CN112897500B - Method for preparing cracked carbon in air and application - Google Patents
Method for preparing cracked carbon in air and application Download PDFInfo
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- CN112897500B CN112897500B CN202110074137.1A CN202110074137A CN112897500B CN 112897500 B CN112897500 B CN 112897500B CN 202110074137 A CN202110074137 A CN 202110074137A CN 112897500 B CN112897500 B CN 112897500B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
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- 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
The invention discloses a method for preparing cracked carbon in an air atmosphere and application thereof. The method comprises the following steps: uniformly mixing the carbon precursor and NaCl; the mixture is pressed into slices, then the mixture is coated with NaCl, and then the mixture is pressed into slices again, is subjected to cold isostatic pressing and pressure maintaining, and then is heated; and washing with deionized water, and drying in vacuum to obtain the carbon precursor-derived cracking carbon. And preparing the cracking carbon, super P, PVDF and a solvent into slurry, coating the slurry on a copper foil, cutting the copper foil into a pole piece after complete drying, and assembling the pole piece and a lithium piece into a battery. The method can prepare the cracking carbon in the air atmosphere, solves the problem that the cracking carbon can not be prepared in the air, has wide application range of carbon precursors, and shows excellent electrochemical performance when the prepared cracking carbon is used as a negative electrode material of a lithium ion battery.
Description
Technical Field
The invention relates to a method for preparing cracked carbon in air and application thereof, and belongs to the technical field of carbon material preparation and lithium ion battery cathode materials.
Background
Among the various materials, carbon materials are one of the most widely studied materials. The variety of carbon materials is many, and the carbon materials can be divided into zero-dimensional carbon quantum dots, one-dimensional carbon nanotubes and two-dimensional graphene according to dimensions; hard carbon and soft carbon can be classified according to graphitization; there are various hetero atoms (N, O, S, B, F, etc.) doped with carbon according to the composition. Even the same carbon material, structurally different, can be classified into many classes, for example, carbon nanotubes can be classified into single-walled and multi-walled, chiral and achiral, semiconducting and conducting carbon nanotubes, etc. Carbon materials have a wide variety of properties due to their diverse structures and compositions. Carbon materials are now widely used in the fields of energy, catalysis, and biology, and have become one of the most important materials.
The cracking carbon is also one of carbon materials, and is widely applied to the fields of energy, catalysis and the like. The cracking carbon is mainly prepared by cracking carbon-containing organic matters at high temperature, the cracking reaction almost needs to be carried out under inert atmosphere, and no related research can realize the preparation of the cracking carbon under the non-inert atmosphere at present. The preparation of carbon materials in air is challenging because carbon is oxidized to carbon dioxide at 400-500 ℃, and gases such as water vapor and carbon dioxide are released when carbon-containing organic substances are cracked.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prior art has the technical problem that the carbon material is difficult to prepare in the air.
In order to solve the technical problem, the invention provides a method for preparing cracked carbon in an air atmosphere, which is characterized by comprising the following steps of:
step 1): uniformly mixing the carbon precursor and NaCl;
step 2): pressing the mixture obtained in the step 1) into tablets, and then pressing into tablets again after coating potassium bromide outside the tablets;
step 3): carrying out cold isostatic pressing on the sheet obtained in the step 2), maintaining the pressure, and then heating;
and step 4): washing the sheet obtained in the step 3) with deionized water, and then drying in vacuum to obtain the carbon precursor derived cracking carbon.
Preferably, the carbon precursor in step 1) is a carbon-containing small molecule, a carbon-containing polymer, a carbon-containing biomass or a carbon-containing metal organic framework material.
Preferably, the mixing in step 1) is performed by grinding or ball milling.
Preferably, the pressure of tabletting in the step 2) is 4MPa.
Preferably, the pressure of the cold isostatic pressing in the step 3) is 200MPa, and the pressure maintaining time is 0.5 hour.
Preferably, the heating in step 3) is specifically: after the temperature is raised to 700 ℃, the temperature is kept for 2 hours.
The invention also provides application of the pyrolytic carbon prepared by the method for preparing the pyrolytic carbon in the air atmosphere, which is characterized in that the pyrolytic carbon, super P, PVDF and a solvent are prepared into slurry, the slurry is coated on a copper foil, and the copper foil is cut into pole pieces after being completely dried and assembled with lithium pieces into a battery.
Preferably, the mass ratio of the cracking carbon to the super P and PVDF is 8:1:1.
preferably, the solvent is azomethylpyrrolidone.
The method can prepare the cracking carbon in the air atmosphere, solves the problem that the cracking carbon can not be prepared in the air, has wide application range of carbon precursors, and shows excellent electrochemical performance when the prepared cracking carbon is used as a negative electrode material of a lithium ion battery.
Drawings
FIG. 1 is a schematic diagram of the preparation of cracked carbon in air;
FIG. 2 is a photograph and a graph of yield versus yield for various carbon precursor-derived cracked carbons;
FIG. 3 is an electron microscope image of various carbon precursor-derived cracked carbons;
fig. 4 is a comprehensive characterization of Glucose (Glucose/NaCl (3);
fig. 5 is a graph showing electrochemical performance characterization of Glucose (Glucose/NaCl (3).
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1
Weighing (glucose and sodium chloride), zirconia ball milling beads and isopropanol (mass ratio of 1. And (4) putting the ball-milled slurry into a forced air drying oven for complete drying. The dried mixture was ground in a mortar. 300mg of glucose/sodium chloride mixed fine powder is pressed into tablets with the diameter of 12.7mm by using the pressure of 4MPa. The glucose/sodium chloride tablets were coated with potassium bromide, pressed with the same into tablets with a diameter of 20mm and then treated with cold isostatic pressing at 200MPa for 0.5h. The cold isostatic pressing treated sheet is heated to 700 ℃ at a rate of 3 ℃/min and kept for 2 hours. Soaking the high-temperature calcined tablet in water to remove salt in the tablet, repeatedly washing the tablet with deionized water for 3 times, and then completely drying the tablet to obtain the glucose-derived pyrolysis carbon. The mass ratio of glucose to sodium chloride can be from 2.
Glucose-derived cracked carbon, super P and PVDF were formulated into a slurry in a mass ratio of 8. And coating the uniformly mixed slurry on a copper foil, completely drying, cutting into pole pieces with the diameter of 12mm, assembling the pole pieces and a lithium piece into a 2032 button battery, and carrying out electrochemical performance test.
Example 2
Weighing (polyvinylidene fluoride and sodium chloride), zirconia ball milling beads and isopropanol (mass ratio of 1. And (4) putting the ball-milled slurry into a forced air drying box for complete drying. The dried mixture was ground with a mortar. 300mg of polyvinylidene fluoride/sodium chloride mixed fine powder is pressed into a sheet with the diameter of 12.7mm by using the pressure of 4MPa. Coating polyvinylidene fluoride/sodium chloride sheet with potassium bromide, pressing into sheet with diameter of 20mm, and cold isostatic pressing at 200MPa for 0.5 hr. The cold isostatic pressing treated sheet is heated to 700 ℃ at the speed of 3 ℃/min and is kept for 2 hours. And (3) soaking the high-temperature calcined sheet in water to remove salt in the sheet, repeatedly washing the sheet for 3 times by using deionized water, and then completely drying the sheet to obtain the pyrolysis carbon derived from the polyvinylidene fluoride. The mass ratio of polyvinylidene fluoride to sodium chloride can be from 2.
Polyvinylidene fluoride-derived pyrolysis carbon, super P and PVDF are prepared into slurry according to the mass ratio of 8. And coating the uniformly mixed slurry on a copper foil, completely drying, cutting into pole pieces with the diameter of 12mm, assembling the pole pieces and a lithium piece into a 2032 button battery, and carrying out electrochemical performance test.
Example 3
The camphor tree leaves are washed clean by deionized water and then are put into an oven at 60 ℃ for complete drying. And (3) putting the dried camphor tree leaves into a muffle furnace, heating to 260 ℃ at a heating rate of 10 ℃/min, and preserving heat for 6 hours to obtain a product named as Leaf-260.
Weighing (Leaf-260 and sodium chloride), zirconia ball milling beads and isopropanol (mass ratio of 1:2: 1) in a ball milling tank, and carrying out ball milling at 600rpm for 6h. And (4) putting the ball-milled slurry into a forced air drying oven for complete drying. The dried mixture was ground in a mortar. 300mg of Leaf-260/sodium chloride mixed fine powder was pressed into a tablet having a diameter of 12.7mm under a pressure of 4MPa. The Leaf-260/sodium chloride tablets were coated with potassium bromide, pressed into tablets of 20mm diameter with the same, and then treated with cold isostatic pressing at 200MPa for 0.5h. The cold isostatic pressing treated sheet is heated to 700 ℃ at the speed of 3 ℃/min and is kept for 2 hours. Soaking the high-temperature calcined slices in water, removing salt in the slices, repeatedly washing the slices with deionized water for 3 times, and then completely drying to obtain the pyrolysis carbon derived from the camphor tree leaves. The mass ratio of Leaf-260 to sodium chloride can be from 2.
The camphor tree leaf derived pyrolysis carbon, super P and PVDF are prepared into slurry according to the mass ratio of 8. And coating the uniformly mixed slurry on a copper foil, completely drying, cutting into pole pieces with the diameter of 12mm, assembling the pole pieces and a lithium piece into a 2032 button battery, and carrying out electrochemical performance test.
Example 4
First, micron-sized ZIF-67 was prepared. 5g of polyvinylpyrrolidone (Mw: 1,300,000) and 5.88g of copper nitrate hexahydrate are weighed into 500mL of methanol and dissolved with stirring to obtain solution A. 6.626g of 2-methylimidazole was weighed out and dissolved in 500mL of methanol with stirring to obtain a solution B. Solution B was poured into stirring solution a. The mixed solution was stirred for 10 minutes and then allowed to stand at room temperature for 24 hours. The solution was centrifuged and washed three times with methanol to give a precipitate. Finally the precipitate was dried under vacuum at 60 ℃ for 24 hours.
Weighing ZIF-67 and sodium chloride (in a mass ratio of 2. 300mg of the mixed fine powder of ZIF-67/sodium chloride was pressed into a tablet having a diameter of 12.7mm under a pressure of 4MPa. The ZIF-67/sodium chloride tablets were coated with potassium bromide, pressed into tablets of 20mm diameter with the same press, and then treated with cold isostatic pressing at 200MPa for 0.5h. The cold isostatic pressing treated sheet is heated to 700 ℃ at a rate of 3 ℃/min and kept for 2 hours. And (3) soaking the high-temperature calcined slice in water to remove salt in the slice, repeatedly washing the slice for 3 times by using deionized water, and then completely drying the slice to obtain the ZIF-67 derived pyrolysis carbon. The mass ratio of ZIF-67 to sodium chloride may be from 2.
ZIF-67 derived cracked carbon, super P and PVDF were prepared into a slurry in a mass ratio of 8. And coating the uniformly mixed slurry on a copper foil, completely drying, cutting into pole pieces with the diameter of 12mm, assembling the pole pieces and a lithium piece into a 2032 button battery, and carrying out electrochemical performance test.
FIG. 1 is a schematic diagram of the preparation of cracked carbon in air.
FIG. 2 is a photograph and a graph of yield versus yield for various carbon precursor-derived cracked carbons; the method comprises the following steps of A, B, C and D, wherein A is a picture and a yield-yield graph of micromolecule glucose derived cracked carbon, B is a picture and a yield-yield graph of macromolecule polyvinylidene fluoride derived cracked carbon, C is a picture and a yield-yield graph of biomass camphor tree leaf derived cracked carbon, and D is a picture and a yield-yield graph of metal organic framework material ZIF-67 derived cracked carbon.
FIG. 3 is an electron micrograph of various carbon precursor-derived cracked carbons; wherein (a) is a scanning electron micrograph of Glucose (Glucose/NaCl (3)), (B) is a scanning electron micrograph of polyvinylidene fluoride (PVDF/NaCl (1)), (C) is a scanning electron micrograph of camphor tree Leaf (Leaf-260/NaCl (2.
Fig. 4 is a comprehensive characterization of Glucose (Glucose/NaCl (3); wherein A is an X-ray diffraction pattern, B is a Raman pattern, C is a nitrogen absorption-desorption isothermal curve, and D is a pore size distribution.
Fig. 5 is a graph showing electrochemical performance characterization of Glucose (Glucose/NaCl (3); wherein, A is an impedance diagram of a new battery before circulation, B is an impedance diagram of the battery after 1000 circles of circulation under the current density of 1000mA/g, C is a multiplying power performance diagram of the battery under different current densities, and D is a long circulation diagram of the battery under the current density of 1000 mA/g.
Claims (8)
1. A method for preparing cracked carbon in an air atmosphere is characterized by comprising the following steps:
step 1): uniformly mixing the carbon precursor and NaCl;
step 2): pressing the mixture obtained in the step 1) into tablets, and then pressing into tablets again after coating potassium bromide outside the tablets;
step 3): carrying out cold isostatic pressing on the sheet obtained in the step 2), maintaining the pressure, and then heating; the heating is specifically as follows: heating to 700 ℃ at the speed of 3 ℃/min, and then preserving heat for 2 hours;
step 4): washing the sheet obtained in the step 3) with deionized water, and then drying in vacuum to obtain the carbon precursor derived cracking carbon.
2. The method for preparing pyrolytic carbon in air atmosphere of claim 1, wherein the carbon precursor in step 1) is a carbon-containing small molecule, a carbon-containing macromolecule, a carbon-containing biomass or a carbon-containing metal organic framework material.
3. The method for preparing pyrolytic carbon under air atmosphere of claim 1, wherein the mixing in step 1) is by grinding or ball milling.
4. The method for preparing a pyrolysis carbon under an air atmosphere according to claim 1, wherein the pressure of the tablet in the step 2) is 4MPa.
5. The method for preparing cracked carbon under an air atmosphere in accordance with claim 1, wherein the cold isostatic pressing in step 3) is carried out at a pressure of 200MPa and a dwell time of 0.5 hours.
6. The use of the pyrolytic carbon prepared by the method of preparing pyrolytic carbon according to any one of claims 1 to 5, wherein the pyrolytic carbon is prepared into a slurry with super P, PVDF and a solvent, the slurry is coated on a copper foil, and after being completely dried, the slurry is cut into pole pieces, and the pole pieces and lithium pieces are assembled into a battery.
7. The use of claim 6, wherein the mass ratio of the cracked carbon to the super P, PVDF is 8:1:1.
8. use according to claim 6, wherein the solvent is azomethylpyrrolidone.
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