CN113148976B - Biomass porous hard carbon material and preparation method and application thereof - Google Patents

Biomass porous hard carbon material and preparation method and application thereof Download PDF

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CN113148976B
CN113148976B CN202110447439.9A CN202110447439A CN113148976B CN 113148976 B CN113148976 B CN 113148976B CN 202110447439 A CN202110447439 A CN 202110447439A CN 113148976 B CN113148976 B CN 113148976B
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hard carbon
carbon material
porous hard
water
koh
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CN113148976A (en
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傅倩茹
张久俊
颜蔚
郑辉
王健宜
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Beijing Nadian New Energy Technology Co.,Ltd.
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University of Shanghai for Science and Technology
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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
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • 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
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

The invention provides a biomass porous hard carbon material and a preparation method and application thereof, belonging to the technical field of energy storage materials. The preparation method of the biomass porous hard carbon material provided by the invention comprises the following steps: mixing whole wheat flour, KOH and water to obtain a liquid mixture; removing water from the liquid mixture to obtain a solid gel; and calcining the solid gel in a protective atmosphere, and washing to obtain the biomass porous hard carbon material. According to the invention, the whole wheat flour is used as the biomass raw material to prepare the porous hard carbon material, the whole wheat flour has wide sources and low raw material cost, the porous hard carbon material can be prepared by one-step calcination under the action of KOH, the operation is simple, the production cost is low, and the finally prepared disordered porous hard carbon material has a large specific surface area and excellent sodium storage performance.

Description

Biomass porous hard carbon material and preparation method and application thereof
Technical Field
The invention relates to the technical field of energy storage materials, in particular to a biomass porous hard carbon material and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIBs) have been widely used in electric vehicles, portable electronic products, and the like. However, the low abundance and high cost of lithium limit the large-scale application of lithium ion batteries in energy storage grids. In recent years, sodium Ion Batteries (SIBs) have attracted much attention due to their high energy density and abundance of sodium resources. However, since the radius of sodium ions is 1.3 times that of lithium ions, there is a problem that reaction kinetics are slow during discharging/charging, thereby resulting in poor electrochemical performance.
The biomass carbon material is widely concerned by people due to the advantages of environmental friendliness, excellent electrochemical performance and the like, and can be applied to a negative electrode material of a sodium-ion battery to improve the electrochemical performance of the negative electrode material. In the prior art, the biomass raw material is adopted to prepare the carbon material, and the problems of complex operation and higher cost generally exist.
Disclosure of Invention
The invention aims to provide a biomass porous hard carbon material and a preparation method and application thereof, the invention takes whole wheat flour as a biomass raw material, and the porous hard carbon material can be prepared by one-step calcination under the action of KOH, the operation is simple, and the cost is low; and the prepared porous hard carbon material has a large specific surface area and excellent sodium storage performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a biomass porous hard carbon material, which comprises the following steps:
mixing whole wheat flour, KOH and water to obtain a liquid mixture;
removing water from the liquid mixture to obtain a solid gel;
and calcining the solid gel in a protective atmosphere, and washing to obtain the biomass porous hard carbon material.
Preferably, the mass ratio of the KOH to the whole wheat flour is (1-2): 1.
preferably, the usage ratio of the whole wheat flour to the water is 1g: (5-15) mL.
Preferably, the temperature of the water is 70-90 ℃ when the whole wheat flour, KOH and water are mixed.
Preferably, the water in the liquid mixture is removed by drying, and the drying temperature is 70-90 ℃.
Preferably, the calcining temperature is 600-800 ℃, and the holding time is 1-2 h.
Preferably, the rate of temperature rise to the temperature of the calcination is 4 to 6 ℃/min.
Preferably, the washing comprises a hydrochloric acid washing and a water washing sequentially.
The invention provides the biomass porous hard carbon material prepared by the preparation method in the technical scheme, and the specific surface area of the biomass porous hard carbon material is 638.97-1929.47 m 2 g -1 。
The invention provides application of the biomass porous hard carbon material in the technical scheme as a negative electrode material of a sodium-ion battery.
The invention provides a preparation method of a biomass porous hard carbon material, which comprises the following steps: mixing whole wheat flour, KOH and water to obtain a liquid mixture; removing water from the liquid mixture to obtain a solid gel; and calcining the solid gel in a protective atmosphere, and then washing to obtain the biomass porous hard carbon material. According to the invention, the porous hard carbon material is prepared by taking the whole wheat flour as the biomass raw material, the whole wheat flour has wide sources and low raw material cost, the porous hard carbon material can be prepared by one-step calcination under the action of KOH, the operation is simple, the production cost is low, the finally prepared disordered porous hard carbon material has a large specific surface area and excellent sodium storage performance, and the disordered porous hard carbon material can be used as a sodium ion battery cathode material and shows excellent cycle performance and rate capability.
Drawings
FIG. 1 is an XRD pattern of biomass porous hard carbon materials prepared in examples 1-5;
FIG. 2 is an SEM image of biomass porous hard carbon materials prepared in examples 1-5;
FIG. 3 is a BET diagram of the biomass porous hard carbon material prepared in examples 1 to 5;
FIG. 4 is a graph of the long cycle performance of the sodium ion battery with the biomass porous hard carbon material prepared in examples 1-5 as the sodium electric anode material under the condition that the current density is 0.1A/g;
FIG. 5 is a graph of the long cycle performance of the sodium ion battery with the current density of 1A/g, using the biomass porous hard carbon material prepared in examples 1-5 as the sodium electric anode material;
fig. 6 is a rate performance diagram of the sodium ion battery with the biomass porous hard carbon materials prepared in examples 1 to 5 as the sodium electric negative electrode material under different current density conditions.
Detailed Description
The invention provides a preparation method of a biomass porous hard carbon material, which comprises the following steps:
mixing whole wheat flour, KOH and water to obtain a liquid mixture;
removing water from the liquid mixture to obtain a solid gel;
and calcining the solid gel in a protective atmosphere, and washing to obtain the biomass porous hard carbon material.
According to the invention, the whole wheat flour is used as the biomass raw material to prepare the porous hard carbon material, the whole wheat flour is wide in source and low in raw material cost, the porous hard carbon material can be prepared by one-step calcination under the action of KOH, the operation is simple, the production cost is low, and the finally prepared disordered porous hard carbon material has a large specific surface area and excellent sodium storage performance, and has good electrochemical performance when used as a sodium ion battery cathode material.
The present invention mixes whole wheat flour, KOH, and water to obtain a liquid mixture. The source of the whole wheat flour is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the mass ratio of KOH to whole wheat flour is preferably (1 to 2): 1, specifically 1. In the present invention, the ratio of the whole wheat flour to water is preferably 1g: (5-15) mL, more preferably 1g:10mL. In the present invention, the temperature of the water is preferably 70 to 90 ℃, more preferably 80 ℃. The method for mixing the whole wheat flour, the KOH and the water is not particularly limited, all the components can be uniformly mixed, the components can be stirred and mixed, and the obtained liquid mixture is transparent solution. In the invention, KOH is used as an activating agent, and the whole wheat flour is calcined under the action of the KOH, so that the finally obtained carbon material is ensured to have a porous structure; in addition, the invention directly mixes the whole wheat flour, KOH and water, and KOH can promote the hydrolysis of the flour polysaccharide chain; meanwhile, the hydrolysis of the whole wheat flour polysaccharide chain can be further accelerated by preferably controlling the temperature of water to be 70-90 ℃, so that the etching of KOH on the whole wheat flour in the subsequent calcining process is facilitated.
After obtaining the liquid mixture, the invention removes the water in the liquid mixture to obtain solid gel. In the present invention, the manner of removing water from the liquid mixture is preferably drying, and the temperature of the drying is preferably 70 to 90 ℃, more preferably 80 ℃. The drying time is not particularly limited, and the moisture can be fully removed, and the drying time can be specifically 10-15 h, and preferably 12h. In the present invention, after removing the water from the liquid mixture, a brown solid gel is obtained.
After the solid gel is obtained, the solid gel is calcined in a protective atmosphere and then washed to obtain the biomass porous hard carbon material. In the present invention, the protective gas providing the protective atmosphere is preferably nitrogen. In the invention, the calcination temperature is preferably 600-800 ℃, and specifically can be 600 ℃, 700 ℃ or 800 ℃; according to the invention, the temperature is preferably raised from room temperature to the temperature required by calcination, and the heating rate of raising the temperature to the temperature required by calcination is preferably 4-6 ℃/min, and more preferably 5 ℃/min; the heat preservation time of the calcination is preferably 1-2 h, and specifically can be 1h, 1.5h or 2h. In the present invention, during calcination, KOH reacts with and etches away a portion of the carbon in the whole wheat flour, and the resulting salt and excess KOH are removed by washing, thereby forming a hard carbon material with a porous structure.
In the present invention, the washing preferably includes hydrochloric acid washing and water washing sequentially. According to the invention, preferably, the calcined material is cooled to room temperature and then washed with hydrochloric acid; the hydrochloric acid washing adopts hydrochloric acid with the concentration of 1mol/L, and the invention preferably removes residual KOH in the material obtained after calcination by hydrochloric acid washing. In the invention, the water used for water washing is preferably deionized water, and the material obtained after hydrochloric acid washing is preferably washed to be neutral by water washing.
In the present invention, the washing preferably further includes drying. The present invention is not particularly limited to the above drying, and can sufficiently dry the material.
The invention provides the biomass porous hard carbon material prepared by the preparation method in the technical scheme, and the specific surface area of the biomass porous hard carbon material is 638.97-1929.47 m 2 g -1 Preferably 816.28 to 1929.47m 2 g -1 More preferably 1431.88 to 1929.47m 2 g -1 More preferably 1517.42 to 1929.47m 2 g -1 。
The invention provides application of the biomass porous hard carbon material in the technical scheme as a negative electrode material of a sodium-ion battery. The specific application method of the biomass porous hard carbon material as the negative electrode material of the sodium-ion battery is not particularly limited, and the method known by the technical personnel in the field can be adopted.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding whole wheat flour and KOH into water at the temperature of 80 ℃, and uniformly stirring and mixing to obtain a liquid mixture; wherein the mass ratio of KOH to whole wheat flour is 1: 10mL;
drying the liquid mixture in an oven at 80 ℃ for 12h to remove water in the liquid mixture to obtain solid gel;
under the protection of nitrogen, heating the solid gel from room temperature (25 ℃) to 700 ℃ at the heating rate of 5 ℃/min, and carrying out heat preservation and calcination for 2h; and then cooling to room temperature, washing the calcined material by using hydrochloric acid with the concentration of 1mol/L to remove redundant KOH, then washing to neutrality by using deionization, and drying to obtain the biomass porous hard carbon material, which is recorded as PHC-700-1.
Example 2
Preparing a biomass porous hard carbon material according to the method of example 1, except that the mass ratio of the KOH and the whole wheat flour is 1.5; the finally obtained biomass porous hard carbon material is marked as PHC-600-1.5.
Example 3
A biomass porous hard carbon material was prepared according to the method of example 1, except that the mass ratio of KOH to whole wheat flour was 1.5; the finally obtained biomass porous hard carbon material is marked as PHC-700-1.5.
Example 4
A biomass porous hard carbon material was prepared according to the method of example 1, except that the mass ratio of KOH to whole wheat flour was 1.5; the finally obtained biomass porous hard carbon material is marked as PHC-800-1.5.
Example 5
A biomass porous hard carbon material was prepared according to the method of example 1, except that the mass ratio of KOH to whole wheat flour was 2; and marking the finally obtained biomass porous hard carbon material as PHC-700-2.
The biomass porous hard carbon materials prepared in examples 1 to 5 were characterized and tested for their performance, as follows:
fig. 1 is an XRD pattern of the biomass porous hard carbon material prepared in examples 1 to 5. As can be seen from fig. 1, as the calcination temperature increases, the peak value moves to a higher angle, and the peak value intensity increases, which indicates that the interlayer spacing of the biomass porous hard carbon material decreases and gradually becomes ordered; as the KOH ratio increases, the peak moves to higher angles and the peak intensity increases, indicating that the interlamellar spacing of the biomass porous hard carbon material decreases and gradually tends to be ordered.
Fig. 2 is an SEM image of the biomass porous hard carbon material prepared in examples 1 to 5, in which the scale is 1 μm, and a to e are SEM images of the biomass porous hard carbon material in examples 1 to 5 in sequence. As shown in FIG. 2, the PHC-600-1.5 material in a has a porous structure; the PHC-700-1.5 material in the b presents a highly developed porous structure; in the step c, the PHC-800-1.5 material has higher calcination temperature, the pore wall is thinner and folds appear; d shows that the activator KOH dosage is less and the activation is not sufficient when the PHC-700-1 material is prepared; as can be seen from e, the amount of KOH used as an activator is large, and the pore wall is thin and has more wrinkles when the PHC-700-2 material is prepared.
Fig. 3 is a BET graph of the biomass porous hard carbon materials prepared in examples 1 to 5. As can be seen from FIG. 3, the PHC-700-1 material prepared in example 1 had a specific surface area of 638.97m 2 g -1 The PHC-600-1.5 material prepared in example 2 has a specific surface area of 816.28m 2 g -1 The PHC-700-1.5 material prepared in example 3 had a specific surface area of 1431.88m 2 g -1 The PHC-700-1 material prepared in example 4 has a specific surface area of 1517.42m 2 g -1 The PHC-700-2 material prepared in example 5 had a specific surface area of 1929.47m 2 g -1 。
The biomass porous hard carbon materials prepared in the embodiments 1 to 5 are used as sodium electric negative electrode materials to prepare sodium ion batteries for performance test, and specifically, the biomass porous hard carbon materials prepared in the embodiments 1 to 5 are respectively ground into powder, acetylene black, polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) are added to be ground into slurry, the slurry is coated on copper foil, the sodium ion batteries are assembled in a glove box, and the blue-electricity system is used for sodium ion battery cycle performance test.
FIG. 4 is a long cycle performance diagram of the sodium ion battery with the biomass porous hard carbon material prepared in examples 1-5 as the sodium electric anode material under the condition that the current density is 0.1A/g. As can be seen from FIG. 4, when 700 cycles are performed under the condition that the current density is 0.1A/g, the reversible specific capacity of the PHC-700-1 material prepared in example 1 can reach 122.2mAh g -1 The reversible specific capacity of the PHC-600-1.5 material prepared in example 2 can reach 178.7mAh g -1 The reversible specific capacity of the PHC-700-1.5 material prepared in example 3 can reach 238.2mAh g -1 The reversible specific capacity of the PHC-700-1 material prepared in example 4 can reach 133.8mAh g -1 The reversible specific capacity of the PHC-700-2 material prepared in example 5 can reach 136.9mAh g -1 The coulombic efficiencies were all close to 100%.
Fig. 5 is a long cycle performance diagram of the sodium ion battery with the biomass porous hard carbon materials prepared in examples 1 to 5 as the sodium electricity negative electrode material under the condition that the current density is 1A/g. As can be seen from FIG. 5, when 2000 cycles were performed at a current density of 1A/g, the reversible specific capacity of the PHC-700-1 material prepared in example 1 was 93.6mAh g -1 The reversible specific capacity of the PHC-600-1.5 material prepared in example 2 can reach 141.7mAh g -1 The reversible specific capacity of the PHC-700-1.5 material prepared in example 3 can reach 184mAh g -1 The reversible specific capacity of the PHC-700-1 material prepared in example 4 can reach 105.1mAh g -1 The reversible specific capacity of the PHC-700-2 material prepared in example 5 can reach 118.9mAh g -1 The coulombic efficiencies were all close to 100%.
FIG. 6 shows the raw materials prepared in examples 1 to 5The material porous hard carbon material is used as a sodium electric anode material, and the multiplying power performance of the sodium ion battery is shown under different current density conditions. As can be seen from FIG. 6, when the current densities were 0.1, 0.2, 0.3, 0.5, 1, 2, 5, 10, 20 and 40Ag -1 The PHC-700-1 material prepared in example 1 had reversible specific capacities of 130.5, 120.3, 114.0, 103.7, 93.7, 75.4, 56.6, 29.0, 19.0, and 9.5mAh g, respectively -1 When the current density returns to 0.1Ag -1 The reversible specific capacity is kept at 146.1mAh g -1 (ii) a The reversible specific capacities of the PHC-600-1.5 materials prepared in example 2 were 185.6, 174.8, 162.1, 149.0, 139.2, 128.6, 115.6, 93.0, 72.6 and 52.0mAh g, respectively -1 When the current density returns to 0.1Ag again -1 The reversible specific capacity is kept at 182.6mAh g -1 (ii) a The PHC-700-1.5 material prepared in example 3 had reversible specific capacities of 309.8, 276.3, 233.3, 208.2, 190.7, 180.2, 160.4, 99.5, 77.7 and 59mAh g, respectively -1 When the current density returns to 0.1Ag -1 The reversible specific capacity is kept at 268.6mAh g -1 (ii) a The reversible specific capacities of the PHC-700-1 material prepared in example 4 were 140.9, 124.3, 115.3, 104.7, 93.1, 78.2, 65, 58.2, 33 and 20.6mAh g, respectively -1 When the current density returns to 0.1Ag -1 The reversible specific capacity is kept at 139.8mAh g -1 (ii) a The reversible specific capacities of the PHC-700-2 material prepared in example 5 were 200.8, 163.8, 145.8, 132.9, 119.6, 107.2, 89.1, 63.3, 42.8 and 25.7mAh g, respectively -1 When the current density returns to 0.1Ag -1 The reversible specific capacity is kept at 180.4mAh g -1 。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (6)

1. The application of the biomass porous hard carbon material as the negative electrode material of the sodium ion battery, and the preparation method of the biomass porous hard carbon material comprises the following steps:
mixing whole wheat flour, KOH and water to obtain a liquid mixture; the mass ratio of the KOH to the whole wheat flour is (1.5 to 2): 1;
removing water from the liquid mixture to obtain a solid gel;
calcining the solid gel in a protective atmosphere at the temperature of 700-800 ℃ for 1-2h, and then washing to obtain a biomass porous hard carbon material;
the specific surface area of the biomass porous hard carbon material is 1431.88 to 1929.47m 2 g -1 。
2. Use according to claim 1, wherein the ratio of wholemeal flour to water is 1g: (5 to 15) mL.
3. Use according to claim 2, characterized in that the temperature of the water when mixing the wholemeal flour, KOH and water is 70 to 90 ℃.
4. The use according to claim 1, characterized in that the water is removed from the liquid mixture by drying at a temperature of 70 to 90 ℃.
5. Use according to claim 1, characterized in that the rate of temperature rise to the calcination temperature is 4 to 6 ℃/min.
6. Use according to claim 1, wherein the washing comprises a hydrochloric acid wash and a water wash carried out in sequence.
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