CN110155983B - Preparation method of cotton-based porous biomass carbon - Google Patents
Preparation method of cotton-based porous biomass carbon Download PDFInfo
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- CN110155983B CN110155983B CN201910481973.4A CN201910481973A CN110155983B CN 110155983 B CN110155983 B CN 110155983B CN 201910481973 A CN201910481973 A CN 201910481973A CN 110155983 B CN110155983 B CN 110155983B
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- 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
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- 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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of cotton-based porous biomass carbon, which comprises the following steps: (1) Cleaning cotton in a certain weight part, and drying to obtain a product A; (2) Mixing and grinding the product A and metal chloride according to a certain mass ratio to obtain a product B; (3) Spreading the product B in an alumina porcelain boat, placing the alumina porcelain boat in a tube furnace in inert atmosphere, heating to 800-1300 ℃ at a certain heating rate, and carbonizing at high temperature to obtain a product C; (4) soaking the product C in hydrochloric acid solution to obtain a product D; (5) Repeatedly washing the product D with water until the pH=7, and drying to obtain the cotton-based porous biomass carbon material. The invention has the advantages that: according to the invention, cotton is used as a raw material, and the porous biomass carbon with a larger specific surface area is prepared by adopting grinding treatment with metal chloride to achieve the purpose of pore-forming, regulating and controlling different mass ratios of the cotton and the metal chloride and controlling proper calcination temperature.
Description
Technical Field
The invention relates to a preparation method of a sodium ion battery anode material, in particular to a preparation method of cotton-based porous biomass carbon.
Background
The concept of Sodium Ion Batteries (SIBs) was proposed in the 1970-1980 s in parallel with Lithium Ion Batteries (LIBs). Subsequently, LIB was successfully commercialized by sony in 1991, and then a great deal of research was conducted to develop LIB. However, there is little research on SIBIt has been carried out even for thirty years that research into sodium insertion materials for energy storage has almost disappeared. Recently, the explosive growth of numerous electrical devices involving various consumer electronics, power tools and electric vehicles has led to a great demand for LIBs, which may be hampered by limited lithium reserves (20 ppm in the earth's cluster). In view of this, researchers were again focusing on SIB, because of the sodium-rich resource (23600 ppm). In addition, the Na element is adjacent to Li in the alkali metal group so that they have many similar physicochemical properties. Thus, when effectively solving some of the problems, the SIB can replicate the success of the LIB. Not surprisingly, the electrochemical principle of SIB is similar to that of LIB, na during charging + Extracted from the positive electrode and migrate to the negative electrode to react with the negative electrode material. When discharging, the opposite process occurs, extracting Na from the negative electrode + And migrates to the positive electrode to return to the original state, accompanied by electron transfer in the external circuit to provide electrical energy.
Compared with LIB, SIB has the following characteristics: the sodium resource is abundant and the price is low; (2) SIB allows for the use of low concentration electrolyte, thereby reducing cost; (3) Na (Na) + The aluminum foil is not alloyed with aluminum, and the aluminum foil can be used as a current collector for the negative electrode, so that the cost and the weight are further reduced; (4) SIB has no overdischarge characteristics, allowing discharge to zero volts. The negative electrode material is a key factor of current restrictions. The SIB negative electrode material has the defects of low first charge and discharge efficiency, poor long-cycle performance and the like, so that the development of a novel SIB negative electrode material with high first efficiency and good cycle stability is urgent.
Since the sodium ion has a larger atomic radius than lithium ion, it is difficult for sodium ions to intercalate into the graphite layer spacing due to the small graphite layer spacing (0.34, nm). Hard carbon as the SIB anode material has many advantages over conventional graphite electrode materials. The hard carbon layer has larger spacing, loose and porous graphite-like layered structure which is staggered with each other, and can store a large amount of sodium ions. The selection of suitable precursors for the synthesis of hard carbon is particularly important.
Biomass resources are rich, carbon elements are abundant, most of the biomass resources belong to renewable resources, and carbon materials prepared from the biomass resources are widely focused by scientific researchers in various countries of the world by virtue of the advantages of good conductivity, high specific surface area and the like, and meanwhile, the biomass resources are green, sustainable, low in price, wide in distribution, easy to collect and the like, so that the biomass resources bring convenience to industrial mass production. In addition, the carbon material prepared from the biomass raw material also reflects the concept of green chemistry. Cotton, which is one of the most common crops, is widely planted in China, is cheap and easy to obtain, contains more than 90% of cellulose, is carbonized and converted into porous biochar, is used as a negative electrode material of SIB, and has important significance for solving the current energy crisis and environmental pollution problems.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the preparation method of the cotton-based porous biomass carbon, which has the advantages of simple preparation process, readily available raw materials, environmental friendliness and higher BET surface area of the product.
In order to solve the technical problems, the technical scheme of the invention is as follows: the preparation method of the cotton-based porous biomass carbon has the innovation points that: the preparation method comprises the following steps:
step 1: cleaning cotton in a certain weight part, and drying to obtain a product A;
step 2: mixing and grinding the product A and metal chloride according to a certain mass ratio to obtain a product B;
step 3: spreading the product B in an alumina porcelain boat, placing the alumina porcelain boat in a tube furnace in inert atmosphere, heating to 800-1300 ℃ at a certain heating rate, and carrying out high-temperature carbonization to obtain a product C;
step 4: soaking the product C in a hydrochloric acid solution to obtain a product D;
step 5: repeatedly washing the product D with water to pH=7, and vacuum drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
Further, the washing in the step 1 adopts distilled water washing.
Further, the drying process in the step 1 is to heat at a heating rate of 1-3 ℃/min, heat at a heating rate of 4-6 ℃/min, heat to 60-80 ℃ and dry at a constant temperature.
Further, the metal chloride in the step 2 is at least one of zinc chloride, ferric chloride, potassium chloride and sodium chloride.
Further, the mass ratio of the product A to the metal chloride in the step 2 is 1:2 to 5.
Further, the grinding time in the step 2 is 30-60 min.
Further, the temperature rising rate in the step 3 is 2-5 ℃/min, and the high-temperature carbonization time is 2-3 h.
Further, the inert atmosphere in the step 3 is nitrogen or argon or nitrogen-argon mixture with any ratio.
Further, in the step 4, the concentration of hydrochloric acid is 1-3 mol/L, and the soaking time is 10-24 h.
The invention has the advantages that:
(1) According to the preparation method of the cotton-based porous biomass carbon, based on the fiber spiral structure of cotton, the surface is modified by metal salt to form a hollow tubular porous structure, so that excellent electrochemical performance is shown; meanwhile, the Xinjiang long stapled cotton is directly used as a raw material, so that the environment is protected, the utilization rate of the cotton is improved, the reutilization of waste crops is realized, the production cost is reduced, the requirements of developing natural waste biomass new materials are met, and the economic, social and ecological benefits of the cotton are improved;
(2) According to the preparation method of the cotton-based porous biomass carbon, a stepped heating and drying process is adopted, the heating mode is mild, and the microcosmic appearance of cotton can be protected from being changed in the drying process;
(3) According to the preparation method of the cotton-based porous biomass carbon, cotton and solid metal chloride powder are directly ground and mixed, so that the hydrolysis of metal chloride in water is avoided, the effect of the metal chloride can be exerted to the maximum extent, the biomass carbon material with larger specific surface area is prepared, the infiltration of electrolyte is facilitated, and the battery performance is improved.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
Fig. 1 is a scanning electron microscope image of a cotton-based porous biomass carbon material prepared in example 2 of the present invention.
Fig. 2 is a graph of nitrogen adsorption and desorption of cotton-based porous biomass carbon prepared in example 2 of the present invention.
FIG. 3 is a graph showing pore size distribution of cotton-based porous biomass carbon prepared in example 2 of the present invention.
Detailed Description
The following examples will provide those skilled in the art with a more complete understanding of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 1 ℃/min, at a heating rate of 4 ℃/min, to 60 ℃ and then at a constant temperature to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:3, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 1000 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water until the pH value is=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
The specific surface area of the cotton-based porous biomass carbon material is 1115.67 m < 2 >/g through testing.
Example 2
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 2 ℃/min, at a heating rate of 5 ℃/min, to 70 ℃ and then at a constant temperature to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:4, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 1000 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water to pH=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material (SEM image is shown in figure 1).
The specific surface area of the cotton-based porous biomass carbon material is 2127.89 m < 2 >/g.
Example 3
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 3 ℃/min, at a heating rate of 6 ℃/min, to 80 ℃ and then drying at a constant temperature to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:5, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 1000 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water until the pH value is=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
The specific surface area of the cotton-based porous biomass carbon material was tested to be 1990.79 m2/g.
Example 4
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 1 ℃/min, at a heating rate of 4 ℃/min, to 60, and then performing constant-temperature drying to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:4, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 800 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water until the pH value is=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
The specific surface area of the cotton-based porous biomass carbon material is 1557.76 m2/g.
Example 5
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 2 ℃/min, at a heating rate of 5 ℃/min, to 70 ℃ and then at a constant temperature to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:4, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 1100 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water until the pH value is=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
The specific surface area of the cotton-based porous biomass carbon material is 1572.04 m2/g.
Example 6
1) Cleaning 0.5 g cotton with distilled water, and drying, wherein the drying is performed at a heating rate of 3 ℃/min, at a heating rate of 6 ℃/min, to 80 ℃ and then drying at a constant temperature to obtain a product A;
2) Mixing the product A and zinc chloride according to the mass ratio of 1:4, and grinding for 30min in a mortar to obtain a product B;
3) Spreading the product B in a white alumina porcelain boat, placing in a tube furnace in nitrogen atmosphere, heating to 1300 ℃ at a heating rate of 2 ℃/min, maintaining for 2 hours, and naturally cooling to obtain a product C;
4) Soaking the product C in 50ml of hydrochloric acid solution with the concentration of 2mol/L at 60 ℃ for 24 hours to obtain a product D;
5) Repeatedly washing the product D with distilled water until the pH value is=7, and drying at 60 ℃ to obtain the cotton-based porous biomass carbon material.
The specific surface area of the cotton-based porous biomass carbon material was tested to be 2264.91 m2/g.
Taking the cotton-based porous biomass carbon material prepared in the example 2 as an example, scanning by an electron microscope, wherein the scanning result is shown in fig. 1, and the prepared cotton-based porous biomass carbon material has a hollow tubular porous structure; the nitrogen adsorption and desorption are carried out, and the result is shown as figure 2, which shows an IV type N2 adsorption isotherm with an H3 hysteresis loop, and shows that micropores and mesopores exist in the sample; the pore size distribution of the prepared cotton-based porous biomass carbon is shown in fig. 3, and the display result corresponds to fig. 2, which shows that micropores and mesopores mainly exist in the cotton-based porous biomass carbon.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A preparation method of cotton-based porous biomass carbon is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: cleaning cotton in a certain weight part, and drying to obtain a product A;
step 2: mixing and grinding the product A and metal chloride according to a certain mass ratio to obtain a product B;
step 3: spreading the product B in an alumina porcelain boat, placing the alumina porcelain boat in a tube furnace in inert atmosphere, heating to 800-1300 ℃ at a certain heating rate, and carrying out high-temperature carbonization to obtain a product C;
step 4: soaking the product C in a hydrochloric acid solution to obtain a product D;
step 5: repeatedly washing the product D with water until the pH value is=7, and vacuum drying at 60 ℃ to obtain a cotton-based porous biomass carbon material;
the drying process in the step 1 is that firstly, the temperature is raised at a heating rate of 1-3 ℃/min, then the temperature is raised at a heating rate of 4-6 ℃/min, the temperature is raised to 60-80 ℃, and then the constant temperature drying is carried out;
the metal chloride in the step 2 is zinc chloride; mass ratio of product a to metal chloride 1:2 to 5; the grinding time is 30-60 min.
2. The method for preparing cotton-based porous biomass carbon according to claim 1, wherein: and in the step 1, distilled water is adopted for cleaning.
3. The method for preparing cotton-based porous biomass carbon according to claim 1, wherein: the heating rate in the step 3 is 2-5 ℃/min, and the high-temperature carbonization time is 2-3 h.
4. The method for preparing cotton-based porous biomass carbon according to claim 1, wherein: and the inert atmosphere in the step 3 is nitrogen or argon or nitrogen-argon mixture with any ratio.
5. The method for preparing cotton-based porous biomass carbon according to claim 1, wherein: in the step 4, the concentration of hydrochloric acid is 1-3 mol/L, and the soaking time is 10-24 h.
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| CN110668421A (en) * | 2019-10-29 | 2020-01-10 | 江苏科技大学 | Preparation method of biomass porous carbon material |
| CN111232948A (en) * | 2020-01-16 | 2020-06-05 | 厦门理工学院 | Cotton-derived porous carbon electrode material and synthesis method and application thereof |
| CN113421990A (en) * | 2021-05-28 | 2021-09-21 | 西安理工大学 | Iron-based biomass carbon intermediate layer of lithium-sulfur battery, preparation method and lithium-sulfur battery |
| CN113666355B (en) * | 2021-07-28 | 2023-11-21 | 新疆大学 | Preparation method of tomato skin residue derived porous carbon material |
| CN114883538B (en) * | 2022-03-31 | 2024-02-20 | 蜂巢能源科技股份有限公司 | Composite positive electrode material and preparation method and application thereof |
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| CH589007A5 (en) * | 1973-05-04 | 1977-06-30 | Boehlen Bruno | Active carbon prodn. from organic polymers - by carbonisation in presence of zinc chloride |
| US8784764B2 (en) * | 2008-12-15 | 2014-07-22 | Corning Incorporated | Methods for forming activated carbon material for high energy density ultracapacitors |
| CN104843673A (en) * | 2015-04-30 | 2015-08-19 | 昆明理工大学 | Porous carbon material preparing method |
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| CN106587055A (en) * | 2016-11-17 | 2017-04-26 | 华南理工大学 | Biomass-based porous carbon material, preparation method thereof, and application thereof in supercapacitor |
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