CN110171814B - Method for synthesizing carbon nanosheet by catalysis of water-soluble KCl and energy storage and sustained release application - Google Patents
Method for synthesizing carbon nanosheet by catalysis of water-soluble KCl and energy storage and sustained release application Download PDFInfo
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- CN110171814B CN110171814B CN201910393892.9A CN201910393892A CN110171814B CN 110171814 B CN110171814 B CN 110171814B CN 201910393892 A CN201910393892 A CN 201910393892A CN 110171814 B CN110171814 B CN 110171814B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- Y02E60/10—Energy storage using batteries
Abstract
A method for synthesizing carbon nano-sheets by catalyzing water-soluble KCl and application thereof in energy storage and slow release belong to the technical field of new energy materials and environmental protection. The method comprises the following steps: 1) placing KCl in a vacuum drying oven for drying; 2) placing the dried KCl in a reaction furnace, and then introducing nitrogen or inert gas to remove air in the reaction furnace; 3) heating the reaction furnace to 500-650 ℃, and preserving heat for 10-15 min at 500-650 ℃; 4) introducing C into the reaction furnace 2 H 2 Reacting for 30-60 min; 5) and after the reaction is finished, taking out the sample, ultrasonically washing the sample in deionized water, and drying the sample. The invention adopts water-soluble KCl as the catalyst, avoids the acid washing process of removing the traditional metal or metal oxide catalyst, and is clean and environment-friendly; the method disclosed by the invention is simple to operate, low in cost, clean and environment-friendly, and can be applied to the fields of energy storage and slow release of fertilizers.
Description
Technical Field
The invention belongs to the technical field of new energy materials and environmental protection, and particularly relates to a method for preparing a micro-nano carbon sheet by using water-soluble KCl as a catalyst substrate and adopting a chemical vapor deposition method, and application of the micro-nano carbon sheet in energy storage and fertilizer slow release.
Background
In recent decades, as fossil fuels become life resources for social development, problems of exhaustion of fossil fuels, environmental pollution and the like gradually emerge, and energy and environmental problems have become hot spots of concern in various countries around the world. Under such circumstances, energy storage is urgently needed to find a new environment-friendly alternative energy source. Since the advent of the lithium ion battery in the 90 s of the 20 th century, the lithium ion battery has attracted attention of people due to its advantages of high specific energy, no memory, long service life, portability and the like, and is now available in the market. With the rapid increase of the demand of the lithium ion battery in the market, the supply problem of the lithium resource and the cost problem of the lithium ion battery are gradually revealed. In this context, researchers have gradually turned their eyes to the sodium element, the same family element of lithium. The research on sodium ion batteries is started at the earliest in about 80 s of the 20 th century, and gradually becomes a research hotspot in recent decades, and the research on sodium ion batteries aims to solve the problem that some lithium ion batteries cannot be hedged. The carbon material is a very potential negative electrode material for both lithium ion batteries and sodium ion batteries, but the graphite which is most widely applied at present has low theoretical capacity for the lithium ion batteries and is not suitable for development in the high-capacity field; for sodium ion batteries, graphite is not suitable for sodium ion batteries because sodium ions have a larger ionic radius than lithium ions. In recent years, studies have been made mainly on the nano-size and porous carbon materials, and the nano-size and porous carbon materials can increase the specific surface area of the materials and improve the material performance.
There are many methods for nano-and porous carbon materials, such as shear peeling in liquids, splitting of graphite crystals, and Chemical Vapor Deposition (CVD) techniques. Among these techniques, CVD is a simple process and can be used to produce high quality, controlled morphology carbon. Effective catalysts for growing carbon materials can be largely divided into two categories: metal particles and metal oxides. However, the inevitable need for acid washing to remove these substrates for both catalysts not only has some damage to the structure of the carbon, but also may contaminate the sample, while being environmentally unfriendly and uneconomical. Therefore, there is a need to find an efficient and economical carbon growth substrate to solve the problems of the existing catalysts.
In addition, in the aspect of agriculture, fertilizers such as potassium fertilizer are important agricultural materials and play an important role in increasing the crop yield. However, in the actual use process, the utilization rate of the fertilizer is low due to the washing of rainwater and the like, and in order to increase the yield, people only increase the using amount of the fertilizer, so that the abuse of the fertilizer is caused, and a series of problems are caused. On one hand, the potassium fertilizer and other chemical fertilizers which are put into the soil are partially deposited in the soil and are not absorbed by crops, so that the absorption of the crops on calcium, magnesium and other ions is influenced, and the crop yield is reduced; on the other hand, under the scouring action of rainwater, the fertilizer can enter rivers to cause eutrophication of water bodies, which is extremely unfavorable for water quality and aquatic organisms. In order to solve the problem, the current solution mainly comprises strict control of the input amount of the fertilizer by laws and regulations, replacement of the traditional fertilizer with farmyard manure, and the like. In the invention, a method for slowly releasing the fertilizer is provided, and the carbon is used for coating the potassium fertilizer, so that the great loss of the potassium fertilizer in rainwater weather is slowed down, the higher fertilizer effect in soil is kept, and the method is a green way for reducing the pollution of the fertilizer and improving the fertilizer effect.
Disclosure of Invention
The invention aims to provide a method for synthesizing carbon nanosheets by catalyzing water-soluble KCl and application of the method in energy storage and slow release, aiming at the defects in the background art. The invention adopts water-soluble KCl as the catalyst, avoids the acid washing process of removing the traditional metal or metal oxide catalyst, and is clean and environment-friendly; the washed KCl can be recycled, so that the utilization rate of raw materials is greatly improved, and the cost is reduced; the unwashed KCl @ C can also be used as a slow-release potash fertilizer to be put into agricultural production, and the problem of serious fertilizer pollution at present is solved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for synthesizing carbon nanosheets by catalyzing water-soluble KCl is characterized by comprising the following steps:
2, placing the KCl dried in the step 1 in a reaction zone of a reaction furnace, and introducing nitrogen or inert gas into the reaction furnace for 3-5 min to completely remove air in the reaction furnace; wherein the flow rate of nitrogen or inert gas is 50-120 mL/min;
step 3, heating the reaction furnace to 500-650 ℃ at a heating rate of 5-10 ℃/min, and keeping the temperature at 500-650 ℃ for 10-15 min to keep the temperature stable so as to activate KCl;
Step 4, introducing C into the reaction furnace at the speed of 30-40 mL/min 2 H 2 Reacting for 30-60 min by using gas;
step 5, after the reaction is finished, naturally cooling, and taking out a sample after the temperature in the furnace is reduced to room temperature;
and 6, ultrasonically washing the sample obtained in the step 5 in deionized water for 8-10 times, and drying to obtain the carbon nanosheet.
The invention also provides application of the carbon nano sheet in the field of energy storage, and the carbon nano sheet can be used as a negative electrode of a lithium ion or sodium ion battery.
The invention also provides application of the sample obtained in the step 5 in the field of slow release of fertilizers.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts water-soluble KCl as the catalyst, avoids the acid washing process of removing the traditional metal or metal oxide catalyst, and is clean and environment-friendly; the washed KCl can be recycled, so that the utilization rate of raw materials is greatly improved, and the cost is reduced; the unwashed KCl @ C sample can also be used as a slow-release potash fertilizer to be put into agricultural production, and the problem of serious fertilizer pollution at present is solved.
2. The method disclosed by the invention is simple to operate, low in cost, clean and environment-friendly, and can be applied to the fields of energy storage and slow release of fertilizers.
Drawings
FIG. 1 is a scanning electron microscope image of a micro-nano scale carbon sheet prepared in example 3 of the present invention;
fig. 2, fig. 3 and fig. 4 are scanning electron microscope images of a micro-nano scale carbon sheet prepared in embodiment 4 of the present invention at different positions, respectively;
fig. 5, 6, 7 and 8 are transmission electron microscope images of a micro-nano scale carbon sheet prepared in example 4 of the present invention at different positions, respectively;
fig. 9 is an XRD chart of the micro-nano scale carbon sheet prepared in example 4 of the present invention;
fig. 10 is a raman spectrum of a micro-nano scale carbon sheet prepared in example 4 of the present invention;
fig. 11 is a cyclic charge-discharge diagram of a lithium ion battery assembled with a micro-nano scale carbon sheet electrode according to embodiment 4 of the present invention;
fig. 12 is a circular charge-discharge diagram of a sodium ion battery assembled with a micro-nano scale carbon sheet electrode manufactured in example 4 of the present invention.
Detailed Description
The invention is further described below with reference to specific embodiments:
example 1
A method for synthesizing carbon nanosheets by catalyzing water-soluble KCl is characterized by comprising the following steps:
2, placing the KCl dried in the step 1 in a reaction zone of a reaction furnace, and then introducing nitrogen into the reaction furnace for 5min to completely remove air in the reaction furnace; wherein the flow rate of nitrogen is 100 mL/min;
Step 3, heating the reaction furnace to 500 ℃ at the heating rate of 8 ℃/min, and keeping the temperature at 500 ℃ for 15min to keep the temperature stable so as to activate KCl;
step 4, introducing C into the reaction furnace at the speed of 30mL/min 2 H 2 Reacting for 60 min;
step 5, after the reaction is finished, naturally cooling, and taking out a KCl @ C sample after the temperature in the furnace is reduced to room temperature;
and 6, ultrasonically washing the KCl @ C sample obtained in the step 5 in deionized water for 8-10 times, wherein the ultrasonic time is 30-60 min each time, and drying to obtain the carbon nanosheet.
Example 2
This example is different from example 1 in that: in the step 3, heating the reaction furnace to 550 ℃ at the heating rate of 5 ℃/min, and keeping the temperature at 550 ℃ for 15min to keep the temperature stable; in the step 4, C is introduced into the reaction furnace at the speed of 40mL/min 2 H 2 And (5) reacting for 30 min. The remaining procedure was the same as in example 1.
Example 3
This example and implementationExample 1 compares, with the difference that: in the step 3, heating the reaction furnace to 600 ℃ at the heating rate of 10 ℃/min, and keeping the temperature at 600 ℃ for 15min to keep the temperature stable; in the step 4, C is introduced into the reaction furnace at the speed of 40mL/min 2 H 2 Reacting for 30min under the action of gas. The rest of the procedure was the same as in example 1.
FIG. 1 is a scanning electron microscope image of a micro-nano scale carbon sheet prepared in example 3 of the present invention; as can be seen from fig. 1, the micro-nano-scale carbon sheet obtained in example 3 had a laminated structure.
Example 4
This example is different from example 1 in that: in step 3, the reaction furnace is heated to 650 ℃ at the heating rate of 8 ℃/min, and the temperature is kept stable by keeping the temperature at 650 ℃ for 15 min. The rest of the procedure was the same as in example 1.
The surface morphology of the obtained micro-nano scale carbon sheet is observed by a scanning electron microscope, and the obtained results of the scanning electron microscope are shown in fig. 2, 3 and 4. Fig. 2, fig. 3 and fig. 4 are scanning electron microscope images of a micro-nano scale carbon sheet prepared in embodiment 4 of the present invention at different positions, respectively; as can be seen from fig. 2, 3 and 4, the micro-nano scale carbon sheet prepared in example 4 has other morphologies: smooth carbon sheets, stepped carbon sheets, and stepped carbon sheets. From SEM results, the micro-nano scale carbon sheet is composed of a plurality of carbon sheets, and most samples have smooth surfaces; but also had rough surfaces in some portions of the sample, including striped carbon sheets and stepped carbon sheets. In addition, a plurality of round carbon sheets are gathered on the surface of the striped carbon sheet, and form a structure similar to a carbon flower like a flower petal, and the thickness of the flower petal is 40 nm. The formation of the striped carbon sheet and the stepped carbon sheet leads to abundant texture structures on the surface of the micro-nano scale carbon sheet, and is beneficial to the application of the micro-nano scale carbon sheet in energy storage.
The microstructure of the obtained micro-nano scale carbon sheet was further observed by a transmission electron microscope, and the obtained transmission electron microscope results are shown in fig. 5 to 8. Fig. 5, 6, 7 and 8 are transmission electron microscope images of a micro-nano scale carbon sheet prepared in example 4 of the present invention at different positions, respectively; fig. 5-8 show that smooth surfaces, striated surfaces, and stepped surfaces have been observed in SEM images, while the lattice structure of the material is not as pronounced and is amorphous carbon.
The obtained micro-nano scale carbon sheet is subjected to phase characteristic measurement by an X-ray diffraction (XRD) analyzer, and the obtained XRD spectrum is shown in figure 9. Fig. 9 is an XRD chart of the micro-nano scale carbon sheet prepared in example 4 of the present invention; as can be seen from fig. 9, the micro-nano scale carbon sheet prepared in example 4 includes amorphous carbon and a certain amount of KCl.
Example 5
And a lithium ion battery prepared by using the micro-nano scale carbon sheet obtained in the embodiment 4 as a negative electrode. Mixing the micro-nano scale carbon sheet obtained in the embodiment 4 with Ketjen black and polytetrafluoroethylene according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone, and uniformly mixing to obtain slurry; and (3) coating the slurry on a copper foil by using the copper foil as a current collector, and drying overnight at 80 ℃ under a vacuum of 0.1Pa to obtain the carbon electrode. At 1mol/L LiPF 6 And as an electrolyte, assembling a simulated lithium ion battery to perform constant-current charge and discharge tests.
As shown in fig. 11, when the cycle ratio of the lithium ion battery assembled with the micro/nano-scale carbon sheet electrode prepared in embodiment 4 of the present invention is 1C, the lithium ion battery has a reversible capacity of 264.5mAh/g after 190 cycles of cycle, and has good cycle stability.
Example 6
And a sodium ion battery prepared by using the micro-nano scale carbon sheet obtained in the embodiment 4 as a negative electrode. Mixing the micro-nano scale carbon sheet obtained in the embodiment 4 with Ketjen black and polytetrafluoroethylene according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone, and uniformly mixing to obtain slurry; and (3) coating the slurry on a copper foil by using the copper foil as a current collector, and drying overnight at 80 ℃ under a vacuum of 0.1Pa to obtain the carbon electrode. And (3) assembling a simulated sodium ion battery by using 1mol/L sodium perchlorate as electrolyte to perform constant-current charge and discharge tests.
As shown in fig. 12, the sodium ion battery assembled with the micro/nano-scale carbon sheet electrode prepared in example 4 of the present invention has a reversible capacity of 230.1mAh/g after 140 cycles at a current amount of 200mAh/g, and a capacity retention rate of 80.88% with respect to the second cycle. As can be seen from the data in the figure, it has better capacity performance and cycle stability.
Example 7
A simulation using the KCl @ C sample obtained in step 5 of example 4 as a fertilizer release. After the KCl @ C sample obtained in the step 5 in the embodiment 4 is washed 8-10 times by deionized water, the XRD spectrum of the material and the Raman spectrum in the figure 10 still contain KCl peaks, which shows that the KCl-coated carbon (KCl @ C sample) has a certain slowing effect on the dissolution of KCl, and has development potential and application prospect in the field of slow release of chemical fertilizers.
Claims (4)
1. A method for synthesizing carbon nanosheets by catalysis of water-soluble KCl is characterized by comprising the following steps:
step 1, placing KCl in a vacuum drying box for drying;
2, placing the KCl dried in the step 1 in a reaction furnace, and then introducing nitrogen or inert gas for 3-5 min to completely remove air in the reaction furnace; wherein the flow rate of nitrogen or inert gas is 50-120 mL/min;
step 3, heating the reaction furnace to 500-650 ℃, and preserving heat for 10-15 min at 500-650 ℃;
step 4, introducing C into the reaction furnace at the speed of 30-40 mL/min 2 H 2 Reacting for 30-60 min by using gas;
step 5, after the reaction is finished, naturally cooling, and taking out a sample after the temperature in the furnace is reduced to room temperature;
and 6, ultrasonically washing the sample obtained in the step 5 in deionized water, and drying to obtain the carbon nanosheet.
2. Use of carbon nanoplatelets obtainable by the process of claim 1 in the field of energy storage.
3. Use of carbon nanoplatelets obtained according to the process of claim 1 as negative electrode in lithium or sodium ion batteries.
4. The method of claim 1 wherein the sample obtained in step 5 is used in the field of slow release of fertilizers.
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