CN110171814A - Water-soluble KCl catalyzes and synthesizes the method and energy storage, sustained release application of carbon nanosheet - Google Patents
Water-soluble KCl catalyzes and synthesizes the method and energy storage, sustained release application of carbon nanosheet Download PDFInfo
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- CN110171814A CN110171814A CN201910393892.9A CN201910393892A CN110171814A CN 110171814 A CN110171814 A CN 110171814A CN 201910393892 A CN201910393892 A CN 201910393892A CN 110171814 A CN110171814 A CN 110171814A
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- kcl
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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
-
- 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
-
- 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
-
- 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
-
- 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 kind of water solubility KCl catalyzes and synthesizes the method and its application in energy storage, sustained release of carbon nanosheet, belongs to new energy materials and environmental technology field.The following steps are included: 1) KCl is placed in a vacuum drying oven drying；2) KCl after drying is placed in reacting furnace, nitrogen or inert gas is then passed to, to exclude the air in reacting furnace；3) reacting furnace is heated to 500~650 DEG C, and 10~15min is kept the temperature at 500~650 DEG C；4) C is passed through into reacting furnace2H2, react 30~60min；5) sample, and supersound washing in deionized water after reaction, are taken out, it is dry.The present invention, as catalyst, avoids the acid cleaning process of removal conventional metals or metal oxide catalyst, clean and environmental protection using water solubility KCl；The method of the present invention is easy to operate, low in cost, clean and environmental protection, can be applied to energy storage and slow-release fertilizer field.
Description
Technical field
The invention belongs to new energy materials and environmental technology field, and in particular to a kind of to use water solubility KCl as catalyst
Matrix and use chemical vapour deposition technique prepare the method for micro/nano-scale carbon plate and its application in energy storage and slow-release fertilizer.
Background technique
Recent decades, as fossil fuel becomes the lifeblood resource of social development, fossil fuel exhaustion, environmental pollution etc. are asked
Topic gradually reveals, and energy and environment problem has become the hot spot of countries in the world concern.In this context, energy stores up
It deposits and is badly in need of finding a kind of environmental-friendly novel alternative energy source.Since lithium ion battery the 1990s comes out, lithium ion
Battery gradually attracts people's attention due to having many advantages, such as high specific energy, without memory, long service life, light portable,
It has been seen everywhere in the market to lithium ion battery today.Demand rapid growth with market to lithium ion battery, to lithium
The supply problem of resource and the cost problem of lithium ion battery, are gradually exposed.In this context, researcher
Gradually sight is turned to congeners --- the sodium element of lithium.The research of sodium-ion battery early start is in left side the 1980s
The right side, last decade start to be increasingly becoming research hotspot, and the rise purpose of sodium-ion battery research is to solve to deposit in lithium ion battery
Some the problem of can not liquidating.No matter carbon material is all that one kind extremely has for lithium ion battery or sodium-ion battery
The negative electrode material of potentiality, however the graphite being most widely used at present is low for lithium ion battery theoretical capacity, is unsuitable for
The development of high capacity field；For sodium-ion battery, since the ionic radius of sodium ion is bigger compared with lithium ion, graphite is for sodium
Ion battery is simultaneously not suitable for.In recent years, the research of nanosizing and porous is substantially carried out to carbon material, by nanosizing and more
Holeization can increase material specific surface area, to improve material property.
There are many nanosizing and the methods of porous carbon material, such as shearing in liquid to remove, graphite crystal at present
Splitting and chemical vapor deposition (Chemical Vapor Deposition, CVD) technology.In these techniques, CVD is a kind of
The method of simple process can be used for preparing the carbon of high quality, morphology controllable.Effective catalyst for growing carbon material mainly may be used
It is divided into two classes: metallic particles and metal oxide.However, unavoidably needing pickling to eliminate these both catalyst
Substrate not only has certain damage to the structure of carbon, it is also possible to pollute sample, while unfriendly and uneconomical to environment.
It is, thus, sought for a kind of efficiently carbon growth substrate with economy, to solve the problems, such as that existing catalyst exists.
In addition, agriculturally, the chemical fertilizer such as potash fertilizer are important material used for agriculture, there is important work to crop yield is improved
With.But in the actual use process, washing away for rainwater etc. causes the utilization rate of chemical fertilizer low, and in order to increase yield, people only have
The usage amount for increasing chemical fertilizer, results in the abuse of chemical fertilizer, and then cause a series of problem.On the one hand, it puts into soil
The chemical fertilizer such as potash fertilizer, a part deposition not absorbed by crops in the soil, influences absorption of the crop to calcium, magnesium plasma,
Reduce crop yield；On the other hand, under rainwash effect, chemical fertilizer can enter in rivers, cause the eutrophy of water body
Change, it is totally unfavorable to water quality and aquatic organism.For this problem, current solution mainly includes tight by laws and regulations
Lattice control the input amount of chemical fertilizer and replace traditional fertilizer etc. with farmyard manure.In the present invention, it is proposed that a kind of slow release chemical fertilizer
Method, by with carbon coating potash fertilizer, slowing down its being largely lost in rainwater weather, keep in the soil higher fertilizer efficiency make
With, be it is a kind of reduction pollution by chemical fertilizer, promoted fertilizer efficiency green approach.
Summary of the invention
It is an object of the present invention to propose that a kind of water solubility KCl catalyzes and synthesizes carbon and receives for defect existing for background technique
The method and its application in energy storage, sustained release of rice piece.The present invention, as catalyst, avoids removal using water solubility KCl
The acid cleaning process of conventional metals or metal oxide catalyst, clean and environmental protection；And can recycle again the KCl after washing makes
With greatly improving the utilization rate of raw material, reduce costs；Not washed KCl C is alternatively arranged as a kind of slow-release potassium fertilizer throwing
Enter agricultural production, solves the problems, such as current serious pollution by chemical fertilizer.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of method that water solubility KCl catalyzes and synthesizes carbon nanosheet, which comprises the following steps:
KCl is placed in a vacuum drying oven by step 1, dry 12 at 80~120 DEG C~for 24 hours；
Step 2, the reaction zone that KCl of the step 1 after dry is placed in reacting furnace, nitrogen or indifferent gas are passed through into reacting furnace
3~5min of body, to exclude the air in reacting furnace completely；Wherein, the throughput of nitrogen or inert gas is 50~120mL/
min；
Reacting furnace is heated to 500~650 DEG C with the heating rate of 5~10 DEG C/min by step 3, and at 500~650 DEG C
10~15min of lower heat preservation makes temperature keep stablizing, to activate KCl；
Step 4 is passed through C into reacting furnace with the rate of 30~40mL/min2H2Gas reacts 30~60min；
Step 5, after reaction, Temperature fall is cooled to room temperature to in-furnace temperature, takes out sample；
Supersound washing 8~10 times in deionized water of step 6, the sample for obtaining step 5, it is dry, it can be obtained described
Carbon nanosheet.
The present invention also provides above-mentioned carbon nanosheets in the application of energy storage field, can be used as lithium ion or sodium-ion battery
Cathode.
Application of the sample obtained the present invention also provides above-mentioned steps 5 in slow-release fertilizer field.
Compared with prior art, the invention has the benefit that
1, the present invention avoids removal conventional metals or metal oxide catalyst using water solubility KCl as catalyst
Acid cleaning process, clean and environmental protection；And the KCl after washing can be recycled again, greatly improve the utilization rate of raw material,
It reduces costs；Not washed KCl C sample is alternatively arranged as a kind of slow-release potassium fertilizer investment agricultural production, solves serious at present
Pollution by chemical fertilizer problem.
2, the method for the present invention is easy to operate, low in cost, clean and environmental protection, can be applied to energy storage and slow-release fertilizer field.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of micro/nano-scale carbon plate made from the embodiment of the present invention 3；
Fig. 2, Fig. 3 and Fig. 4 are respectively scanning electricity of the micro/nano-scale carbon plate made from the embodiment of the present invention 4 under different location
Mirror figure；
Fig. 5, Fig. 6, Fig. 7 and Fig. 8 are respectively that micro/nano-scale carbon plate made from the embodiment of the present invention 4 is saturating under different location
Penetrate electron microscope picture；
Fig. 9 is the XRD diagram of micro/nano-scale carbon plate made from the embodiment of the present invention 4；
Figure 10 is the Raman map of micro/nano-scale carbon plate made from the embodiment of the present invention 4；
Figure 11 is the cycle charge-discharge of the lithium ion battery of micro/nano-scale carbon plate electrode assembling made from the embodiment of the present invention 4
Figure；
Figure 12 is the cycle charge-discharge of the sodium-ion battery of micro/nano-scale carbon plate electrode assembling made from the embodiment of the present invention 4
Figure.
Specific embodiment
The invention will be further described With reference to embodiment:
Embodiment 1
A kind of method that water solubility KCl catalyzes and synthesizes carbon nanosheet, which comprises the following steps:
Step 1 weighs a certain amount of KCl and is placed in a vacuum drying oven, the dry 12h at 80 DEG C；
Step 2, the reaction zone that KCl of the step 1 after dry is placed in reacting furnace, are then passed through nitrogen into reacting furnace
5min, to exclude the air in reacting furnace completely；Wherein, the throughput of nitrogen is 100mL/min；
Reacting furnace is heated to 500 DEG C with the heating rate of 8 DEG C/min by step 3, and heat preservation 15min makes temperature at 500 DEG C
Degree keeps stablizing, to activate KCl；
Step 4 is passed through C into reacting furnace with the rate of 30mL/min2H2Gas reacts 60min；
Step 5, after reaction, Temperature fall is cooled to room temperature to in-furnace temperature, takes out KCl@C sample；
Step 6, KCl@C sample supersound washing 8~10 times in deionized water for obtaining step 5, each ultrasonic time
It is dry for 30~60min, the carbon nanosheet can be obtained.
Embodiment 2
Compared with Example 1, difference is the present embodiment: will react stove heating in step 3 with the heating rate of 5 DEG C/min
To 550 DEG C, and keeping the temperature 15min at 550 DEG C makes temperature keep stablizing；Rate in step 4 with 40mL/min is into reacting furnace
It is passed through C2H2Gas reacts 30min.Remaining step is same as Example 1.
Embodiment 3
Compared with Example 1, difference is the present embodiment: being added reacting furnace with the heating rate of 10 DEG C/min in step 3
Heat is to 600 DEG C, and keeping the temperature 15min at 600 DEG C makes temperature keep stablizing；With the rate of 40mL/min to reacting furnace in step 4
Inside it is passed through C2H2Gas reacts 30min.Remaining step is same as Example 1.
Fig. 1 is the scanning electron microscope (SEM) photograph of micro/nano-scale carbon plate made from the embodiment of the present invention 3；As shown in Figure 1, embodiment 3 obtains
The micro/nano-scale carbon plate arrived has stepped construction.
Embodiment 4
Compared with Example 1, difference is the present embodiment: will react stove heating in step 3 with the heating rate of 8 DEG C/min
To 650 DEG C, and keeping the temperature 15min at 650 DEG C makes temperature keep stablizing.Remaining step is same as Example 1.
It is observed using configuration of surface of the scanning electron microscope to obtained micro/nano-scale carbon plate, obtained scanning electron microscope result
As shown in Figure 2,3, 4.Fig. 2, Fig. 3 and Fig. 4 are respectively micro/nano-scale carbon plate made from the embodiment of the present invention 4 under different location
Scanning electron microscope (SEM) photograph；As Fig. 2, Fig. 3 and Fig. 4 it is found that other patterns occurs in micro/nano-scale carbon plate made from embodiment 4: smooth carbon
Piece, ladder-like carbon plate and step-like carbon plate.As can be seen that micro/nano-scale carbon plate is made of many carbon plates, greatly from SEM result
Most samples have smooth surface；But also there is rough surface in some parts of sample, including striated carbon plate and ladder-like
Carbon plate.In addition, there are many round carbon plates to be gathered in striped carbon plate surface, and it is similar to petal, form the structure of similar carbon flower, petal
With a thickness of 40nm.The formation of striated carbon plate and ladder-like carbon plate results in micro/nano-scale carbon plate surface texture knot abundant
Structure is conducive to its application in energy storage.
It is further looked at using microstructure of the transmission electron microscope to obtained micro/nano-scale carbon plate, obtained transmission
Electron microscopic findings are as viewed in figures 5-8.Fig. 5, Fig. 6, Fig. 7 and Fig. 8 are respectively micro/nano-scale carbon made from the embodiment of the present invention 4
Transmission electron microscope figure of the piece under different location；Fig. 5-8 display, the smooth surface occurred in SEM image, striated surface
And step-like surface has all been observed to obtain, while the lattice structure of material is not obvious, and is amorphous carbon.
Phase is carried out to obtained micro/nano-scale carbon plate using X-ray diffraction analysis instrument (X-ray diffraction, XRD)
Position pattern measurement, it is as shown in Figure 9 to obtain XRD spectrum.Fig. 9 is the XRD diagram of micro/nano-scale carbon plate made from the embodiment of the present invention 4；
It as shown in Figure 9, include amorphous carbon and a certain amount of KCl in micro/nano-scale carbon plate made from embodiment 4.
Embodiment 5
A kind of lithium ion battery prepared using the micro/nano-scale carbon plate that embodiment 4 obtains as cathode.It will implement
The micro/nano-scale carbon plate and Ketjen black that example 4 obtains, polytetrafluoroethylene (PTFE) are mixed according to the ratio that mass ratio is 8:1:1,
N-Methyl pyrrolidone is added, is uniformly mixed and obtains slurry；Collector is done using copper foil, above-mentioned slurry is coated on copper foil,
At 80 DEG C, 0.1Pa dried overnight under vacuum, carbon electrode is obtained.With the LiPF of 1mol/L6As electrolyte, assembling simulation lithium
Ion battery carries out constant current charge-discharge test.
As shown in figure 11, the lithium ion battery of micro/nano-scale carbon plate electrode assembling made from the embodiment of the present invention 4, is recycling
When multiplying power is 1C, the reversible capacity with 264.5mAh/g after 190 circle of circulation, and there is good cyclical stability.
Embodiment 6
A kind of sodium-ion battery prepared using the micro/nano-scale carbon plate that embodiment 4 obtains as cathode.It will implement
The micro/nano-scale carbon plate and Ketjen black that example 4 obtains, polytetrafluoroethylene (PTFE) are mixed according to the ratio that mass ratio is 8:1:1,
N-Methyl pyrrolidone is added, is uniformly mixed and obtains slurry；Collector is done using copper foil, above-mentioned slurry is coated on copper foil,
At 80 DEG C, 0.1Pa dried overnight under vacuum, carbon electrode is obtained.Using the sodium perchlorate of 1mol/L as electrolyte, assembling simulation
Sodium-ion battery carries out constant current charge-discharge test.
As shown in figure 12, the sodium-ion battery of micro/nano-scale carbon plate electrode assembling made from the embodiment of the present invention 4,
Under the magnitude of current of 200mAh/g, the reversible capacity with 230.1mAh/g after 140 circle of circulation, relative to the second circle capacity retention ratio
It is 80.88%.It can be seen that it with preferable volumetric properties and cyclical stability from the data in figure.
Embodiment 7
A kind of KCl@C sample obtained using step 5 in embodiment 4 is as the simulated experiment of slow-release fertilizer.In embodiment 4
The KCl@C sample that step 5 obtains by deionized water wash 8-10 times after, the XRD spectrum of material and the Raman figure of Figure 10
Still containing the peak of KCl in spectrum, show that the carbon (KCl@C sample) of KCl cladding of the present invention slows down work with certain to the dissolution of KCl
With in slow-release fertilizer field with development potentiality and application prospect.
Claims (4)
1. a kind of method that water solubility KCl catalyzes and synthesizes carbon nanosheet, which comprises the following steps:
KCl is placed in a vacuum drying oven by step 1, is dried；
KCl of the step 1 after dry is placed in reacting furnace by step 2,3~5min of nitrogen or inert gas is then passed to, with complete
Exclude the air in reacting furnace；Wherein, the throughput of nitrogen or inert gas is 50~120mL/min；
Reacting furnace is heated to 500~650 DEG C by step 3, and 10~15min is kept the temperature at 500~650 DEG C；
Step 4 is passed through C into reacting furnace with the rate of 30~40mL/min2H2Gas reacts 30~60min；
Step 5, after reaction, Temperature fall is cooled to room temperature to in-furnace temperature, takes out sample；
Step 6, the sample for obtaining step 5 supersound washing in deionized water, it is dry, the carbon nanosheet can be obtained.
2. the carbon nanosheet that claim 1 the method obtains is in the application of energy storage field.
3. application of the carbon nanosheet that claim 1 the method obtains as lithium ion battery or the cathode of sodium-ion battery.
4. the sample that step 5 obtains in claim 1 the method is in the application in slow-release fertilizer field.
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Cited By (1)
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|---|---|---|---|---|
| WO2022177699A3 (en) * | 2021-01-26 | 2022-09-22 | University Of Kansas | Highly stable metal halide perovskite colloidal compositions |
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