CN114420464A - Novel method for expanding carbon nanofiber electrode material by using biological enzyme - Google Patents
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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
- H01G11/40—Fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
Abstract
The invention discloses a new method for reaming a carbon nanofiber electrode material by using biological enzyme, which comprises the following steps: a) adding porous carbon of polyacrylonitrile and corn straw into N, N-Dimethylformamide (DMF), stirring for 2h, adding beta-cyclodextrin, continuously stirring for 6h, and ultrasonically dispersing for 30min to obtain a spinning solution precursor; b) performing high-voltage electrostatic spinning on the mixed solution to obtain beta-cyclodextrin doped nano fibers; c) putting the nano-fibers into a conical flask, adding an alpha-amylase solution, then putting into a constant-temperature water bath, and carrying out enzymolysis after heat preservation for 1-3 hours; d) and (3) freeze-drying the nano-fiber after enzymolysis, and then sequentially carrying out pre-oxidation and nitrogen protection carbonization to obtain the porous carbon nano-fiber. The method uses the biomass of beta-cyclodextrin as a pore-enlarging agent, dopes the biomass into the nano-fibers by an electrostatic spinning method, manufactures pores on the nano-fibers by an enzymatic hydrolysis method, and prepares the activated carbon nano-fibers after pre-oxidation and carbonization, and has strong controllability, no pollution and high pore-enlarging efficiency.
Description
Technical Field
The invention relates to the technical field of energy storage electrode material activation methods, in particular to a novel method for expanding a carbon nanofiber electrode material by using biological enzyme.
Background
With global energy depletion and increasingly prominent environmental pollution, a clean, efficient and sustainable energy source and new technologies related to energy conversion and storage must be found. The super capacitor is an energy storage device which can be charged or discharged safely in a very short time, and has a long cycle life. Such devices that can flexibly store energy have become candidates for wide applications due to their high power density and simple structure, including hybrid electric vehicles, mobile electronic devices, distributed sensor networks, and the like.
The super capacitor mainly comprises a positive electrode, a negative electrode, a diaphragm and an electrolyte. The electrode material is one of the key components of the super capacitor, and therefore, the development of the high-efficiency electrode material is crucial to the construction of the high-performance super capacitor. The carbon nanofiber not only has the advantages of good conductivity, thermal stability, low density, high mechanical strength, chemical corrosion resistance and the like of the carbon fiber material, but also has the advantages of large length-diameter ratio, compact structure and large specific surface area of the nanofiber material. The carbon nanofiber prepared by the electrostatic spinning method has the characteristics of simple process, controllable structure, adjustable components and the like, and draws wide attention of researchers.
At present, the activation methods of carbon nanofibers mainly include a chemical activation method and a physical activation method. The chemical activation is usually performed by KOH, NaOH or ZnCl2Etc. as activatorsPore-enlarging, strong alkali has high corrosivity, and the preparation process is easy to corrode instrument and equipment, and the prepared carbon material needs to be repeatedly cleaned. And zinc chloride is also a toxic substance, and has hidden danger to people and environment. The physical activation method mainly uses water vapor and CO2The gases are used as an activating agent, and a large amount of gases causing greenhouse effect are generated in the activating process. Therefore, the development of the carbon nanofiber pore-expanding method which is strong in controllability, green and pollution-free and high in pore-expanding efficiency is very important for protecting the environment.
CN 113314349A Chinese invention patent discloses a polyacrylonitrile/wood-based derived carbon porous material and preparation and application thereof. Belongs to the technical field of wood energy storage. According to the method, the polyacrylonitrile polymer material is filled in the carbonized wood pore channel, and then the polyacrylonitrile is carbonized at high temperature in the CO2 atmosphere, and meanwhile, the physical activation of the carbonized wood is completed, so that the specific surface area of the carbonized wood is effectively increased while the pore channel structure of the carbonized wood is efficiently utilized, the polyacrylonitrile/wood-based derived carbon porous material is prepared, and the excellent performance of the supercapacitor is shown.
The problems of the method are as follows: the method is used for preparing a wood-based derived carbon porous material, and firstly, the wood-based derived carbon porous material structurally belongs to a massive porous material and is not a carbon nanofiber electrode material; secondly, the activation method adopted is in CO2Activation method for producing CO in large amount2 。
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel method for reaming a carbon nanofiber electrode material by using biological enzyme, which is characterized in that biomass such as beta-cyclodextrin is used as a pore-enlarging agent, the biomass is doped into nanofibers by an electrostatic spinning method, pores are produced on the nanofibers by an enzyme hydrolysis method, and the active carbon nanofibers are prepared by pre-oxidation and carbonization, so that the controllability is strong, the environment is green, no pollution is caused, and the pore-enlarging efficiency is high.
In order to solve the technical problems, the invention adopts the following technical means:
a novel method for expanding a carbon nanofiber electrode material by using biological enzyme comprises the following steps:
a) mixing the following materials in percentage by mass (32-39): adding the porous carbon of polyacrylonitrile and corn straw into N, N-Dimethylformamide (DMF) and stirring for 2h, adding beta-cyclodextrin into a DMF solution, wherein the beta-cyclodextrin accounts for 10-50% of the total mass of the porous carbon of polyacrylonitrile and corn straw, and the total mass of the porous carbon of polyacrylonitrile and corn straw and the beta-cyclodextrin accounts for 20-30% of the mass of the N, N-dimethylformamide; continuously stirring for 6h, and performing ultrasonic dispersion for 30min to obtain a spinning solution precursor;
b) placing the mixed solution into an electrostatic spinning instrument injector, and performing high-voltage electrostatic spinning to obtain beta-cyclodextrin doped nanofibers;
c) putting the prepared nano-fiber into a conical flask, adding an alpha-amylase solution, then putting into a constant-temperature water bath kettle, and preserving heat for 1-3 hours for enzymolysis;
d) and taking out the nano-fiber after enzymolysis, freeze-drying, putting into a porcelain boat, and sequentially pre-oxidizing and carbonizing under the protection of nitrogen to obtain the porous carbon nano-fiber.
The invention uses the electrostatic spinning method to prepare the nano-fiber, and has the characteristics of controllable structure, adjustable components and the like; in the process of generating the nano-fiber by the electrostatic spinning technology, the beta-cyclodextrin is pre-doped into the nano-fiber, and then the nano-fiber is hydrolyzed by alpha-amylase to generate a pore structure on the nano-fiber, so that the electrochemical performance of the carbonized material is improved, and the process avoids the emission of a large amount of CO2 gas caused by activation.
The further preferred technical scheme is as follows:
the mass ratio of the polyacrylonitrile to the corn straw porous carbon is 9: 1.
the parameters of the high-voltage electrostatic spinning are as follows: the positive pressure is 15KV, the negative pressure is 3KV, the spinning space is 20cm, and the solution spraying speed is 0.015 ml/min.
The enzyme activity of the alpha-amylase solution is 10-60U/ml, and the mass of the solution is 50-200 times of that of the added nano-fiber.
The pre-oxidation parameters are as follows: the heating rate is 1 ℃/min, the temperature is kept at 280 ℃ for 2h, and the cooling rate is 2 ℃/min.
The nitrogen protection carbonization is characterized in that under the nitrogen protection condition, the carbonization is carried out, the temperature rising rate is 2 ℃/min to the carbonization temperature, the carbonization temperature is 700 ℃, 800 ℃ and 900 ℃, the temperature is kept for 2h, and the temperature reduction rate is 5 ℃/min.
The application of the flexible porous carbon nanofiber prepared by the invention in a super capacitor is evaluated by electrochemical tests, and the specific steps are as follows:
mixing porous carbon nanofiber, acetylene black, conductive graphite and polytetrafluoroethylene dispersion liquid (60 mass percent) according to a mass ratio of 8: 0.75: 0.75: 0.5 of the powder is added into a mortar and fully mixed to be pasty, and the pasty powder is evenly smeared on foamed nickel with the thickness of 2cm multiplied by 1cm, the smearing area is 1cm multiplied by 1cm, the foamed nickel is put into a vacuum drying oven to be dried for 8 hours, and then the foamed nickel is pressed into an electrode slice under the pressure of 6 MPa. A CHI660E electrochemical workstation is utilized, a platinum sheet electrode is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, porous carbon nanofiber is used as a working electrode, and 6 mol/L KOH aqueous solution is used as electrolyte to form a three-electrode system. And testing the electrochemical performance of the material electrode in a voltage range of-1.0-0V.
The biomass of beta-cyclodextrin is used as a pore-enlarging agent, is uniformly dispersed in a spinning solution precursor, and is doped into the nanofiber by an electrostatic spinning method. The alpha-amylase can hydrolyze 1, 4-glycosidic bond of the beta-cyclodextrin, hydrolyze the beta-cyclodextrin exposed on the surface of the nanofiber into oligosaccharide or monosaccharide, and the oligosaccharide or monosaccharide falls off from the original position on the nanofiber to form a pore structure. Meanwhile, cheap and reproducible porous carbon of the corn straws is used for replacing part of a carbon source of high polymer PAN, original N, P, S and other trace elements of the biomass straws are doped in situ, the wettability of the material to electrolyte is increased, the electrochemical performance of the material is increased while the environment is protected, and the porous carbon nanofibers are obtained through preoxidation and carbonization.
Drawings
Fig. 1 is an electron microscope image of the nanoporous carbon fiber obtained in example 2.
FIG. 2 is a nitrogen adsorption/desorption diagram and a pore size analysis curve of the nanoporous carbon fiber obtained in example 2.
FIG. 3 is a constant current charge and discharge curve for different current densities for example 2.
Detailed Description
To better illustrate the technical means and effects of the present invention adopted to achieve the intended purpose, the following description is made with reference to the specific embodiments and the accompanying drawings.
The porous carbon of corn stalk that this embodiment part used is the laboratory self-control, smashes corn stalk, washs, dries the back, and the mass ratio of adding activator KOH and straw is 1: 1, carbonizing at 800 ℃ for 2h in a tube furnace under the protection of nitrogen, cleaning to be neutral and drying to obtain the product.
This example illustrates the following three examples, depending in part on the amount of biomass activator β -cyclodextrin added:
example 1
And (3) mixing the components in a mass ratio of 9: adding the porous carbon of polyacrylonitrile and corn straw 1 into N, N-Dimethylformamide (DMF), and stirring for 2 h. Adding beta-cyclodextrin into the DMF solution, wherein the beta-cyclodextrin accounts for 10% of the total mass of the polyacrylonitrile and the corn straw porous carbon, the total mass of the polyacrylonitrile, the corn straw porous carbon and the beta-cyclodextrin accounts for 25% of the mass of the N, N-dimethylformamide, continuously stirring for 6h, and then carrying out ultrasonic dispersion for 30min to obtain a spinning solution precursor. Obtaining the nano-fiber by high-voltage electrostatic spinning, wherein the electrostatic spinning parameters are as follows: the positive pressure is 15KV, the negative pressure is 3KV, the spinning space is 20cm, and the solution spraying speed is 0.015 ml/min.
Weighing 1g of nano-fiber, putting the nano-fiber into an erlenmeyer flask, adding 150ml of 50U/ml of medium-temperature liquid alpha-amylase solution, then putting the erlenmeyer flask into a constant-temperature water bath kettle at 75 ℃, and preserving heat for 1.5 hours. Taking out the nano-fiber after enzymolysis, freeze-drying, and placing into a muffle furnace for pre-oxidation, wherein the parameters are as follows: the heating rate is 1 ℃/min, the temperature is kept at 280 ℃ for 2h, and the cooling rate is 2 ℃/min. Then carbonizing under the protection of nitrogen, wherein the parameters are as follows: heating to 800 ℃ at the temperature rise rate of 2 ℃/min, preserving heat for 2h, cooling to 5 ℃/min, and cooling to room temperature to obtain the porous carbon nanofiber.
Example 2
And (3) mixing the components in a mass ratio of 9: adding the porous carbon of polyacrylonitrile and corn straw 1 into N, N-Dimethylformamide (DMF), and stirring for 2 h. Adding beta-cyclodextrin into the DMF solution, wherein the beta-cyclodextrin accounts for 20% of the total mass of the polyacrylonitrile and the corn straw porous carbon, the total mass of the polyacrylonitrile, the corn straw porous carbon and the beta-cyclodextrin accounts for 25% of the mass of the N, N-dimethylformamide, continuously stirring for 6h, and then carrying out ultrasonic dispersion for 30min to obtain a spinning solution precursor. Obtaining the nano-fiber by high-voltage electrostatic spinning, wherein the electrostatic spinning parameters are as follows: the positive pressure is 15KV, the negative pressure is 3KV, the spinning space is 20cm, and the solution spraying speed is 0.015 ml/min.
Weighing 1g of nano-fiber, putting the nano-fiber into an erlenmeyer flask, adding 150ml of 50U/ml of medium-temperature liquid alpha-amylase solution, then putting the erlenmeyer flask into a constant-temperature water bath kettle at 75 ℃, and preserving heat for 1.5 hours. Taking out the nano-fiber after enzymolysis, freeze-drying, and placing into a muffle furnace for pre-oxidation, wherein the parameters are as follows: the heating rate is 1 ℃/min, the temperature is kept at 280 ℃ for 2h, and the cooling rate is 2 ℃/min. Then carbonizing under the protection of nitrogen, wherein the parameters are as follows: heating to 800 ℃ at the temperature rise rate of 2 ℃/min, preserving heat for 2h, cooling to 5 ℃/min, and cooling to room temperature to obtain the porous carbon nanofiber.
Example 3
And (3) mixing the components in a mass ratio of 9: adding the porous carbon of polyacrylonitrile and corn straw 1 into N, N-Dimethylformamide (DMF), and stirring for 2 h. Adding beta-cyclodextrin into the DMF solution, wherein the beta-cyclodextrin accounts for 30% of the total mass of the polyacrylonitrile and the corn straw porous carbon, the total mass of the polyacrylonitrile, the corn straw porous carbon and the beta-cyclodextrin accounts for 25% of the mass of the N, N-dimethylformamide, continuously stirring for 6h, and then carrying out ultrasonic dispersion for 30min to obtain a spinning solution precursor. Obtaining the nano-fiber by high-voltage electrostatic spinning, wherein the electrostatic spinning parameters are as follows: the positive pressure is 15KV, the negative pressure is 3KV, the spinning space is 20cm, and the solution spraying speed is 0.015 ml/min.
Weighing 1g of nano-fiber, putting the nano-fiber into an erlenmeyer flask, adding 150ml of 50U/ml of medium-temperature liquid alpha-amylase solution, then putting the erlenmeyer flask into a constant-temperature water bath kettle at 75 ℃, and preserving heat for 1.5 hours. Taking out the nano-fiber after enzymolysis, freeze-drying, and placing into a muffle furnace for pre-oxidation, wherein the parameters are as follows: the heating rate is 1 ℃/min, the temperature is kept at 280 ℃ for 2h, and the cooling rate is 2 ℃/min. Then carbonizing under the protection of nitrogen, wherein the parameters are as follows: heating to 800 ℃ at the temperature rise rate of 2 ℃/min, preserving heat for 2h, cooling to 5 ℃/min, and cooling to room temperature to obtain the porous carbon nanofiber.
As can be seen from fig. 1, 2 and 3, the porous carbon nanofiber obtained in the present embodiment avoids a large amount of CO2 discharged to the outside during the activation process, and the carbonized carbon nanofiber material has excellent electrochemical properties.
FIG. 1 is an electron micrograph of example 2 after carbonization, but with a significant carbon nanofiber structure remaining.
Fig. 2 is a drawing of nitrogen absorption/desorption and pore size analysis curve analysis after carbonization in example 2, and it can be seen from the drawing that the carbon nanofiber prepared by the method has a hierarchical pore structure of macropores, mesopores and micropores, so that the diffusion distance of electrolyte ions from the mesopores to the micropores is very short, and the pore structure can provide a fast channel for electron transfer in an electrolyte.
FIG. 3 is a constant current charge and discharge curve of the carbonized material of example 2 at different current densities, the curve being close to the shape of an isosceles triangle even at current densities as high as 10A/g, showing a near ideal capacitance performance. The specific capacitance of the material was 187.1F/g at a current density of 0.5A/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, which is defined in the appended claims.
Claims (6)
1. A novel method for expanding a carbon nanofiber electrode material by using biological enzyme is characterized by comprising the following steps:
a) mixing the following materials in percentage by mass (32-39): adding the porous carbon of polyacrylonitrile and corn straw into N, N-Dimethylformamide (DMF) and stirring for 2h, adding beta-cyclodextrin into a DMF solution, wherein the beta-cyclodextrin accounts for 10-50% of the total mass of the porous carbon of polyacrylonitrile and corn straw, and the total mass of the porous carbon of polyacrylonitrile and corn straw and the beta-cyclodextrin accounts for 20-30% of the mass of the N, N-dimethylformamide; continuously stirring for 6h, and performing ultrasonic dispersion for 30min to obtain a spinning solution precursor;
b) placing the mixed solution into an electrostatic spinning instrument injector, and performing high-voltage electrostatic spinning to obtain beta-cyclodextrin doped nanofibers;
c) putting the prepared nano-fiber into a conical flask, adding an alpha-amylase solution, then putting into a constant-temperature water bath kettle, and preserving heat for 1-3 hours for enzymolysis;
d) and taking out the nano-fiber after enzymolysis, freeze-drying, putting into a porcelain boat, and sequentially pre-oxidizing and carbonizing under the protection of nitrogen to obtain the porous carbon nano-fiber.
2. The method for reaming the carbon nanofiber electrode material by using the biological enzyme as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the polyacrylonitrile to the corn straw porous carbon is 9: 1.
3. the method for reaming the carbon nanofiber electrode material by using the biological enzyme as claimed in claim 1, wherein the method comprises the following steps: the parameters of the high-voltage electrostatic spinning are as follows: the positive pressure is 15KV, the negative pressure is 3KV, the spinning space is 20cm, and the solution spraying speed is 0.015 ml/min.
4. The method for reaming the carbon nanofiber electrode material by using the biological enzyme as claimed in claim 1, wherein the method comprises the following steps: the enzymolysis is to decompose beta-cyclodextrin in the nanofiber by using alpha-amylase to form a pore channel structure, the enzyme activity of an alpha-amylase solution is 10-60U/ml, and the mass of the solution is 50-200 times that of the added nanofiber.
5. The method for reaming the carbon nanofiber electrode material by using the biological enzyme as claimed in claim 1, wherein the method comprises the following steps: the pre-oxidation parameters are as follows: the heating rate is 1 ℃/min, the temperature is kept at 280 ℃ for 2h, and the cooling rate is 2 ℃/min.
6. The method for reaming the carbon nanofiber electrode material by using the biological enzyme as claimed in claim 1, wherein the method comprises the following steps: the nitrogen protection carbonization is characterized in that under the nitrogen protection condition, the carbonization is carried out, the temperature rising rate is 2 ℃/min to the carbonization temperature, the carbonization temperature is 700 ℃, 800 ℃ and 900 ℃, the temperature is kept for 2h, and the temperature reduction rate is 5 ℃/min.
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| CN115537974A (en) * | 2022-10-27 | 2022-12-30 | 浙江科技学院 | Method for preparing carbon nanofiber with surface micropore morphology from alkali lignin and polyacrylonitrile |
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