CN112357904B - Biomass carbon microsphere, preparation method, supercapacitor and application - Google Patents
Biomass carbon microsphere, preparation method, supercapacitor and application Download PDFInfo
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- CN112357904B CN112357904B CN202011254134.8A CN202011254134A CN112357904B CN 112357904 B CN112357904 B CN 112357904B CN 202011254134 A CN202011254134 A CN 202011254134A CN 112357904 B CN112357904 B CN 112357904B
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- 239000004005 microsphere Substances 0.000 title claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 239000002028 Biomass Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 14
- 239000011593 sulfur Substances 0.000 claims abstract description 14
- 235000019990 fruit wine Nutrition 0.000 claims abstract description 12
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 8
- 229930006000 Sucrose Natural products 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000005720 sucrose Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010276 construction Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 2
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 abstract description 12
- 239000003575 carbonaceous material Substances 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000033228 biological regulation Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000006230 acetylene black Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000009656 pre-carbonization Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- -1 sulfur glutaraldehyde Chemical compound 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 210000005253 yeast cell Anatomy 0.000 description 1
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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
- 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
-
- 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
- H01G11/42—Powders or particles, e.g. composition thereof
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention belongs to the technical field of carbon materials, and discloses biomass carbon microspheres, a preparation method, a supercapacitor and application thereof, wherein the preparation method of the biomass carbon microspheres comprises the following steps: fermenting in a sulfur-containing sucrose solution of fruit wine yeast; adding a certain amount of glutaraldehyde and sulfur into the system, and carrying out ultrasonic treatment; transferring the solution into a hydrothermal kettle, reacting to obtain a brown product, and performing suction filtration, washing and drying; and (3) placing the product in a tube furnace in a nitrogen atmosphere, cooling, washing and drying to obtain the final carbon microsphere with the internal fine structure. The method has the advantages of simplicity, convenience, easy operation, environmental friendliness, wide applicability and the like. The invention is suitable for biomass carbon microspheres, has more excellent application performance, is simple and convenient, is easy to operate and is easy for mass production. The carbon microsphere prepared by the method has ultrahigh capacitance performance; the method is simple and convenient to operate, environment-friendly and easy to prepare in batches; the method is suitable for different kinds of yeast.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a biomass carbon microsphere, a preparation method, a supercapacitor and an application.
Background
At present: carbon materials have been widely used in many fields due to their excellent mechanical strength, chemical inertness, and excellent electrical and thermal conductivity. The porous carbon microspheres have the unique characteristics of regular geometric shape, controllable size, fine structure, obvious high bulk density, high specific surface area and the like, so that the carbon material has new structural characteristics and the application field of the carbon material is expanded. With the continuous improvement of the demand of high-end products, the construction and the regulation of the internal fine structure of the microsphere are important. Despite the efforts of researchers to do so, the preparation of carbon microspheres with fine structures inside remains a difficult point in the field. The solution polymerization method is a commonly used method for preparing the carbon microspheres with fine structures at present, and Lu and the like prepare multi-cavity nano microspheres by using a surface energy induction method; yang et al prepared mesoporous carbon microspheres of different sizes by self-assembly of emulsion; qiao et al prepared multi-chambered micron-sized carbon microspheres using constrained-domain polymerization. The above experiments can be summarized as follows: the difficulty in preparing carbon microspheres with internal fine structures is due to the difficulty in achieving simultaneous manipulation of the micron-sized shell and the nano-sized interior with conventional methods. It is noted that there is a large class of microsphere precursors in the biological world, including seeds, pollen and cells. However, no literature reports a method for regulating the internal structure of the material. Undeniably, biomass precursors, in addition to their wide sources and low cost, have micron-sized and robust cell wall shells, which bring natural advantages for the regulation of internal structures and subsequent separations. Especially, yeast cells have the characteristics of variety diversity, high propagation speed and environmental friendliness, and are widely concerned. The biomass is used as a carbon microsphere precursor, related reports of hollow carbon microspheres and porous carbon microspheres exist, but related methods and structures for fine regulation and control of internal structures do not exist.
Through the above analysis, the problems and defects of the prior art are as follows: the existing microsphere synthesis method cannot be applied to the precise construction and regulation of the internal structure of the biomass carbon microsphere, and the regulation of the internal structure of the biomass carbon microsphere is a blank technical field.
The difficulty in solving the above problems and defects is: even if the polymer microsphere is used as a precursor to regulate the internal structure of the microsphere, the regulation of the internal structure of the microsphere is very difficult, so that the precise regulation of the internal structure of the material such as biomass is very challenging work, and the conventional method is to prepare hollow or disordered porous carbon microspheres.
The significance of solving the problems and the defects is as follows: the method for preparing the carbon microspheres with the fine internal structure by using the biomass material as the precursor is expanded, and the method has applicability to different types of yeasts.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a biomass carbon microsphere, a preparation method, a supercapacitor and application.
The invention is realized in such a way that the preparation method of the biomass carbon microsphere comprises the following steps:
fermenting in a sulfur-containing sucrose solution of fruit wine yeast;
adding a certain amount of glutaraldehyde and sulfur into the system, and carrying out ultrasonic treatment;
transferring the solution into a hydrothermal kettle, reacting to obtain a brown product, and performing suction filtration, washing and drying;
and (3) placing the product in a tube furnace under the nitrogen atmosphere, cooling, washing and drying to obtain the final carbon microsphere with the internal fine structure.
Further, 5g of fruit wine yeast is fermented for 10-24h in a system with a sucrose solution with the mass fraction of 5% and the sulfur content of 20 ppm.
Further, glutaraldehyde and sulfur were added to the above system and sonicated for 1-2 h.
And further transferring the solution into a hydrothermal kettle, reacting at 200 ℃ for 5-24h to obtain a brown product, and performing suction filtration, washing and drying.
Further, the product was placed in a tube furnace under nitrogen atmosphere at a temperature rise rate of 1-10 DEG/min to 750 DEG and 950 ℃.
The sucrose of the invention is bred by yeast, and the high activity is easy to modify in order to generate fresh yeast; the sulfur content of 20ppm in the sucrose is used for delaying the fermentation time of yeast, ensuring the purity of the strain and being beneficial to killing mixed bacteria; glutaraldehyde is used as a cross-linking agent, which is beneficial to fully cross-linking the protein micro-beam structure in the yeast, so that a key effect is provided for the construction of a fine structure, and the sulfur glutaraldehyde added in the later stage enters cells and has capillary force, which is beneficial to the glutaraldehyde to smoothly enter the cells. Similarly, ultrasound also serves to provide external forces to push glutaraldehyde and sulfur into the interior of the cell. A large amount of glutaraldehyde and sulfur internally form a finely structured carbon skeleton. The hydrothermal reaction is used for providing the function of pre-carbonization, which is beneficial to keeping the stability of the yeast microsphere structure in the carbonization stage without being damaged
Another object of the present invention is to provide an electrode material prepared from a carbon material and a binder and acetylene black-forming slurry; the carbon material comprises the following components in percentage by mass: adhesive: acetylene black is 8:1: 1.
Another object of the present invention is to provide a supercapacitor assembled from said electrode material.
Another object of the present invention is to provide a solar energy system equipped with the supercapacitor.
Another object of the present invention is to provide a wind power generation system mounted with the supercapacitor.
The invention further aims to provide a new energy automobile provided with the super capacitor.
By combining all the technical schemes, the invention has the advantages and positive effects that: the invention provides a strategy for constructing a fungal house by using an architectural method to realize the construction and regulation of the fine structure in the biomass carbon precursor microsphere. The invention takes fruit wine yeast as a research case, and researches a regulation and control method and a related mechanism for changing a structure from a hollow structure to a mesoporous structure. The experimental development proves that the method is also suitable for the beer yeast and the flour yeast. The method has the advantages of simplicity, convenience, easy operation, environmental friendliness, wide applicability and the like. The invention is suitable for biomass carbon microspheres, has more excellent application performance, is simple and convenient, is easy to operate and is easy for mass production. The carbon microsphere prepared by the method shows ultrahigh capacitance performance; the method is simple and convenient to operate, environment-friendly and easy to prepare in batches; the method is suitable for different kinds of yeast.
The invention is shown by a transmission electron microscope, a scanning electron microscope and a pore size distribution diagram, and is a carbon microsphere with a micron structure, and the internal structure can realize the controllable construction of a solid structure, a mesoporous structure, a macroporous structure and a hollow structure; the specific capacitance can reach 339F g without any activation treatment when the catalyst is used for electrochemical performance -1 (ii) a Glutaraldehyde and S simple substances added in the experimental operation process do not exist in the form of byproducts, but form an internal carbon skeleton in the combination of the yeast microspheres and the protein micro-beam, and the size and the number of internal cavities are determined by the quantity of the internal carbon skeleton to form a 'fungus house', so the method is environment-friendly; mainly utilizes ultrasonic and hydrothermal environments to realize gram-grade production each time, so the operation is simple and convenient and the batch production is easy; the method is carried outThe results show that the yeast has the same applicability when being used for other yeast species.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a flow chart of a preparation method of biomass carbon microspheres according to an embodiment of the invention.
Fig. 2 is a flow chart of a preparation method of biomass carbon microspheres according to an embodiment of the present invention.
FIG. 3 is a transmission electron microscope image and a scanning electron microscope image of the fruit wine yeast with internal fine structure prepared by the embodiment of the invention.
FIG. 4 is a pore size distribution diagram of the prepared fruit wine yeast with internal fine structure provided by the embodiment of the invention.
FIG. 5(a) is a cyclic voltammogram at different sweep rates provided by an embodiment of the present invention.
Fig. 5(b) is a constant current charge-discharge diagram under different current densities according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a biomass carbon microsphere, a preparation method, a super capacitor and application thereof, and the invention is described in detail with reference to the accompanying drawings.
As shown in fig. 1, the preparation method of biomass carbon microspheres provided by the invention comprises the following steps:
s101: fermenting 5g of fruit wine yeast in a sucrose solution with the mass fraction of 5% for 10-24h in a system with the sulfur content of 20 ppm;
s102: adding a certain amount of glutaraldehyde and sulfur into the system, and carrying out ultrasonic treatment for 1-2 h;
s103: transferring the solution into a hydrothermal kettle, reacting for 5-24h at 200 ℃ to obtain a brown product, and performing suction filtration, washing and drying;
s104: and placing the product in a tubular furnace in a nitrogen atmosphere at a heating rate of 1-10 ℃/min to 750-.
In the present invention, the fruit wine yeast was purchased from Nicotiana tabasheeri, Inc.
In the present invention, the mass concentration is 1.0 to 4.0 wt.%.
The preparation method of biomass carbon microspheres provided by the invention can be implemented by adopting other steps by persons of ordinary skill in the art, and the preparation method of biomass carbon microspheres provided by the invention in fig. 1 is only one specific example.
According to the invention, carbon materials, a binder and acetylene black are homogenized to prepare an electrode material for assembling a super capacitor; testing the performance of the characterization electrode material; (ii) a The carbon material comprises the following components in percentage by mass: adhesive: acetylene black is 8:1: 1.
As shown in fig. 3, a transmission electron microscope image and a scanning electron microscope image of the prepared fruit wine yeast with an internal fine structure provided by the embodiment of the invention are shown.
As shown in FIG. 4, the pore size distribution diagram of the prepared fruit wine yeast with internal fine structure provided by the embodiment of the invention is shown.
As shown in FIG. 5(a), embodiments of the present invention provide cyclic voltammograms at different sweep rates.
As shown in fig. 5(b), the constant current charging and discharging diagram provided by the embodiment of the invention under different current densities.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. The preparation method of the biomass carbon microsphere is characterized by comprising the following steps:
fermenting in a sulfur-containing sucrose solution of fruit wine yeast;
adding a certain amount of glutaraldehyde and sulfur into the system, and carrying out ultrasonic treatment for 1-2 h;
transferring the solution into a hydrothermal kettle, reacting to obtain a brown product, and performing suction filtration, washing and drying;
placing the product in a tubular furnace in a nitrogen atmosphere, cooling, washing and drying to obtain the carbon microspheres with the micron structures, wherein the internal structure can realize the controllable construction of solid, mesoporous, macroporous and hollow structures;
fermenting 5g of fruit wine yeast in a sucrose solution with the mass fraction of 5% and a system with the sulfur content of 20ppm for 10-24 h; the mass concentration is 1.0-4.0 wt.%.
2. The preparation method of the biomass carbon microspheres as claimed in claim 1, wherein the solution is transferred to a hydrothermal kettle, and reacted at 200 ℃ for 5-24h to obtain a brown product, and the brown product is filtered, washed and dried.
3. The method for preparing biomass carbon microspheres as claimed in claim 1, wherein the product is placed in a tubular furnace under nitrogen atmosphere at a temperature rise rate of 1-10 °/min to 750-.
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