CN112599367B - Method for preparing lotus root starch derived carbon electrode material with assistance of microwaves - Google Patents
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- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 33
- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 33
- 229920002472 Starch Polymers 0.000 title claims abstract description 33
- 239000008107 starch Substances 0.000 title claims abstract description 33
- 235000019698 starch Nutrition 0.000 title claims abstract description 33
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 239000003513 alkali Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 2
- 239000012776 electronic material Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229930091371 Fructose Natural products 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000011276 addition treatment Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
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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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a micro-meterA method for preparing lotus root starch derived carbon electrode material with wave assistance belongs to the technical field of new energy electronic materials. The obtained electrode material is cheap and easy to obtain, and has excellent electrochemical performance. The preparation method of the lotus root starch derived carbon electrode material prepared by microwave assistance comprises the following steps: weighing 10g of lotus root starch and 20ml of deionized water, dispersing, transferring into a microwave reaction kettle, and heating for 6 hours at 190 ℃. Cooling to room temperature, suction filtering, washing and drying. According to mSample (A)：mKOH=1: 0.5 KOH was dissolved in a beaker and mixed with the sample and dried. The sample was heated at 700 ℃ for 1 h. And (5) carrying out sample preparation test after acid washing and drying. The obtained lotus root starch-derived carbon electrode material is prepared at 0.2A g‑1The specific capacitance value is 480g‑1，10 A g‑1The capacity retention rate reaches 0.2Ag‑155% of the total amount, excellent electrochemical performance. The lotus root starch derived carbon electrode material prepared by the invention has the advantages of low cost, low price, easy obtainment, stable structure and high practical application value.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to a method for preparing a lotus root starch derived carbon supercapacitor electrode material by microwave assistance.
Background
With the unregulated exploitation and utilization of fossil fuels and the pollution and destruction of the environment, the traditional energy situation can not meet the sustainable requirements of the existing economic development, and novel energy forms such as wind energy, solar energy, lithium ion batteries, super capacitors and other novel energy storage devices are demanded. The super capacitor has the advantages of high charging and discharging speed, high specific capacity and the like, is expected to become energy storage equipment with the greatest prospect and practical value. The performance of the supercapacitor is often dependent on the performance of the electrode material, so that finding a suitable electrode material is important. The natural biomass material is widely concerned by people because of wide distribution, low price, easy obtaining, no toxicity and no harm, and is an electrode material with wide application prospect.
The lotus root starch contains a large amount of glucose, fructose and other saccharides, can form a carbon microspherical shape after carbonization, and has better shape characteristics and electrochemical performance. At present, the application of the lotus root starch in the aspect of electrode materials of the super capacitor is not reported. In order to further develop the application of the lotus root starch in the aspect of electrode materials of the super capacitor, further research and promotion are carried out on the lotus root starch to obtain better electrochemical performance. (Bo, XK; Xiaong, K; Zhang, Y; et al. Microwave-assisted conversion of biological waters to pseudoatmospheric hydrocarbons for high-performance supercapacitors [ J ]. Journal of energy chemistry, 2019, 39: 1-7.)
In order to improve the electrochemical performance of the lotus root starch-based derived carbon material supercapacitor, a typical and effective method is to adopt a microwave-assisted KOH activation carbonization method, and the activated carbon material is a biomass derived carbon electrode material with a larger comparative area and a higher specific capacity. The invention takes lotus root starch purchased in the market as a raw material, has rich sources, and is cheap and easy to obtain. The lotus root starch derived carbon is prepared by microwave assistance, and then is carbonized and activated at high temperature, so that the prepared lotus root starch derived carbon has excellent electrochemical performance when being used as a super capacitor electrode material. At 0.2A g-1The specific capacitance value is 480F g-1，10 A g-1Can still reach 264F g-1The capacitance value remains 0.2A g-155% of the time, a new way of thinking is provided for the application of biomass as the electrode material of the super capacitor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the method for preparing the lotus root starch derived carbon electrode material with microwave assistance, which is simple, low in cost and excellent in performance.
The technical scheme of the invention is as follows:
an electrode material of a super capacitor is prepared by preparing lotus root starch derived carbon with the assistance of microwave.
According to the invention, the preparation method of the lotus root starch derived carbon electrode material prepared by microwave assistance comprises the following steps:
(1) weighing 10g of lotus root starch and 20ml of deionized water, uniformly dispersing, and then transferring into a microwave reaction kettle. Setting the reaction temperature to be 160-200oAnd C, reacting for 2-6 h, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying.
(2) After drying, alkali treatment is carried out according to mSample (A):mKOHAnd (3) dissolving KOH in a beaker at a ratio of 1: 0.2-1: 2, mixing the dissolved KOH with a sample, and drying the mixture.
(3) High-temperature carbonization activation is carried out in Ar gas atmosphere, and the setting parameter is 650-750oC, the rate of temperature rise is 5 oC/min, and keeping the temperature for 1 h. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
According to the present invention, it is preferable that the optimum reaction temperature in the step (1) is 190oC。
According to the present invention, it is preferred that the optimal reaction time in step (1) is 6 hours.
According to the present invention, it is preferable that the optimum ratio by mass of the alkali addition treatment in the step (2) is 1: 0.5.
According to the present invention, it is preferable that the optimum activating carbonization temperature in the step (3) is 700oC。
The technical advantages of the invention are as follows:
(1) the raw material of the invention is lotus root starch, which is easy to prepare and low in price.
(2) The invention adopts microwave-assisted preparation of the lotus root starch derived carbon material to obtain a carbon microsphere shape with the diameter of about 4.5um, and the material has the advantages of high graphitization degree, stable structure, excellent electrochemical performance and the like.
Description of the figures and accompanying tables
FIG. 1 is a scanning electron microscope image of the lotus root starch-based derived carbon material prepared in example 1 of the present invention.
FIG. 2 is a graph showing the charge and discharge performance of the lotus root starch-based derived carbon material obtained in example 1 of the present invention.
FIG. 3 is a graph showing capacitance values of the lotus root starch-based derived carbon material obtained 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:
10g of lotus root starch and 20ml of deionized water are weighed and transferred into a microwave reaction kettle after dispersion. Set up the reactionThe temperature is 190 ℃, the reaction time is 6 hours, the reaction solution is cooled to room temperature and then is filtered, and then deionized water and absolute ethyl alcohol are used for washing and drying. After drying, alkali treatment is carried out according to mSample (A)：mKOH=1: 0.5, dissolving KOH in a beaker, mixing with the sample, and drying. And (3) keeping the temperature of the dried sample at 700 ℃ and 5 ℃/min for 1h under Ar atmosphere. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
Example 2:
10g of lotus root starch and 20ml of deionized water are weighed and transferred into a microwave reaction kettle after dispersion. Setting the reaction temperature at 190 ℃ and the reaction time at 6 hours, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying. After drying, alkali treatment is carried out according to mSample (A)：mKOH=1:0.2, dissolving KOH in a beaker, mixing with the sample, and drying. And (3) keeping the temperature of the dried sample at 700 ℃ and 5 ℃/min for 1h under Ar atmosphere. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
Example 3:
10g of lotus root starch and 20ml of deionized water are weighed and transferred into a microwave reaction kettle after dispersion. Setting the reaction temperature at 190 ℃ and the reaction time at 6 hours, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying. After drying, alkali treatment is carried out according to mSample (A)：mKOH=1: 0.75, dissolving KOH in a beaker, mixing with the sample, and drying. And (3) keeping the temperature of the dried sample at 700 ℃ and 5 ℃/min for 1h under Ar atmosphere. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
Example 4:
10g of lotus root starch and 20ml of deionized water are weighed and transferred into a microwave reaction kettle after dispersion. Setting the reaction temperature at 190 ℃ and the reaction time at 6 hours, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying. After drying, alkali treatment is carried out according to mSample (A)：mKOH=1: 1, dissolving KOH in a beaker, mixing with a sample, and dryingAnd (5) drying. And (3) keeping the temperature of the dried sample at 700 ℃ and 5 ℃/min for 1h under Ar atmosphere. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
Example 5:
10g of lotus root starch and 20ml of deionized water are weighed and transferred into a microwave reaction kettle after dispersion. Setting the reaction temperature at 190 ℃ and the reaction time at 6 hours, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying. After drying, alkali treatment is carried out according to mSample (A)：mKOH=1: 2, dissolving KOH in a beaker, mixing with the sample, and drying. And (3) keeping the temperature of the dried sample at 700 ℃ and 5 ℃/min for 1h under Ar atmosphere. The sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
Claims (1)
1. A preparation method for preparing lotus root starch derived carbon electrode material with the assistance of microwave, wherein the microscopic morphology of the lotus root starch derived carbon electrode material is a carbon microsphere with the diameter of 4.5 um;
the preparation method comprises the following steps:
(1) weighing 10g of lotus root starch and 20ml of deionized water, uniformly dispersing, and then transferring into a microwave reaction kettle; setting the reaction temperature to 190 ℃ and the reaction time to 6h, cooling to room temperature, performing suction filtration, washing with deionized water and absolute ethyl alcohol in sequence, and drying;
(2) after drying, alkali treatment is carried out according to mSample (A):mKOH1:0.5, dissolving KOH in a beaker, mixing with a sample, and drying;
(3) carrying out high-temperature carbonization activation in Ar gas atmosphere, setting parameters to be 700 ℃, heating rate to be 5 ℃/min, and keeping the temperature for 1 h; the sample preparation test was performed after acid washing with 1M HCl aqueous solution and drying.
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| CN111146451A (en) * | 2019-12-27 | 2020-05-12 | 扬州大学 | Lotus root starch carbon sphere biofuel cell and preparation method thereof |
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| CN107697913B (en) * | 2017-11-17 | 2020-06-23 | 四川理工学院 | Preparation method of walnut shell-based high-capacitance graded porous carbon |
| CN108821257B (en) * | 2018-05-02 | 2021-11-16 | 福建农林大学 | Lotus leaf-based binary mesoporous-microporous multilevel structure biochar and preparation method and application thereof |
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