CN112670101A - Preparation method and application of conventional viscose fiber supercapacitor electrode material - Google Patents
Preparation method and application of conventional viscose fiber supercapacitor electrode material Download PDFInfo
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- CN112670101A CN112670101A CN202110000921.8A CN202110000921A CN112670101A CN 112670101 A CN112670101 A CN 112670101A CN 202110000921 A CN202110000921 A CN 202110000921A CN 112670101 A CN112670101 A CN 112670101A
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Abstract
The invention relates to a preparation method and application of a conventional viscose fiber supercapacitor electrode material. The preparation method comprises the following steps: pre-carbonizing viscose fibers at 300-400 ℃ for 1h, and then naturally cooling to room temperature; mixing Co (NO)3)2·6H2Dissolving O in 25ml of deionized water, adding 0.275g of a pre-carbonized sample, stirring at room temperature for 24 hours, centrifuging and drying; soaking the dried sample in 5ml of KOH solution, and drying in an oven; and then activating for 1h at 700 ℃ in an argon atmosphere, washing the obtained activated product with a dilute acid solution, then washing the activated product with distilled water to be neutral, and drying to finally obtain the conventional viscose fiber supercapacitor electrode material. The preparation process is simple and has controllability; prepared conventional viscose fiber supercapacitor electrode materialThe material has the advantages of excellent electrochemical performance, good rate performance and the like, and is very suitable to be used as an electrode material in the field of super capacitors.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to a preparation method and application of a conventional viscose fiber supercapacitor electrode material.
Background
Viscose fiber, called viscose fiber for short, is a main variety of artificial fiber, and is made up by using natural fiber (wood fiber and cotton linter) as raw material, through the processes of alkalization, ageing and sulfonation, etc. to obtain soluble cellulose xanthate, then dissolving it in dilute alkali liquor to obtain viscose fibre, and making wet spinning so as to obtain the invented product. LI Xiangye et al, using polyvinylpyrrolidone (PVP) as a soft template, blended PVP and Polyacrylonitrile (PAN) and applied an electrospinning method to prepare a relatively good supercapacitor electrode material with a specific capacitance of 248.6F/g at 1A/g (LI Xiangye, Bai Tianjiaiao, Weng Xin, Zhang Bing, Wang Zhenzhen, He Tieshi, Application of electrospark polyacrylic copolymer-based carbon nanoparticles in supercapacitors, 2020, 1000-6613.2020-1330). Lai et al activated PAN-based carbon nanofibers using three different molecular weight Polymethylmethacrylate (PMMA) as a pore forming agent, respectively, and found that the PMMA-activated carbon nanofiber electrode material had a maximum specific capacitance of 210F/g (Lai C, Lo C T, Preparation of nano structural carbon nanofibers and the electrochemical performance for supercapacitors, 2015, 183). Zinc acetate and PAN are mixed and then dissolved in dimethylformamide together by Kim to form a mixed bi-component precursor solution, the prepared electrospun precursor is carbonized to obtain the carbon nanofiber composite electrode material with the ZnO/PAN porous structure, and the specific capacitance of the composite electrode material is 178.2F/g (Kim C H, Kim B H, Zinc oxide/activated carbon nanofiber composites for high-performance capacitor electrodes 2015, 274-.
Chinese patent document CN105671692A discloses a method for preparing a nitrogen-rich porous carbon fiber electrode material, which comprises the following steps: mixing melamine and formaldehyde, reacting under the condition that the pH value of a mixed system is 8.8-9.5, and adding formaldehyde after the reaction is finished to separate out melamine resin; dissolving polyacrylonitrile in N, N-Dimethylformamide (DMF), adding melamine resin, stirring and dissolving to obtain spinning solution; carrying out high-voltage electrostatic spinning on the spinning solution to obtain MF/PAN composite fiber; the MF/PAN composite fiber is subjected to pre-oxidation treatment and carbonization treatment to obtain the nitrogen-rich porous carbon fiber electrode material, and the specific capacitance is only 136A/g under the current density of 0.5A/g.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a conventional viscose fiber supercapacitor electrode material with high specific capacitance and good rate performance.
The technical scheme of the invention is as follows:
according to the invention, the preparation method of the conventional viscose fiber supercapacitor electrode material comprises the following steps:
(1) pre-carbonizing viscose fibers at 300-400 ℃ for 1h, and then naturally cooling to room temperature;
(2) 0.35M to 0.8M Co (NO)3)2·6H2Dissolving O in 25ml of deionized water, adding 0.275g of the sample pre-carbonized in the step (1), stirring at room temperature for 24 hours, centrifuging and drying;
(3) soaking the sample obtained in the step (2) in 5ml of KOH solution, wherein the mass ratio of the sample to KOH is 1: 0.5-1: 3, and drying in an oven; then activating for 1h at 700 ℃ in argon atmosphere, and naturally cooling to room temperature;
(4) washing the product obtained in the step (3) with a dilute acid solution, and then washing with distilled water to be neutral;
(5) the product obtained in the step (4) is treated at 40oC~80oAnd drying for 12-24 hours under the condition of C to obtain the conventional viscose fiber supercapacitor electrode material.
According to the present invention, it is preferable that the temperature increase rate in the step (1) is 5 ℃/min.
According to the present invention, it is preferable that Co (NO) in the step (2)3)2·6H2O is commercially available.
According to the present invention, it is preferable that Co (NO) in the step (2)3)2·6H2O is 0.65M each.
According to the present invention, it is preferred that the mass ratio of the sample to KOH in step (3) is 1: 1.
The application of the conventional viscose fiber supercapacitor electrode material is used for the electrode material of a supercapacitor.
The technical advantages of the invention are as follows:
(1) the invention has simple preparation process and controllability, and can control the ratio of the sample to KOH andCo2+to control performance.
(2) The conventional viscose fiber supercapacitor electrode material prepared by the invention has the advantages of stable structure, excellent electrochemical performance, good rate capability, high specific capacitance and the like, and is very suitable for being applied to the field of supercapacitors as an electrode material.
Drawings
FIG. 1 is a transmission electron microscope image of a conventional viscose fiber supercapacitor electrode material prepared in example 1 of the present invention.
FIG. 2 shows Co-free samples obtained by comparative examples of the present invention2+And (3) a transmission electron microscope image of the doped conventional viscose fiber supercapacitor electrode material.
FIG. 3 is a graph of specific capacitance versus current density for a conventional viscose fiber supercapacitor electrode material made in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
the viscose fibres were pre-carbonized at 300 ℃ for 1h, after which they were allowed to cool to room temperature. 0.05M Co (NO)3)2·6H2O was dissolved in 25ml of deionized water, and 0.275g of the pre-carbonized sample was added thereto, stirred at room temperature for 24 hours, and then centrifuged and dried.
Soaking the dried sample in 5ml of KOH solution (the mass ratio of the pre-carbonized product to the KOH is 1: 1), and drying in an oven; then activated for 1h at 700 ℃ in an argon atmosphere, and naturally cooled to room temperature.
Washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the conventional viscose fiber supercapacitor electrode material.
Adopts a three-electrode system, takes 2M sulfuric acid solution as electrolyte,the specific capacitance measured at 1A/g is 368F/g, and the rate capability is better. The transmission electron microscope image of the conventional viscose fiber supercapacitor electrode material prepared in the example is shown in fig. 1, and Co can be known from fig. 12+Doped into the material structure.
Example 2:
the viscose fibres were pre-carbonized at 300 ℃ for 1h, after which they were allowed to cool to room temperature. 0.05M Co (NO)3)2·6H2O was dissolved in 25ml of deionized water, and 0.275g of the pre-carbonized sample was added thereto, stirred at room temperature for 24 hours, and then centrifuged and dried.
Soaking the dried sample in 5ml of KOH solution (the mass ratio of the pre-carbonized product to the KOH is 1: 0.5), and drying in an oven; then activated for 1h at 700 ℃ in an argon atmosphere, and naturally cooled to room temperature.
Washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the conventional viscose fiber supercapacitor electrode material.
A three-electrode system is adopted, 2M sulfuric acid solution is used as electrolyte, the specific capacitance measured by 1A/g is 346F/g, and the rate performance is good.
Example 3:
the viscose fibres were pre-carbonized at 300 ℃ for 1h, after which they were allowed to cool to room temperature. Soaking the sample in 5ml of KOH solution (the mass ratio of the pre-carbonized product to the KOH is 1: 2), and drying in an oven; then activated for 1h at 700 ℃ in an argon atmosphere, and naturally cooled to room temperature. Washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the conventional viscose fiber supercapacitor electrode material.
A three-electrode system is adopted, 2M sulfuric acid solution is used as electrolyte, the specific capacitance measured by 1A/g is 325F/g, and the rate capability is good.
Example 4:
the viscose fibres were pre-carbonized at 300 ℃ for 1h, after which they were allowed to cool to room temperature. 0.05M Co (NO)3)2·6H2O was dissolved in 25ml of deionized water, to which 0.275% was addedg of the pre-carbonized sample, was stirred at room temperature for 24 hours, centrifuged and dried.
Soaking the dried sample in 5ml of KOH solution (the mass ratio of the pre-carbonized product to the KOH is 1: 3), and drying in an oven; then activated for 1h at 700 ℃ in an argon atmosphere, and naturally cooled to room temperature. Washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; the product obtained is at 40oAnd C, drying for 24 hours to obtain the conventional viscose fiber supercapacitor electrode material.
A three-electrode system is adopted, 2M sulfuric acid solution is used as electrolyte, the specific capacitance measured by 1A/g is 325F/g, and the multiplying power is good.
Comparative example:
the viscose fibres were pre-carbonized at 300 ℃ for 1h, after which they were allowed to cool to room temperature. Soaking the dried sample in 5ml of KOH solution (the mass ratio of the pre-carbonized product to the KOH is 1: 1), and drying in an oven; then activated for 1h at 700 ℃ in an argon atmosphere, and naturally cooled to room temperature. Washing the obtained product with a dilute hydrochloric acid solution, and then washing the product with distilled water to be neutral; and drying the obtained product at 40 ℃ for 24h to obtain the conventional viscose fiber supercapacitor electrode material.
A three-electrode system is adopted, 2M sulfuric acid solution is used as electrolyte, the specific capacitance measured by 1A/g is 306F/g, and the multiplying power performance is good. The transmission electron microscope image of the electrode material of the conventional viscose fiber supercapacitor prepared in the example is shown in fig. 1, and it can be known from fig. 2 that the polymer is in a lamellar structure.
Claims (5)
1. A preparation method of a conventional viscose fiber supercapacitor electrode material comprises the following steps:
(1) pre-carbonizing viscose fibers at 300-400 ℃ for 1h, and then naturally cooling to room temperature;
(2) mixing 0.035-0.08M Co (NO)3)2·6H2Dissolving O in 25ml of deionized water, adding 0.275g of a pre-carbonized sample, stirring at room temperature for 24 hours, centrifuging and drying;
(3) soaking the dried sample in 5ml of KOH solution, wherein the mass ratio of the sample to KOH is 1: 0.5-1: 3, and then drying in an oven;
(4) the carbon material obtained in the step (3) is put under the protection of argon gas at 700 DEGoC, activating for 1 hour, and naturally cooling to room temperature;
(5) washing the product obtained in the step (4) with a dilute acid solution, and then washing with distilled water to be neutral;
(6) the product obtained in step (5) is treated at 40oC~80oAnd drying for 12-24 hours under the condition of C to obtain the conventional viscose fiber supercapacitor electrode material.
2. The preparation method of the conventional viscose fiber supercapacitor electrode material according to claim 1, wherein the temperature rise rate in the step (1) is 5 ℃/min.
3. The preparation method of the conventional viscose fiber supercapacitor electrode material according to claim 1, wherein Co (NO) in the step (2)3)2·6H2O is 0.65M each.
4. The preparation method of the conventional viscose fiber supercapacitor electrode material according to claim 1, wherein the mass ratio of the pre-carbonized product to KOH in the step (2) is 1: 1.
5. The application of the conventional viscose fiber supercapacitor electrode material is used for the electrode material of a supercapacitor.
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| CN102583333A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing porous nanographite flakes by using corn stalks as carbon source |
| CN102942176A (en) * | 2012-12-04 | 2013-02-27 | 西北师范大学 | Preparation method of cotton fiber coal-base material, and application thereof as electrode material of supercapacitor |
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