CN113562730A - Preparation of microporous gram bacteria carbon material with high specific surface area and application of microporous gram bacteria carbon material in supercapacitor - Google Patents
Preparation of microporous gram bacteria carbon material with high specific surface area and application of microporous gram bacteria carbon material in supercapacitor Download PDFInfo
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- CN113562730A CN113562730A CN202110257433.5A CN202110257433A CN113562730A CN 113562730 A CN113562730 A CN 113562730A CN 202110257433 A CN202110257433 A CN 202110257433A CN 113562730 A CN113562730 A CN 113562730A
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- gram
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a biomass charcoal material taking gram-positive bacteria as a precursor and application research of the biomass charcoal material as a supercapacitor electrode material. The material retains the cell wall structure of gram-positive bacteria to a certain extent, has an ultra-high specific surface area and is mainly of a microporous structure. In particular to a method for alkali activation high-temperature carbonization, which comprises the following steps: firstly, pre-carbonizing a material, mixing the material with alkali, carbonizing the material at a certain temperature, and neutralizing, washing and drying the carbonized material to obtain the product; the gram-positive bacterial carbon has excellent electrochemical performance as a supercapacitor electrode material and has potential application value in the field of energy application.
Description
Technical Field
The invention relates to a preparation method of a microporous gram bacteria carbon material with a high specific surface area, and also relates to an application of the microporous gram bacteria carbon material with the high specific surface area as an electrode material in a super capacitor, wherein the material has excellent electrochemical characteristics and energy storage application potential, and belongs to the field of catalytic energy storage.
Background
With the increasing prominence of the environmental pollution problem, the adjustment of energy structure and the development of new energy have become the key to solve the problem, wherein energy storage is one of the important ways to solve the problem. The super capacitor has very fast charge and discharge rate, wide working temperature range, good cycle stability and safety, and has a large application market in the fields of new energy automobiles, mobile electronic equipment, standby power systems and the like.
Carbon materials are considered to be one of the most promising materials for industrial applications because of their wide source, low cost, ease of preparation and non-toxicity. The structural characteristics of the carbon material will inherit the structural characteristics of the raw materials to a certain extent, so that the selection of the raw materials is more critical to the material structure, and becomes one of the research hotspots in the material field in recent years. Various biomass carbon materials have been reported, for example, carbon materials prepared using tea leaves, coconut shells, human hair, bamboo, cotton stalks, soybeans, waxberries, etc. as raw materials. In addition, it is desirable to enrich the element and functional group types of the carbon material by doping with hetero atoms so as to impart special application functions to the material. Such as nitrogen doping, the feedstock is co-heated with urea (nitrogen source) to produce a nitrogen-doped carbon material. It is also possible to purposefully select biomass materials with heteroatoms (e.g., N, P, S, B, etc.) by material selection.
Gram bacteria, especially gram-positive bacteria, have a thick (20-80nm) and dense peptidoglycan layer (15-50 layers), each 1nm thick, accounting for about 50-80% of the dry cell weight. Peptidoglycan is also called as sticky peptide, peptidoglycan scaffolds of various bacterial cell walls are the same, the composition and connection mode of tetrapeptide side chains are different according to strains, so that gram bacteria have a compact and ordered arrangement mode in structure, elements such as nitrogen, oxygen, sulfur, phosphorus and the like in different combination modes can be introduced due to the diversity of the tetrapeptide side chains in the composition, and the gram bacteria are used as carbon source materials and can possibly endow corresponding materials with special structure and functional characteristics.
Disclosure of Invention
In order to meet the use requirement of a supercapacitor material with a high charge-discharge rate, the first purpose of the invention is to prepare a material which has a high specific surface area and can provide a rapid ion transfer channel for an interface reaction process, and the material is required to have a large enough specific surface area and abundant pores so as to provide a convenient place for a charge transfer process.
The second purpose of the invention is to provide a simple and effective preparation method with low cost and universality for preparing gram-positive bacteria microporous carbon with high specific surface area.
The third purpose of the present invention is to provide an application of the microporous gram bacteria carbon material with high specific surface area in the field of supercapacitors, such that the microporous gram bacteria carbon material has excellent electrochemical characteristics and great potential for energy storage applications.
In order to realize the technical purpose, the invention provides a preparation method of a microporous gram bacteria charcoal material with high specific surface area, which selects raw materials containing gram bacteria, firstly pre-carbonizes the materials, then mixes the materials with alkali for processing and carbonizes at a certain temperature, and prepares the microporous gram bacteria charcoal material with high specific surface area after neutralization, washing and drying.
The invention is characterized by comprising the following raw materials: the gram-positive bacteria of the present invention may be obtained from a single pure cell, a mixed cell, or a cell containing other additives, such as a commercially available cell material and a cell preparation. Has no strict requirements on the source and the purity of the thallus and has certain universality. As the industrial fermentation technology of the thalli is mature at the present stage, the variety of the obtained thalli is relatively rich, the source of raw materials is relatively rich, the selection space of the variety and the shape of the thalli is large, the culture components of the thalli are changed through the culture technology, the chemical components of the thalli are various, the variety of elements is rich, and the method lays a foundation for the application of gram bacteria derived carbon materials in different scenes. In addition, the universality of the preparation method allows the production of gram bacteria thallus to be from industrial fermentation byproducts and the like, increases the additional value of industrial production, reduces the production cost and ensures that the preparation of thallus biomass charcoal materials is more economic and environment-friendly.
The preparation method is optimized, gram-positive bacteria thallus is taken as a raw material, dried for 0.5-24h at 30-120 ℃, pre-carbonized for 0-8h at 500 ℃ under the protection of inert gas atmosphere, alkali-activated by taking 0.1-10 times of potassium hydroxide, sodium hydroxide, calcium hydroxide and the like as activating agents by mass at 900 ℃ under 600-12 mol/L, washed to be neutral by 0.1-12mol/L hydrochloric acid, and dried for 0.5-24h at 30-120 ℃ to obtain the gram-positive bacteria microporous carbon with high specific surface area.
The carbon material prepared by the invention has a layered structure which is closely arranged and is similar to a gram bacteria cell wall structure. The capacitance performance test proves that the gram bacteria source carbon material has good capacitance performance and circulation stability, and meanwhile, the material is simple and nontoxic in preparation process, low in cost and easy to apply in a large range.
Drawings
FIG. 1 is an SEM image of a bifidobacterium biomass charcoal material prepared by an alkali activation method in example 1;
FIG. 2 shows the nitrogen adsorption and desorption isotherms and pore size distribution of the Bifidobacterium biomass charcoal material prepared by the alkali activation method in example 1;
FIG. 3 is the constant current charging and discharging curve of the Bifidobacterium biomass charcoal material prepared by the alkali activation method in 6mol/L KOH solution of example 2 under the current density of 1A/g.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Specific example 1: taking commercial fermented yogurt strain bifidobacterium as an example, but not limited to the raw material, drying the raw material at 30-120 ℃ for 0.5-24h, pre-carbonizing the raw material at 500 ℃ for 0-8h under the protection of inert gas atmosphere, then performing alkali activation by using 0.1-10 times of mass of potassium hydroxide, sodium hydroxide, calcium hydroxide and the like as activating agents at 900 ℃ under 600-10 ℃, washing the product to be neutral by 0.1-12mol/L hydrochloric acid, and drying the product at 30-120 ℃ for 0.5-24h to obtain the gram-positive microporous carbon material with high specific surface area, wherein the structural characteristics of the gram-positive microporous carbon material are illustrated in the attached drawing.
Fig. 1 is an SEM image of a bifidobacterium biomass charcoal material prepared by an alkali activation method, and it can be seen that a tile shape with a certain radian is present, which proves that the alkali activation method retains the original cell wall morphology of bifidobacterium to a certain extent.
FIG. 2 shows the nitrogen adsorption and desorption isotherm and pore size distribution of the bifidobacterium biomass charcoal material prepared by the alkali activation method, and the specific surface area of the prepared charcoal material can reach 2877m2In terms of a/g, the pore diameter is predominantly microporous and the average pore diameter is 0.55 nm. The prepared material is proved to have rich pore channel structures.
Specific example 2: verification of the application of the preparation methodThe supercapacitor properties of the resulting material. The biomass carbon electrode material prepared by an alkali activation method, acetylene black and Polytetrafluoroethylene (PTFE) are prepared into a size of 1 multiplied by 1cm2The thin sheet is pressed on the foamed nickel to be used as a working electrode, mercury oxide is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, and a constant current charge-discharge curve in a range of-1.0 to 0V is tested in 6mol/L KOH solution, so that the result is shown in figure 3, the mass specific capacitance of the electrode material is 199F/g under the current density of 1A/g, and the electrode material has better application potential of super capacitance.
Claims (7)
1. The preparation method of the microporous gram bacteria carbon material with high specific surface area is characterized by comprising the following steps: the gram-positive bacteria thallus is prepared by pretreatment, high-temperature alkali activation carbonization treatment, neutralization, washing and drying.
2. The method for preparing the microporous gram-bacteria carbon material with high specific surface area according to claim 1, wherein the gram-positive bacteria thallus is prepared from a material containing a certain amount of gram-positive bacteria, and can be single pure thallus, mixed thallus or thallus containing other additives.
3. The preparation method of microporous gram-bacteria carbon material with high specific surface area according to claim 1, wherein the pretreatment method comprises the following steps: one or more of methods such as normal temperature drying, freeze drying, hydrothermal pre-carbonization, high temperature pre-carbonization and the like.
4. The preparation and alkali activation carbonization method for microporous gram bacteria carbon material with high specific surface area according to claim 1 is characterized in that: with 0.1-10 times the mass of a base such as: potassium hydroxide, sodium hydroxide, calcium hydroxide and the like are used as activating agents to carry out alkali activation, and the alkali activation is carried out in air or inert atmosphere at the high temperature of 500-1000 ℃ for carbonization to prepare the catalyst.
5. A microporous gram bacteria carbon material with high specific surface area is characterized in that: the material is prepared by the method of claims 1-4.
6. A microporous gram positive bacterial charcoal material of high specific surface area according to claim 5 wherein: the material is similar to a gram-positive bacteria cell wall structure in form, and the pore structure is microporous; the specific surface area of the gram-positive bacteria carbon is 700-2877 m2Per g, and the average pore diameter is 0.53-0.55 nm.
7. The microporous gram-positive bacterial carbon material with high specific surface area as claimed in claim 6, which has capacitance characteristics and can be used as an electrode material of a supercapacitor.
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Application publication date: 20211029 |