon material precursor. And (3) putting the precursor into a vacuum drying oven at 100 ℃, and drying for 12 hours to obtain the dry nitrogen-sulfur co-doped porous magnetic carbon material. The provided nitrogen-sulfur co-doped porous magnetic carbon material has a large specific surface area, and the adsorbent prepared from the nitrogen-sulfur co-doped porous magnetic carbon material has high adsorption capacity and high adsorption speed on methyl orange, and can effectively adsorb and recover the methyl orange in an aqueous solution. However, the hydrothermal method has the problems of complex process, severe conditions and single pore size.
The porous material prepared by the high internal phase emulsion template method has the advantages of simple preparation method, controllable pore size and distribution, interperforation among pores and the like. The preparation method adopts a high internal phase emulsion template method, realizes the preparation of the nitrogen/sulfur co-doped porous carbon material and the construction of the pore structure through crosslinking, polymerization and carbonization, and realizes the regulation and control of the pore structure of the porous carbon material by changing the proportion of monomers in the water phase.
Disclosure of Invention
The invention aims to provide a method for preparing and regulating a high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon aiming at the defects of the prior art. The porous carbon material prepared by the method can be regulated and controlled in pore structure and nitrogen content by adjusting the molar ratio of thiourea to melamine.
The purpose of the invention is realized by the following technical scheme:
a method for preparing and regulating a high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon comprises the following specific steps:
(1) completely dissolving a monomer, a catalyst and a surfactant in deionized water to prepare a water phase;
(2) slowly adding a certain mass of oily solvent serving as an oil phase into the water phase obtained in the step (1) under the condition of mechanical stirring, and stirring for 2 hours to obtain different oil-in-water type high internal phase emulsions;
(3) sealing the high internal phase emulsion obtained in the step (2), carrying out polymerization reaction at 75 ℃ for 24 hours to obtain a solid block-shaped crude product, carrying out Soxhlet extraction on the crude product in ethanol for 24 hours, removing the internal phase, and carrying out vacuum drying to obtain a polymer precursor;
(4) carbonizing the dried polymer precursor for 2h at 700 ℃ under the protection of nitrogen to obtain a porous carbon material;
(5) and mixing a certain amount of potassium hydroxide solution with the prepared porous carbon material, drying, and activating to obtain the nitrogen/sulfur co-doped porous carbon.
Further, the monomers in the step (1) are resorcinol, melamine, thiourea and formaldehyde in a certain proportion.
Further, in the step (1), the molar ratio of thiourea to melamine is 0:1-2:1, and the molar ratio of melamine, resorcinol and formaldehyde is 0.6:1: 3.
Further, the ratio of the volume of the water phase to the volume of the oil phase in the step (2) is 1: 3.
Further, the catalyst in the step (1) is anhydrous sodium carbonate, and the surfactant is tween 20.
Further, the mass fraction of anhydrous sodium carbonate in the aqueous phase is 0.05%, and the mass fraction of tween 20 in the aqueous phase is 10%.
Further, the oily solvent in the step (2) is toluene.
Further, the mass ratio of the potassium hydroxide dry matter to the porous carbon material in step (5) is 2: 1.
Further, the activation in the step (5) is specifically activated for 1-3 hours at 700 ℃ under the protection of nitrogen.
The invention has the beneficial effects that:
(1) the invention develops a method for preparing and regulating a high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon. The porous carbon with different pore structures is prepared by adjusting the molar ratio of thiourea to melamine in a water phase of the high internal phase emulsion template, and the apparent density of the porous polymer is reduced along with the increase of the content of thiourea, so that the regulation and control of the pore structure of the porous carbon material are realized.
(2) The melamine has high nitrogen content, the thiourea has high sulfur content and can be crosslinked with formaldehyde, and the obtained polymer is carbonized to prepare the high-nitrogen-doped porous carbon material, so that the wettability of the material is improved, and the electrochemical performance of the carbon material can be improved by introducing the pseudo-capacitor.
(3) The porous material prepared by the high internal phase emulsion template method has the advantages of simple preparation method, controllable pore size and distribution, interperforation among pores and the like. The preparation method adopts a high internal phase emulsion template method, realizes the preparation of the nitrogen-doped porous carbon material and the construction of the pore structure through crosslinking, polymerization and carbonization, and realizes the regulation and control of the pore structure of the porous carbon material by changing the proportion of monomers in a water phase.
Drawings
FIG. 1 is an electron micrograph of porous polymer precursors prepared according to examples 1, 2, 3 and 4; wherein (a): example 1, (b): example 2, (c): example 3, (d): example 4;
FIG. 2 is an electron micrograph of nitrogen-doped porous carbon prepared in examples 1, 2, 3, 4; wherein (a): example 1, (b): example 2, (c): example 3, (d): example 4;
fig. 3 is a nitrogen adsorption and desorption graph of nitrogen-doped porous carbon prepared in examples 1, 2, 3 and 4;
FIG. 4 is a graph of the X-ray energy electron spectrum of example 4;
fig. 5 is a constant current charge and discharge curve of the nitrogen-doped porous carbon prepared in examples 1, 2, 3 and 4.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
Dissolving resorcinol, thiourea, melamine, a formaldehyde solution, anhydrous sodium carbonate and tween 20 in deionized water to obtain a water phase, wherein the mass fraction of the tween 20 in the water phase is 10%, the mass fraction of the anhydrous sodium carbonate in the water phase is 0.05%, the molar ratio of the thiourea to the melamine is 0:1, the molar ratio of the melamine, the resorcinol and the formaldehyde is 0.6:1:3, and the mass fraction of the formaldehyde solution is 37%; slowly dripping toluene into the water phase under the condition of mechanical stirring (dripping is finished within 2 h), and continuously stirring for 2h after dripping is finished to obtain an oil-in-water type high internal phase emulsion with the internal phase volume fraction of 75%; carrying out polymerization reaction at 75 ℃ after sealing, and obtaining a solid block-shaped crude product after reaction for 24 hours; and (3) Soxhlet extracting the crude product in absolute ethyl alcohol for 24h, removing an internal phase, and vacuum drying to obtain a porous polymer precursor. And carbonizing the dried precursor for 2h at 700 ℃ under the protection of nitrogen to obtain the porous carbon material. Mixing potassium hydroxide with a carbon material in a mass ratio of 2:1, drying, and activating for 2 hours at 700 ℃ under the protection of nitrogen to obtain the nitrogen-doped porous carbon.
Example 2: the specific experimental procedure was the same as in example 1, with a molar ratio of thiourea to melamine in the aqueous phase of the high internal phase emulsion prepared of 0.5: 1.
Example 3: the specific experimental procedure was the same as in example 1, with a molar ratio of thiourea to melamine in the aqueous phase of the high internal phase emulsion prepared of 1: 1.
Example 4: the specific experimental procedure was the same as in example 1, with a molar ratio of thiourea to melamine in the aqueous phase of the high internal phase emulsion prepared of 2: 1.
Table 1 data of nitrogen/sulfur co-doped porous carbon prepared under different conditions
Figure 1 illustrates that the pore size of the precursor increases significantly with increasing amounts of thiourea.
Fig. 2 illustrates that the pore size of the porous carbon gradually increases with the amount of thiourea after carbonization.
Fig. 3 illustrates that the specific surface area of the porous carbon gradually increases with the amount of thiourea.
Fig. 4 illustrates the doping of both elements nitrogen/sulfur into porous carbon.
FIG. 5 illustrates that the specific capacitance of the porous carbon gradually increases with increasing amounts of thiourea, and the highest capacitance reaches 221F g-1。
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (9)
1. A method for preparing and regulating a high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon is characterized by comprising the following steps:
(1) completely dissolving a monomer, a catalyst and a surfactant in deionized water to prepare a water phase;
(2) slowly adding a certain mass of oily solvent serving as an oil phase into the water phase obtained in the step (1) under the condition of mechanical stirring, and stirring for 2 hours to obtain different oil-in-water type high internal phase emulsions;
(3) sealing the high internal phase emulsion obtained in the step (2), carrying out polymerization reaction at 75 ℃ for 24 hours to obtain a solid block-shaped crude product, carrying out Soxhlet extraction on the crude product in ethanol for 24 hours, removing the internal phase, and carrying out vacuum drying to obtain a polymer precursor;
(4) carbonizing the dried polymer precursor for 2h at 700 ℃ under the protection of nitrogen to obtain a porous carbon material;
(5) and mixing a certain amount of potassium hydroxide solution with the prepared porous carbon material, drying, and activating to obtain the nitrogen/sulfur co-doped porous carbon.
2. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the monomers in the step (1) are resorcinol, melamine, thiourea and formaldehyde in a certain proportion.
3. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 2, characterized in that: in the step (1), the molar ratio of thiourea to melamine is 0:1-2:1, and the molar ratio of melamine, resorcinol and formaldehyde is 0.6:1: 3.
4. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the ratio of the volume of the water phase to the volume of the oil phase in the step (2) is 1: 3.
5. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the catalyst in the step (1) is anhydrous sodium carbonate, and the surfactant is tween 20.
6. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 5, wherein the method comprises the following steps: the mass fraction of the anhydrous sodium carbonate in the water phase is 0.05%, and the mass fraction of the Tween 20 in the water phase is 10%.
7. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the oily solvent in the step (2) is toluene.
8. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the mass ratio of the potassium hydroxide to the porous carbon material in the step (5) is 2: 1.
9. The method for preparing and regulating the high internal phase emulsion template of nitrogen/sulfur co-doped porous carbon according to claim 1, characterized in that: the activation in the step (5) is specifically activated for 1-3h at 700 ℃ under the protection of nitrogen.
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Cited By (2)
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| CN113044838A (en) * | 2021-04-01 | 2021-06-29 | 福州大学 | High internal phase emulsion template method for preparing and regulating nitrogen/boron co-doped porous carbon |
| CN114709085A (en) * | 2022-04-22 | 2022-07-05 | 福州大学 | Nitrogen-doped sulfonated porous carbon/polyaniline composite electrode material and preparation method thereof |
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