CN104167301A - Method for using carbonized Enteromorpha to prepare supercapacitor electrode material - Google Patents
Method for using carbonized Enteromorpha to prepare supercapacitor electrode material Download PDFInfo
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- CN104167301A CN104167301A CN201410242886.0A CN201410242886A CN104167301A CN 104167301 A CN104167301 A CN 104167301A CN 201410242886 A CN201410242886 A CN 201410242886A CN 104167301 A CN104167301 A CN 104167301A
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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
A method for using carbonized Enteromorpha to prepare supercapacitor electrode material. The invention belongs to the technical field of preparation of supercapacitor electrode materials in functional materials, and particularly relates to a method for using Enteromorpha as raw material to prepare carbon material through high-temperature pyrolysis (carbonization). The method is characterized by using the technology of preparing active carbon material through biomass carbonization. The method that is adopted is as follows: after performing vacuum freeze drying on Enteromorpha, high temperature carbonization treatment is performed under gas protection, and active carbon material is obtained after washing and drying. The active carbon material prepared by the invention has the advantages that raw material is easy to get, waste materials are utilized, preparation technology is simple, and the specific area is large. When the active carbon material is prepared into a supercapacitor electrode, good electrochemical stability and typical double-electrical-layer capacitance performance are achieved, and recycling value of Enteromorpha and application potential in the field of energy utilization are shown.
Description
Technical field
The invention belongs to electrode material for super capacitor preparing technical field in functional material, particularly a kind ofly by carbonization Enteromorpha, prepare carbon-based material as the method for electrode material for super capacitor.
Background technology
In recent years, ultracapacitor is with its good charge-discharge performance and be better than the high-specific-power of traditional capacitor, the feature of high power capacity, in fields such as telecommunications, Aero-Space, military and national defense and new-energy automobiles, shows unprecedented application prospect.Electrode material is one of key factor determining ultracapacitor performance, because material with carbon element has good electric conductivity, with and form the feature of loose structure, make material with carbon element obtain extensive concern and research in field of energy source materials.The raw materials wide material sources of material with carbon element, and biomass have low cost and recyclability, become one of important sources of material with carbon element.
Current, utilize pure-natural biological material to prepare porous carbon materials and there are bright prospects, as cocoanut shell, Pericarppium Armeniacae Amarum and bamboo; Utilize Hydrothermal Synthesis technology, rice husk, straw etc. can be changed into carbon micron or nano material, comprise micro particles, sub-micro mitron and nanofiber etc.The method that this template action of utilizing biomass is synthesized ad hoc structure material with carbon element, has controlled and the feature that can scale of pattern, thereby is suitable for amplifying and produces.
Biomass carbonization refers to the process that biomass (stalk: cotton, the vegetable stems such as fiber crops, sunflower of combing, forestry three biologies: forestry waste and wood machining residues) is generated to product and byproduct by certain processes, chemical reaction.The incomplete thermal degradation that biomass occur under without oxidizing atmosphere situations such as air, with the process of the products such as Formed condensable liquid (mixture of wood tar and pyrolkigneous liquid can obtain wood tar, pyrolkigneous liquid by purification separation).The advantages such as biomass carbonization is high because having the rate of heat addition, and heating process is controlled, are widely used.
In recent years, due to reasons such as global climate is abnormal, body eutrophications, the green tide outburst of the large-scale Enteromorpha in ocean often occurs, a large amount of Enteromorphas gather bank, block the fairway, and destroy marine ecosystems, serious harm inshore fishing, tourism development simultaneously.Therefore, research and utilization carbonization Enteromorpha is prepared super capacitor carbon electrode material as raw material and is had the double-deck meaning of environment benefits and economic gains.
At present, there is not yet the relevant report that carbonization Enteromorpha is prepared electrode material for super capacitor both at home and abroad.
Summary of the invention
The object of the present invention is to provide and a kind ofly take natural Enteromorpha as raw material, utilize biomass carbonization method to prepare the method for active carbon material.
Object of the present invention realizes in the following manner, take Enteromorpha as raw material, utilizes biomass carbonization method to prepare active carbon electrode material, comprises the following steps.
(1) Enteromorpha freezing dry process: a certain amount of Enteromorpha is cleaned, carried out vacuum freeze drying.
(2) Enteromorpha carbonisation: the sample of bone dry is placed in to special tube type resistance furnace, is warming up to 600 ~ 950 ℃ under nitrogen atmosphere protection, constant temperature carbonization is 3 ~ 6 hours at this temperature, is cooled to room temperature, uses washed with de-ionized water until filtrate is colourless.
(3) carbide acid cleaning process: carbide is used respectively hydrochloric acid and washed with de-ionized water, to neutral, finally by product vacuumize, obtains needed porous active material with carbon element.
(4) preparation of activated carbon electrodes: by prepared activated carbon sample grind into powder, and be ground in mortar with binding agent PVDF by a certain percentage, drip a small amount of 1-METHYLPYRROLIDONE and be prepared into viscosity mud shape thing, take graphite paper as collector, by active material load on it, then vacuumize, finally obtains electrode material to be prepared.
In described step (2), accompanying drawing 4 is shown in by special tube type resistance furnace.
Vacuumize temperature in described step (3) and (4) is 60 ℃, and be 24 hours drying time.
The ultrasonic power adopting in described step (3) is 60W, and temperature is 60 ℃.
The present invention compares and has following advantages with prior art and material.
1. Enteromorpha raw material cheapness and wide material sources, carbonisation is simple to operation and temperature is controlled, thereby can be suitable for the production of the scale of amplifying.
2. use the prepared porous carbon electrode material of this method larger than electric capacity, good cycling stability.
Accompanying drawing explanation
Fig. 1 is the SEM photo of active carbon material prepared in example 1.
Fig. 2 is the XRD collection of illustrative plates of active carbon material prepared in example 1.
Fig. 3 is the charge-discharge test figure of active carbon electrode material prepared in example 1.
Fig. 4 is the carbonizing plant schematic diagram of the prepared absorbent charcoal material of the present invention: 1. nitrogen cylinder; 2. high pure nitrogen; 3. nitrogen valve; 4. nitrogen pressure reducer; 5. clip; 6. rubber tube; 7. spinner flowmeter; 8. triple valve; 9. vacuum pump; 10. quartz ampoule; 11. high temperature process furnances; 12. temperature controllers; 13,14. tail gas bottles; 15. workbench.
Embodiment
Below by example, the invention will be further described.
Example 1.
By clean Enteromorpha vacuum freeze drying 48 hours, until bone dry.The sample of bone dry is placed in to special tube type resistance furnace; under nitrogen atmosphere protection, be warming up to 950 ℃; constant temperature carbonization 3 hours; under room temperature, take out carbide, clean to filtrate colourlessly, then carbide is placed in to the ultrasonic dispersion of hydrochloric acid solution; then at 60 ℃ of condition lower magnetic forces, stir 12 hours; with deionized water suction filtration to filtrate, be neutral, finally by product vacuumize, obtain needed porous active material with carbon element.By prepared activated carbon sample grind into powder, the ratio that is 9: 1 with binding agent PVDF in active carbon material is mixed, drip a small amount of 1-METHYLPYRROLIDONE and be prepared into viscosity mud shape thing, take graphite paper as collector, viscosity mud shape thing is loaded on graphite paper, after vacuumize, obtain active carbon electrode material to be prepared.
Example 2.
By clean Enteromorpha vacuum freeze drying 48 hours, until bone dry.The sample of bone dry is placed in to special tube type resistance furnace; under nitrogen atmosphere protection, be warming up to 600 ℃; constant temperature carbonization 3 hours; under room temperature, take out carbide, clean to filtrate colourlessly, then carbide is placed in to the ultrasonic dispersion of hydrochloric acid solution; then at 60 ℃ of condition lower magnetic forces, stir 12 hours; with deionized water suction filtration to filtrate, be neutral, finally by product vacuumize, obtain needed porous active material with carbon element.By prepared activated carbon sample grind into powder, the ratio that is 9: 1 with binding agent PVDF in active carbon material is mixed, drip a small amount of 1-METHYLPYRROLIDONE and be prepared into viscosity mud shape thing, take graphite paper as collector, viscosity mud shape thing is loaded on graphite paper, after vacuumize, obtain active carbon electrode material to be prepared.
Claims (5)
1. take Enteromorpha as a raw material, utilize biomass carbonization method to prepare the method for active carbon electrode material, its feature comprises the following steps:
(1) freezing dry process: by clean Enteromorpha vacuum freeze drying 2 ~ 3 days, until Enteromorpha bone dry;
(2) Enteromorpha carbonisation: the sample of bone dry is placed in to special tube type resistance furnace, is warming up to 600 ~ 950 ℃ under nitrogen atmosphere protection, constant temperature carbonization is 3 ~ 6 hours at this temperature, uses washed with de-ionized water until filtrate is colourless;
(3) carbide activation process: carbide is placed in the ultrasonic dispersion of hydrochloric acid solution 1 ~ 2 hour of 4 ~ 6mol/L, then at 60 ℃ of condition lower magnetic forces, stir 12 hours, with deionized water suction filtration to filtrate, be neutral, finally by product vacuumize, obtain needed porous active material with carbon element;
(4) preparation of activated carbon electrodes: by prepared activated carbon sample grind into powder, and even with binding agent PVDF ground and mixed in mortar by a certain percentage, drip a small amount of 1-METHYLPYRROLIDONE and be prepared into viscosity mud shape thing, take graphite paper as carrying the collector of active material, by viscosity mud shape thing blade coating to graphite paper, then vacuumize, finally obtains electrode material to be prepared.
2. according to claim 1ly take Enteromorpha as raw material, utilize biomass carbonization method to prepare the method for active carbon electrode material, it is characterized in that described step (1) raw material is Enteromorpha.
3. according to claim 1ly take Enteromorpha as raw material, utilize biomass carbonization method to prepare the method for active carbon electrode material, it is characterized in that in described step (3), utilizing homemade carbonizing plant, pyrolysis under nitrogen atmosphere, pyrolysis temperature is 600 ~ 950 ℃, and pyrolysis time is 3 ~ 6 hours.
4. according to claim 1ly take Enteromorpha as raw material, utilize biomass carbonization method to prepare the method for active carbon electrode material, it is characterized in that in described step (3), for making material with carbon element activation, adopting chlorohydric acid pickling, concentration of hydrochloric acid is 4 ~ 6mol/L.
5. piece according to claim 1 take Enteromorpha as raw material, utilize biomass carbonization method to prepare the method for active carbon electrode material, it is characterized in that in described step (4), adopting graphite paper is collector; The quality proportioning of active carbon material and binding agent PVDF is 9: 1, and drips a small amount of 1-METHYLPYRROLIDONE and be prepared into viscosity mud shape thing.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502392A (en) * | 2015-12-29 | 2016-04-20 | 山东大学 | Preparation method of micropore-developed activated carbon |
| CN105776182A (en) * | 2016-04-29 | 2016-07-20 | 陕西科技大学 | Preparation method and application of hollow tubular biochar |
| CN106169378A (en) * | 2016-08-30 | 2016-11-30 | 青岛大学 | A kind of Co3o4@Entermorpha porous carbon fiber surpasses the preparation method holding electrode material |
| CN106477574A (en) * | 2016-10-21 | 2017-03-08 | 青岛富强新材料科技有限公司 | A kind of preparation method of environment-friendly multi-stage pore structure lithium ion battery negative pole carbon material |
| CN106477553A (en) * | 2016-08-31 | 2017-03-08 | 青岛大学 | A kind of preparation method of Enteromorpha carbon nanomaterial |
| CN106531476A (en) * | 2016-12-29 | 2017-03-22 | 湖北文理学院 | Preparation method of metal oxide/ carbon composite material |
| CN106622138A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Enteromorpha biochar |
| CN106809834A (en) * | 2017-04-13 | 2017-06-09 | 合肥工业大学 | A kind of method that vacuum freeze drying prepares activated carbon from activated sludge |
| CN106927463A (en) * | 2017-03-30 | 2017-07-07 | 黑龙江大学 | A kind of method for preparing electrode of super capacitor carbon material as carbon source with radish |
| WO2017160237A1 (en) * | 2016-03-17 | 2017-09-21 | Green Waste Recycling Company Pte Ltd | Devices comprising a carbonaceous material, and uses of the material |
| CN107256805A (en) * | 2017-06-01 | 2017-10-17 | 烟台大学 | A kind of electrode material for super capacitor of carbonization and its production and use |
| CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
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2014
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502392A (en) * | 2015-12-29 | 2016-04-20 | 山东大学 | Preparation method of micropore-developed activated carbon |
| WO2017160237A1 (en) * | 2016-03-17 | 2017-09-21 | Green Waste Recycling Company Pte Ltd | Devices comprising a carbonaceous material, and uses of the material |
| CN105776182A (en) * | 2016-04-29 | 2016-07-20 | 陕西科技大学 | Preparation method and application of hollow tubular biochar |
| CN106169378A (en) * | 2016-08-30 | 2016-11-30 | 青岛大学 | A kind of Co3o4@Entermorpha porous carbon fiber surpasses the preparation method holding electrode material |
| CN106477553A (en) * | 2016-08-31 | 2017-03-08 | 青岛大学 | A kind of preparation method of Enteromorpha carbon nanomaterial |
| CN106477574A (en) * | 2016-10-21 | 2017-03-08 | 青岛富强新材料科技有限公司 | A kind of preparation method of environment-friendly multi-stage pore structure lithium ion battery negative pole carbon material |
| CN106531476A (en) * | 2016-12-29 | 2017-03-22 | 湖北文理学院 | Preparation method of metal oxide/ carbon composite material |
| CN106531476B (en) * | 2016-12-29 | 2018-10-02 | 湖北文理学院 | A kind of preparation method of metal oxide/carbon composite |
| CN106622138A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Enteromorpha biochar |
| CN106927463A (en) * | 2017-03-30 | 2017-07-07 | 黑龙江大学 | A kind of method for preparing electrode of super capacitor carbon material as carbon source with radish |
| CN106809834A (en) * | 2017-04-13 | 2017-06-09 | 合肥工业大学 | A kind of method that vacuum freeze drying prepares activated carbon from activated sludge |
| CN107256805A (en) * | 2017-06-01 | 2017-10-17 | 烟台大学 | A kind of electrode material for super capacitor of carbonization and its production and use |
| CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
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Granted publication date: 20170215 |