CN118888350B - A low-rank coal-based two-dimensional porous nanosheet, preparation method and application - Google Patents
A low-rank coal-based two-dimensional porous nanosheet, preparation method and application Download PDFInfo
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- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 20
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- 239000002033 PVDF binder Substances 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
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- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明涉及新能源储能技术领域，尤其涉及一种低阶煤基二维多孔纳米片、制备方法及应用，通过将低阶煤进行提纯，得到提纯低阶煤；将提纯低阶煤、表面活性剂、碱和水混合、干燥、高温碳化处理、酸洗、水洗和干燥，得到低阶煤基二维多孔纳米片。该制备方法基于低阶煤特殊的“类氧化石墨烯”特性，富含芳香结构的同时又具有大量的含氧官能团，借助表面活性剂的结构诱导作用制备高产率的多孔纳米片，再辅以2D结构设计，增加了多孔纳米片的电子传导特性，进而大幅提高电极材料在电化学反应中的利用效率，而且工艺简单，条件温和，可控性强，更加有利于工业化推广和应用。解决现有技术中存在的多孔碳纳米片制备过程复杂、成本高及产率低的问题。
The present invention relates to the field of new energy storage technology, and in particular to a low-rank coal-based two-dimensional porous nanosheet, a preparation method and an application thereof, wherein the low-rank coal is purified to obtain purified low-rank coal; the purified low-rank coal, a surfactant, an alkali and water are mixed, dried, subjected to high-temperature carbonization treatment, pickled, washed with water and dried to obtain a low-rank coal-based two-dimensional porous nanosheet. The preparation method is based on the special "graphene oxide-like" characteristics of low-rank coal, which is rich in aromatic structures and has a large number of oxygen-containing functional groups. The high-yield porous nanosheet is prepared by the structural induction of the surfactant, and then supplemented by the 2D structural design, which increases the electronic conduction characteristics of the porous nanosheet, thereby greatly improving the utilization efficiency of the electrode material in the electrochemical reaction, and the process is simple, the conditions are mild, the controllability is strong, and it is more conducive to industrial promotion and application. The problem of complex preparation process, high cost and low yield of porous carbon nanosheets existing in the prior art is solved.
Description
Technical Field
The invention relates to the technical field of new energy storage, in particular to a low-rank coal-based two-dimensional porous nano sheet, a preparation method and application.
Background
With the advent of the electric age, the requirements of modern society for energy storage devices have evolved toward high energy density, high power density, high safety, and long cycle life. The hybrid capacitor (Sodium Ion Capacitor, SIC) has the characteristics of high energy of a battery and high power of a super capacitor, so that the crossover type improvement of the comprehensive performances of high energy, high power, long service life, low cost and the like of the electrochemical energy storage device can be expected. The negative electrode of the hybrid capacitor is a battery type electrode which generates Faraday reaction and comprises various carbon materials, titanium-based materials, conversion materials and the like, while the positive electrode of the hybrid capacitor is a capacitor type electrode which generates adsorption reaction and is mainly made of porous carbon materials. Based on this particular construction, the hybrid capacitor effectively combines the advantages of both a battery and a supercapacitor. However, the different energy storage mechanisms lead the positive electrode and the negative electrode to have great unbalance in capacity matching, the energy storage mechanism of the negative electrode material is Faraday reaction, the specific capacity is higher, and the specific capacity of the porous carbon positive electrode material based on the physical adsorption energy storage mechanism is lower. Therefore, the development of hybrid capacitors is severely limited by the low capacity of the positive electrode material. Based on this, development of a positive electrode material having both high magnification and high capacity has become an urgent need for developing a high-performance hybrid capacitor.
The construction of a novel porous structure is an important research direction for developing high-performance porous carbon, and among many porous carbon materials, hierarchical porous carbon having a 3D structure and porous carbon nanoplatelets having a 2D structure have been widely used as capacitive electrode materials. Carbon materials of 2D structure have shorter mass transfer distances and large lateral dimensions compared to 3D structures, and are considered to have greater potential in the energy storage field. And the porous carbon material having a 2D structure is certainly a superior positive electrode material of the hybrid capacitor. The nanometer thickness is combined with rich pore structures, so that on one hand, the tortuosity of a pore canal is reduced, the diffusion of electrolyte ions in the pore canal is accelerated, and on the other hand, the sheet-shaped structure can enable electrolyte to be in direct contact with the outer surface of a material, the outer diffusion of the electrolyte ions from a liquid phase to the solid phase surface of an electrode material is accelerated, and further the utilization efficiency of the electrode material in electrochemical reaction is greatly improved. Graphene, which is a typical two-dimensional nanomaterial, has a large electrical conductivity and an ultra-high theoretical specific surface area (> 2 630m 2g-1), has been widely used as a hybrid capacitor cathode material, but its high manufacturing cost and irreversible self-stacking still have significant challenges.
Currently, the preparation of porous carbon nano-sheets mainly comprises a top-down method and a bottom-up method, wherein the top-down method is to strip thicker 2D materials to obtain nano-sheets, and comprises micro-mechanical stripping, mechanical force auxiliary liquid phase stripping, ion insertion auxiliary liquid stripping, ion exchange auxiliary liquid phase stripping, oxidation auxiliary liquid phase stripping, selective etching auxiliary liquid phase stripping and the like. The bottom-up method is to form carbon nano-sheets through polymerization aromatization of small molecules, including chemical vapor deposition, wet chemical synthesis, organic conversion and the like, and the preparation is relatively simple in process, but the product yield is relatively low, so that industrialization cannot be realized.
Disclosure of Invention
Aiming at the problems of complex preparation process, high cost and low yield of the porous carbon nano-sheet in the prior art, the invention provides a low-rank coal-based two-dimensional porous nano-sheet, a preparation method and application thereof.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
The invention provides a preparation method of a low-rank coal-based two-dimensional porous nano sheet, which comprises the following steps:
Purifying the low-rank coal to obtain purified low-rank coal;
Mixing the purified low-rank coal, a surfactant, alkali and water, and reacting for 20-30 hours at the temperature of 30-90 ℃ and drying to obtain a layered intermediate, wherein the drying temperature is 70-100 ℃;
Carrying out high-temperature carbonization treatment on the layered intermediate to obtain a porous carbon material;
And (3) carrying out acid washing, water washing and drying on the porous carbon material to obtain the low-rank coal-based two-dimensional porous nano sheet.
Further, the method for purifying the low-rank coal to obtain the purified low-rank coal comprises the following steps:
Alkali dissolution treatment is carried out on the low-rank coal to obtain low-rank coal liquid;
And (3) carrying out acid precipitation treatment, water washing and drying on the low-rank coal liquid to obtain purified low-rank coal, wherein the drying temperature is 45-60 ℃.
Further, the conditions for alkali dissolution treatment of the low-rank coal are as follows:
The alkali liquor used for alkali dissolution treatment is sodium hydroxide solution and/or potassium hydroxide solution with the concentration of 1-12 mol/L;
The mass ratio of the low-rank coal to the alkali liquor is 1 (3-15);
The alkali dissolution treatment time is 1-6 h, and the temperature is 20-90 ℃.
Further, the conditions for carrying out acid precipitation treatment on the low-rank coal liquid are as follows:
the acid solution used for the acid precipitation treatment is one or more of hydrochloric acid solution, nitric acid solution, sulfuric acid solution and hydrofluoric acid solution with the concentration of 1-12 mol/L;
The mass ratio of the low-rank coal liquid to the acid liquid is 1 (3-15);
the acid precipitation treatment time is 1-6 h, and the temperature is 20-60 ℃.
Further, the mass ratio of the purified low-rank coal to the surfactant to the alkali is 2:1 (8-12).
Further, the temperature of the high-temperature carbonization treatment of the layered intermediate is 200-1000 ℃, the temperature rising rate is 0.5-5 ℃ per minute, and the time of the high-temperature carbonization treatment is 2-6 hours.
Further, hydrochloric acid solution with the concentration of 0.1-2 mol/L is adopted when the porous carbon material is subjected to acid washing.
Preferably, the low-rank coal is weathered coal or brown coal.
The low-rank coal-based two-dimensional porous nano sheet is prepared by the method.
The application of the low-rank coal-based two-dimensional porous nano-sheet in preparing the anode of the hybrid capacitor is disclosed.
Compared with the prior art, the invention has the following beneficial effects:
The invention provides a preparation method of a low-rank coal-based two-dimensional porous nano sheet, which comprises the steps of purifying low-rank coal to obtain purified low-rank coal; mixing the purified low-rank coal, a surfactant, alkali and water, drying to obtain a layered intermediate, carrying out high-temperature carbonization treatment on the layered intermediate to obtain a porous carbon material, and carrying out acid washing, water washing and drying on the porous carbon material to obtain the low-rank coal-based two-dimensional porous nano sheet. The method adopts low-rank coal as a carbon source, and compared with other coals, the low-rank coal is rich in the structural characteristics of polycyclic aromatic hydrocarbon, so that the carbon nanosheets with larger size and higher carbon yield are obtained, the low-rank coal and the surfactant are uniformly mixed under high-temperature reaction to form a stable lamellar liquid microcrystalline structure, after the low-rank coal is carbonized at high temperature, the low-rank coal is subjected to two-dimensional self-assembly to obtain an ultrathin two-dimensional porous structure, the structure is beneficial to reducing the tortuosity of a pore channel, accelerating the diffusion of electrolyte ions in the pore channel, and on the other hand, the lamellar structure can enable electrolyte to be in direct contact with the outer surface of a material, so that the external diffusion of electrolyte ions from a liquid phase to the solid phase surface of the electrode material is accelerated, the utilization efficiency of the electrode material in electrochemical reaction is greatly improved, the preparation process is simple, the production cost is low, and the method is easy for large-scale production.
The invention provides a low-rank coal-based two-dimensional porous nano sheet, which is prepared by the method. The low-rank coal-based two-dimensional porous nano sheet has high yield and a two-dimensional porous sheet structure, is beneficial to reducing the tortuosity of a pore channel, quickens the diffusion of electrolyte ions in the pore channel, can lead electrolyte to be in direct contact with the outer surface of a material, quickens the out-diffusion of the electrolyte ions from a liquid phase to the solid phase surface of an electrode material, and further greatly improves the utilization efficiency of the electrode material in electrochemical reaction.
The low-rank coal-based two-dimensional porous nano sheet is applied to the preparation of the positive electrode of the hybrid capacitor, and the prepared capacitor has higher charge and discharge speed and energy density, better capacitance performance and cycling stability, low cost, easy industrialization realization and wide application prospect in the energy storage field of super capacitors and the like.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a low-rank coal-based two-dimensional porous nano-sheet.
Fig. 2 is an SEM image of the low-rank coal-based two-dimensional porous nanoplatelets prepared in example 1 of the present invention.
FIG. 3 is an XRD pattern of the low-rank coal-based two-dimensional porous nanoplatelets prepared in examples 1-3 of the present invention.
FIG. 4 is a Raman diagram of the low-rank coal-based two-dimensional porous nanoplatelets prepared in examples 1-3 of the present invention.
Fig. 5 is an N 2 adsorption-desorption graph of the low-rank coal-based two-dimensional porous nanoplatelets prepared in examples 1-3 of the present invention.
FIG. 6 is a graph showing the rate performance of the low-rank coal-based two-dimensional porous nanoplatelets prepared in examples 1-3 of the present invention.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of," and "consisting essentially of," such as "a includes a" encompassing "a and other" and "a includes only a".
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
The invention will now be described in further detail with reference to specific examples, which are intended to illustrate, but not to limit, the invention.
Referring to fig. 1, the invention discloses a preparation method of a low-rank coal-based two-dimensional porous nano sheet, which comprises the following steps:
s1, purifying low-rank coal to obtain purified low-rank coal, wherein the method specifically comprises the following steps:
Alkali dissolution treatment is carried out on low-rank coal to obtain low-rank coal liquid, namely the low-rank coal is placed in a sodium hydroxide solution and/or a potassium hydroxide solution with the concentration of 1-12 mol/L, the alkali dissolution treatment time is 1-6 hours under the condition of 20-90 ℃, the low-rank coal is fully stirred and centrifuged, and supernatant fluid is taken to be the low-rank coal liquid, wherein the mass ratio of the low-rank coal to alkali liquor is 1 (3-15);
And (3) carrying out acid precipitation treatment, water washing and drying on the low-rank coal liquid to obtain purified low-rank coal, namely mixing the low-rank coal liquid with one or more acid solutions of hydrochloric acid solution, nitric acid solution, sulfuric acid solution and hydrofluoric acid solution with the concentration of 1-12 mol/L, carrying out acid precipitation treatment for 1-6h at the temperature of 20-60 ℃, then carrying out water washing for many times until the solution is neutral, centrifuging, and drying at the temperature of 45-60 ℃ to obtain the purified low-rank coal, wherein the mass ratio of the low-rank coal liquid to the acid solution is 1 (3-15).
S2, mixing the purified low-rank coal, a surfactant, alkali and water, and drying to obtain a layered intermediate, wherein the layered intermediate specifically comprises the following components:
Mixing the purified low-rank coal, a surfactant and alkali in a mass ratio of 2:1 (8-12) in water to form a mixed solution, reacting for 20-30 hours at 30-90 ℃ and drying at 70-100 ℃ to obtain a layered intermediate, wherein the concentration of alkali in the mixed solution is 0.7-1.1 mol/L.
S3, carrying out high-temperature carbonization treatment on the layered intermediate to obtain a porous carbon material, wherein the porous carbon material specifically comprises the following components:
Under the protection atmosphere of high-purity nitrogen or argon, heating the layered intermediate to 200-1000 ℃ at the heating rate of 0.5-5 ℃ per minute for high-temperature carbonization treatment for 2-6 hours to obtain a porous carbon material;
S4, carrying out acid washing, water washing and drying on the porous carbon material to obtain the low-rank coal-based two-dimensional porous nano sheet, wherein the specific steps are as follows:
And (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1-2 mol/L, and then washing the porous carbon material with water for multiple times to neutrality, and drying the porous carbon material at 50-80 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Preferably, the low-rank coal is weathered coal or brown coal, and the surfactant is an amphoteric diblock copolymer or an amphoteric triblock copolymer, preferably F127 or P123.
Example 1
Placing brown coal in 6mol/L sodium hydroxide solution, carrying out alkali dissolution treatment for 3h at 60 ℃, wherein the mass ratio of the brown coal subjected to alkali dissolution treatment to the sodium hydroxide solution is 1:10, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 6mol/L hydrochloric acid solution, carrying out acid precipitation treatment for 4h at 50 ℃, wherein the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:10, carrying out repeated washing and centrifuging after the acid precipitation treatment until the solution is nearly neutral, drying to obtain purified low-rank coal, dissolving purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:10 to form mixed solution, stirring for 24h at 90 ℃, and drying at 70 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 0.7mol/L;
heating the layered intermediate to 800 ℃ at a heating rate of 2 ℃ per min under N 2 atmosphere for 2 hours of high-temperature carbonization treatment to obtain a porous carbon material;
and (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1mol/L, washing with water to be neutral, and drying at 50 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 2
Placing brown coal in 6mol/L sodium hydroxide solution, performing alkali dissolution treatment for 3h at 60 ℃, wherein the mass ratio of the brown coal subjected to alkali dissolution treatment to the sodium hydroxide solution is 1:10, fully stirring and centrifuging, collecting supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 6mol/L hydrochloric acid solution, performing acid precipitation treatment for 4h at 50 ℃, wherein the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:10, performing acid precipitation treatment, performing repeated washing and centrifuging until the solution is nearly neutral, and drying to obtain purified low-rank coal;
Dissolving purified low-rank coal, F127 and potassium hydroxide in deionized water according to a mass ratio of 2:1:8 to form a mixed solution, stirring for 24h at 90 ℃ and drying at 70 ℃ to obtain a layered intermediate, wherein the concentration of the mixed solution is 0.7mol/L;
heating the layered intermediate to 800 ℃ at a heating rate of 2 ℃ per min under N 2 atmosphere for 2 hours of high-temperature carbonization treatment to obtain a porous carbon material;
and (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1mol/L, washing with water to be neutral, and drying at 50 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 3
Placing brown coal in 6mol/L sodium hydroxide solution, carrying out alkali dissolution treatment for 3h at 60 ℃, wherein the mass ratio of the brown coal subjected to alkali dissolution treatment to the sodium hydroxide solution is 1:10, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 6mol/L hydrochloric acid solution, carrying out acid precipitation treatment for 4h at 50 ℃, wherein the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:10, carrying out repeated washing and centrifuging after the acid precipitation treatment until the solution is nearly neutral, drying to obtain purified low-rank coal, dissolving purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:12 to form mixed solution, stirring for 24h at 90 ℃, and drying at 70 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 0.7mol/L;
heating the layered intermediate to 800 ℃ at a heating rate of 2 ℃ per min under N 2 atmosphere for 2 hours of high-temperature carbonization treatment to obtain a porous carbon material;
and (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1mol/L, washing with water to be neutral, and drying at 50 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Referring to fig. 2 to 5, in order to test the performance of the low-rank coal-based two-dimensional porous nano-sheet prepared in the invention, the low-rank coal-based two-dimensional porous nano-sheet prepared in the examples 1 to 3 is sequentially subjected to SEM, XRD, raman and N 2 adsorption and desorption tests, so that the low-rank coal-based two-dimensional porous nano-sheet prepared in the invention is spongy, has obvious open pores, is beneficial to reducing the tortuosity of a pore channel, accelerating the diffusion of electrolyte ions in the pore channel, enabling electrolyte to be in direct contact with the outer surface of a material, accelerating the outer diffusion of electrolyte ions from a liquid phase to the solid phase surface of an electrode material, and further greatly improving the utilization efficiency of the electrode material in an electrochemical reaction. The I D/IG value is more than 1.6, which indicates that the prepared low-rank coal-based two-dimensional porous nano-sheet has more defects, and further indicates that the two-dimensional porous nano-sheet has more active sites. The specific surface area in the N 2 adsorption-desorption graph is larger than 1700m 2g-1, which shows that the low-rank coal-based two-dimensional porous nano sheet has higher specific surface area, and the electrode material with high specific surface area generally has more complex pore structure and more pore channels, which is beneficial to the rapid transmission of ions in the electrolyte in the electrode material, and the small particle size and more surface defects can also improve the electronic conductivity of the electrode material, thereby improving the overall electrochemical performance.
Referring to fig. 6, in order to test the performance of the low-rank coal-based two-dimensional porous nano-sheets prepared in this example 1-3 as a positive electrode material, the low-rank coal-based two-dimensional porous nano-sheets prepared in this example 1-3 were mixed with conductive carbon black and polyvinylidene fluoride in a ratio of 8:1:1, respectively, to obtain a positive electrode slurry, the positive electrode slurry was uniformly coated on an aluminum foil, vacuum-dried and cut into electrode sheets with a diameter of 15mm, the electrode sheets were used as working electrodes, sodium sheets were used as counter electrodes, glass fibers were used as separators, and NaClO 4 was used as an electrolyte, and battery assembly was performed in a glove box filled with argon gas. And a rate performance test was performed, and as a result, it was found that the material achieved a high capacity retention of 73.3% when the current density was increased from 0.1 to 10Ag -1 (120.9 to 88mAhg -1). It should be noted that LCN4-LCN6 in the figure refers to the use amount ratio of alkali to purified low-rank coal being 4:1, 5:1 and 6:1 respectively.
Example 4
Placing weathered coal in 1mol/L potassium hydroxide solution, carrying out alkali dissolution treatment for 6h at 90 ℃, dissolving the weathered coal subjected to alkali dissolution treatment in deionized water according to the mass ratio of 1:15, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 1mol/L hydrochloric acid solution, carrying out acid precipitation treatment for 6h at 60 ℃, carrying out washing and centrifuging for multiple times until the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:15, carrying out acid precipitation treatment until the solution is nearly neutral, and drying to obtain purified low-rank coal, dissolving the purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:11 to form mixed solution, stirring for 26h at 80 ℃, and drying at 80 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 0.8mol/L;
heating the layered intermediate to 500 ℃ at a heating rate of 2 ℃ per min under N 2 atmosphere for carbonization treatment for 4 hours to obtain a porous carbon material;
and (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1mol/L, washing with water to be neutral, and drying at 60 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 5
Placing weathered coal in 2mol/L potassium hydroxide solution, carrying out alkali dissolution treatment for 3h at 80 ℃, dissolving the weathered coal subjected to alkali dissolution treatment and the potassium hydroxide solution in a mass ratio of 1:6, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 2mol/L hydrochloric acid solution, carrying out acid precipitation treatment for 3h at 45 ℃, carrying out washing and centrifuging for multiple times after the low-rank coal liquid and the hydrochloric acid solution are subjected to acid precipitation treatment until the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:6, drying until the solution is nearly neutral, dissolving the purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:10 to form mixed solution, stirring for 30h at 50 ℃, and drying at 100 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 1mol/L;
Heating the layered intermediate to 200 ℃ at a heating rate of 0.5 ℃ per min under N 2 atmosphere for carbonization treatment for 6 hours to obtain a porous carbon material;
And (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.1mol/L, washing with water to be neutral, and drying at 70 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 6
Placing weathered coal in 12mol/L sodium hydroxide solution, carrying out alkali dissolution treatment for 2h at 20 ℃, dissolving the weathered coal subjected to alkali dissolution treatment and the sodium hydroxide solution in a mass ratio of 1:5, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 10mol/L hydrochloric acid solution, carrying out acid precipitation treatment for 6h at 20 ℃, carrying out the repeated washing and centrifuging after the low-rank coal liquid and the hydrochloric acid solution are subjected to acid precipitation treatment until the mass ratio of the low-rank coal liquid to the hydrochloric acid solution is 1:8, carrying out washing and centrifuging until the solution is nearly neutral, and drying to obtain purified low-rank coal, dissolving the purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:9 to form mixed solution, stirring for 30h at 20 ℃, and drying at 100 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 1.1mol/L;
Heating the layered intermediate to 1000 ℃ at a heating rate of 5 ℃ per min under N 2 atmosphere for 2 hours of high-temperature carbonization treatment to obtain a porous carbon material;
And (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 0.5mol/L, washing with water to be neutral, and drying at 70 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 7
Placing brown coal in 10mol/L sodium hydroxide solution, carrying out alkali dissolution treatment for 1h at 30 ℃, wherein the mass ratio of the brown coal subjected to alkali dissolution treatment to the sodium hydroxide solution is 1:7, fully stirring and centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in 9mol/L hydrofluoric acid solution, carrying out acid precipitation treatment for 2h at 40 ℃, wherein the mass ratio of the low-rank coal liquid to the hydrofluoric acid solution is 1:7, carrying out repeated washing and centrifuging after the acid precipitation treatment until the solution is nearly neutral, drying to obtain purified low-rank coal, dissolving purified low-rank coal, F127 and potassium hydroxide in deionized water according to the mass ratio of 2:1:12 to form mixed liquid, stirring at 70 ℃ for 29h, and drying at 80 ℃ to obtain layered intermediate, wherein the concentration of the mixed liquid is 0.9mol/L;
Heating the layered intermediate to 700 ℃ at a heating rate of 2 ℃ per min under N 2 atmosphere for carbonization treatment for 4 hours to obtain a porous carbon material;
and (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 1mol/L, washing with water to neutrality, and drying at 70 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 8
Placing lignite in a mixed solution of 10mol/L sodium hydroxide solution and 10mol/L potassium hydroxide solution, carrying out alkali dissolution treatment for 5 hours at 45 ℃, fully stirring and centrifuging the lignite subjected to alkali dissolution treatment to obtain a supernatant to obtain a low-rank coal solution, placing the low-rank coal solution in an 11mol/L hydrochloric acid solution at 55 ℃ for acid precipitation treatment for 1 hour, carrying out the acid precipitation treatment to obtain a solution which is approximately neutral, carrying out washing and centrifugation for multiple times until the solution is dried to obtain purified low-rank coal, dissolving the purified low-rank coal, P123 and sodium hydroxide in deionized water according to the mass ratio of 2:1:10 to form a mixed solution, stirring for 28 hours at 75 ℃, and drying at 90 ℃ to obtain a layered intermediate, wherein the concentration of the mixed solution is 0.75mol/L;
Heating the layered intermediate to 600 ℃ at a heating rate of 3 ℃ per minute under N 2 atmosphere for carbonization treatment for 4 hours to obtain a porous carbon material;
And (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 1.5mol/L, washing with water to neutrality, and drying at 70 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 9
Placing lignite in a mixed solution of 9mol/L potassium hydroxide solution, carrying out alkali dissolution treatment for 3 hours at 45 ℃, dissolving the lignite subjected to alkali dissolution treatment in deionized water according to the mass ratio of 2:1:12 to form mixed solution, stirring thoroughly, centrifuging, taking supernatant to obtain low-rank coal liquid, placing the low-rank coal liquid in a sulfuric acid solution with the mass ratio of 9mol/L and 55 ℃ for acid precipitation treatment for 1 hour, carrying out acid precipitation treatment, washing and centrifuging for multiple times until the solution is nearly neutral, and drying to obtain purified low-rank coal, dissolving the purified low-rank coal, F127 and sodium hydroxide in deionized water according to the mass ratio of 2:1:12 to form mixed solution, stirring 30 hours at 35 ℃ and drying at 70 ℃ to obtain layered intermediate, wherein the concentration of the mixed solution is 1.05mol/L;
Heating the layered intermediate to 600 ℃ at a heating rate of 1 ℃ per minute under N 2 atmosphere for carbonization treatment for 4 hours to obtain a porous carbon material;
And (3) pickling the porous carbon material in a hydrochloric acid solution with the concentration of 2mol/L, washing with water to neutrality, and drying at 70 ℃ to obtain the low-rank coal-based two-dimensional porous nano sheet.
Example 10
A low-rank coal-based two-dimensional porous nanoplatelet prepared by the method described in any of examples 1-9. The low-rank coal-based two-dimensional porous nano sheet has high yield and a two-dimensional porous sheet structure, is beneficial to reducing the tortuosity of a pore channel, quickens the diffusion of electrolyte ions in the pore channel, can lead electrolyte to be in direct contact with the outer surface of a material, quickens the out-diffusion of the electrolyte ions from a liquid phase to the solid phase surface of an electrode material, and further greatly improves the utilization efficiency of the electrode material in electrochemical reaction.
Example 11
The use of the low-rank coal-based two-dimensional porous nanoplatelets of example 10 in the preparation of a hybrid capacitor anode. The prepared capacitor has higher charge and discharge speed and energy density, better capacitance performance and cycling stability, low cost and easy realization of industrialization, and has wide application prospect in the energy storage fields of super capacitors and the like.
In summary, the invention provides a low-rank coal-based two-dimensional porous nano sheet, a preparation method and application thereof. The novel preparation method for preparing the low-rank coal-based porous carbon two-dimensional carbon nano sheet from the middle to the top is provided. The method is based on the special 'graphene oxide-like' characteristic of low-rank coal, namely, the method is rich in aromatic structure and simultaneously has a large amount of oxygen-containing functional groups, the porous carbon nano-sheet with high yield is prepared by means of the structure induction effect of the surfactant, and the 2D structural design is adopted, so that the electron conduction characteristic of the porous carbon is increased, the utilization efficiency of the electrode material in electrochemical reaction is greatly improved, and the method is simple in process, mild in condition and strong in controllability, and is more beneficial to industrial popularization and application. The resulting carbon nanoplatelets exhibit excellent electrochemical performance in hybrid capacitors. The method is not only hopeful to obtain the porous carbon nano sheet electrode material for the high-performance hybrid capacitor, but also is beneficial to widening the application field of low-rank coal.
The foregoing description of the preferred embodiment of the present invention is not intended to limit the technical solution of the present invention in any way, and it should be understood that the technical solution can be modified and replaced in several ways without departing from the spirit and principle of the present invention, and these modifications and substitutions are also included in the protection scope of the claims.
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