CN102205963A - Method for preparing activated carbon for biomass-based super capacitor - Google Patents
Method for preparing activated carbon for biomass-based super capacitor Download PDFInfo
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- CN102205963A CN102205963A CN 201110062358 CN201110062358A CN102205963A CN 102205963 A CN102205963 A CN 102205963A CN 201110062358 CN201110062358 CN 201110062358 CN 201110062358 A CN201110062358 A CN 201110062358A CN 102205963 A CN102205963 A CN 102205963A
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- activated carbon
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- super capacitors
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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
The invention discloses a method for preparing activated carbon for a biomass-based super capacitor, in particular relates to a new method for preparing activated carbon with high specific surface area and high specific capacitance by the steps of hydrolysis of biomass with concentrated acid, in-situ polycondensation and carbonization of saccharic acid solution and activation under certain conditions. The method comprises the following specific steps of: firstly, hydrolyzing biomasses with inorganic acid with a certain concentration, and filtering to obtain a saccharic acid solution and filter residues; adjusting the concentration of the saccharic acid solution, performing polycondensation and carbonization to prepare hydrothermal carbon; mixing the hydrothermal carbon with an activating agent in a certain mass ratio for activating to finally obtain the activated carbon for the super capacitor. The method for preparing activated carbon for the super capacitor by using biomasses is a pollution-free process route meeting the requirement of sustainable development.
Description
Technical field
The present invention relates to a kind of preparation method of biomass-based activated carbon for super capacitors, be specifically related to activation treatment under a kind of concentrated acid hydrolyzing biomass, the charing of sugar acid solution in-situ polycondensation, the certain condition, preparation has the novel method of high-specific surface area and high specific capacitance carbon content active.
Background technology
Develop rapidly in social economy, resource is today of shortage day by day, novel energy-storing element ultracapacitor is rapidly developed, it has remedied battery and low, anti-high rate during charging-discharging difference of fuel battery power and the little shortcoming of traditional capacitor energy storage density well, continuous application in fields such as electromobile, mobile communication, information technology, aerospace and science and techniques of defence, make it more and more be subjected to people's attention, various countries make the evolutionary operation(EVOP) of electrochemical capacitor one after another, classify it strategic research object of state key as.The particularly appearance of environmentally friendly vehicle, electromobile, high-power and electrochemical capacitor has more shown its unprecedented application prospect.Therefore, the research of electrochemical capacitor presents unprecedented research boom in recent years.And electrode materials is the key factor of decision electrochemical capacitor performance, so the research of electrochemical capacitor electrode material has become the focus of electrochemical capacitor research.
In the various electrode materialss of ultracapacitor, cheap absorbent charcoal material be most widely used general also be the most sophisticated class of technology.The raw material of wood-charcoal material has good heat conduction and conductivity, and its density is low, and the resist chemical performance is good, and thermal expansivity is little, and Young's modulus is not high.Can make variforms such as powder, bulk, fiber, cloth, felt by different methods, also have multiple allotropic substance (as graphite, diamond, soccerballene) simultaneously, also can have different space structures because of the difference of degree of graphitization, make electrode materials so be widely used in electrochemical field.It is raw material with the refinery coke that patent CNIO1648706A discloses a kind of, through grinding, is that activator prepares activated carbon for super capacitors with potassium hydroxide.It is raw material with hard fruit shells such as apricot shell, peach shell or corn cob that patent CN101759181A discloses a kind of, is activator with a certain amount of phosphoric acid, and potassium primary phosphate or SODIUM PHOSPHATE, MONOBASIC are that expanding agent prepares the gac that specific capacitance reaches 200F/g.It is raw material with starch (oxidative crosslinked starch, corn cationic starch, graft copolymerization starch, Zulkovsky starch or tapioca (flour)) that patent CNIO1525132A discloses a kind of, and potassium hydroxide is the method that activator is produced activated carbon for super capacitors.Above patent is raw materials used there being the limited problem in source in varying degrees, is not suitable for scale operation.
The present invention is on the basis of previous work, with this renewable resources of biomass is raw material, adopt and earlier biomass are carried out acid treatment, utilize its hydrolyzed solution in-situ polycondensation carbonization again, activation treatment under the certain condition, preparation has the novel method of high-specific surface area, high specific capacitance carbon content active, and the method that this kind prepares activated carbon for super capacitors yet there are no patent report.
Summary of the invention
The object of the invention provides a kind of novel method of utilizing biomass to prepare activated carbon for super capacitors.
The present invention at first mixes with the mineral acid of 32～72wt% biomass by solid-to-liquid ratio 1: 5～10 (Kg/L), be warming up to 50 ℃, hydrolysis 10 minutes, filter sugar acid solution and filter residue; The acid concentration of adjusting sugar acid solution is 42～62wt%, is under 95 ℃ in temperature, polycondensation and carbonization reaction 6 hours, and solid filtering, washing, drying make hydro-thermal carbon; To mix by mass ratio 1: 2～5 (Kg/Kg) with activator after 500 ℃ of thermal treatments of hydro-thermal carbon, it was reacted 0.5 hour down at 400 ℃, 750～800 ℃ of following priming reactions 1 hour, solid filtering, washing, drying, the gac of preparation is carried out specific surface area and than capacity measurement, obtains specific surface area and reach 3662m
2/ g, specific capacitance reach the gac of 352F/g.
The invention is characterized in: the biomass of described production activated carbon for super capacitors are agricultural wastes and forestry waste such as sawdust, branch such as rice husk, corn cob, maize straw.
The invention is characterized in: described mineral acid is phosphoric acid, sulfuric acid or its mixed acid solution.
The invention is characterized in: described activator is potassium hydroxide, sodium hydroxide and phosphoric acid.
The invention is characterized in: after the sugar acid solution polycondensation and carbonization, filter gained filtrate, after the adjustment acid concentration, return the hydrolyzing process recycle.
Embodiment
Embodiment 1: with rice husk and 72%H
2SO
4By solid-to-liquid ratio is that 1: 10 (Kg/L) mixes, and places 50 ℃ of water-bath hydrolysis 10 minutes, and regulating acid concentration is 52%, filters to obtain sugar acid solution; Sugar acid solution was placed 95 ℃ of water-bath carbonization reaction 6 hours again, filtration, washing, drying, get hydro-thermal carbon, to mix at 1: 3 by mass ratio with potassium hydroxide after 500 ℃ of thermal treatments of hydro-thermal carbon, 400 ℃ were reacted 0.5 hour, 800 ℃ of following priming reactions 1 hour, solid filtering, washing, drying, the preparation specific surface area is 2185m
2/ g, specific capacitance are the activated carbon for super capacitors of 225F/g.
Embodiment 2: changing hydro-thermal carbon is 1: 4 with the activator level ratio, and other conditions are with embodiment 1, and preparing specific surface area is 2435m
2/ g, specific capacitance are the activated carbon for super capacitors of 256F/g.
Embodiment 3: changing hydro-thermal carbon is 1: 5 with the activator level ratio, and other conditions are with embodiment 1, and preparing specific surface area is 3276m
2/ g, specific capacitance are the activated carbon for super capacitors of 272F/g.
Embodiment 4: changing hydro-thermal carbon is 1: 2 with the activator level ratio, and other conditions are with embodiment 1, and preparing specific surface area is 1948m
2/ g, specific capacitance are the activated carbon for super capacitors of 193F/g.
Embodiment 5: the acid concentration that changes polycondensation and carbonization is 42%, and other conditions are with embodiment 3, and preparing specific surface area is 3662m
2/ g, specific capacitance are the activated carbon for super capacitors of 352F/g.
Embodiment 6: the acid concentration that changes polycondensation and carbonization is 62%, and other conditions are with embodiment 3, and preparing specific surface area is 2907m
2/ g, specific capacitance are the activated carbon for super capacitors of 269F/g.
Embodiment 7: the change activator is a sodium hydroxide, and hydro-thermal carbon and activator mass ratio are 1: 3,400 ℃ of down reactions 0.5 hour, and 750 ℃ of following priming reactions 1 hour, other conditions are with embodiment 1, and preparing specific surface area is 2238m
2/ g, specific capacitance are the activated carbon for super capacitors of 213F/g.
Embodiment 8: the solid-to-liquid ratio that changes the rice husk sulphuric acid hydrolysis is 1: 5 (Kg/L), and other conditions are with embodiment 3, and preparing specific surface area is 3058m
2/ g, specific capacitance are the activated carbon for super capacitors of 270F/g.
Embodiment 9: the change activator is a phosphoric acid, and hydro-thermal carbon is 1: 5 with the phosphoric acid quality ratio, 500 ℃ of following priming reactions 1 hour, and solid filtering, washing, drying, preparing specific surface area is 2180m
2/ g, specific capacitance are the activated carbon for super capacitors of 208F/g.
Embodiment 10: changing the sulfuric acid massfraction is 52%, with rice husk and 52%H
2SO
4By solid-to-liquid ratio is that 1: 10 (Kg/L) mixes, and other conditions are with embodiment 1, and preparing specific surface area is 2013m
2/ g, specific capacitance are the activated carbon for super capacitors of 196F/g.
Claims (5)
1. the production method of biomass-based activated carbon for super capacitors, its concrete steps are as follows:
At first biomass are mixed by solid-to-liquid ratio 1: 5～10 (Kg/L) with the mineral acid of 32～72wt%, are warming up to 50 ℃, hydrolysis 10 minutes, filter sugar acid solution and filter residue; The acid concentration of adjusting sugar acid solution is 42～62wt%, is 95 ℃ of following polycondensation and carbonization reaction 6 hours in temperature, filters washing, drying, preparation hydro-thermal carbon; Hydro-thermal carbon is mixed by mass ratio 1: 2～5 (Kg/Kg) with activator, with mixture 400 ℃ of down reactions 0.5 hour, 750～800 ℃ of priming reactions 1 hour, solid filtering, washing, drying, the gac of preparation high-specific surface area and high specific capacitance amount.
2. the production method of a biomass-based activated carbon for super capacitors as claimed in claim 1, it is characterized in that: the biomass of described production gac are: agricultural wastes and forestry waste such as sawdust, branch such as rice husk, corn cob, maize straw.
3. the production method of a biomass-based activated carbon for super capacitors as claimed in claim 1, it is characterized in that: described mineral acid is phosphoric acid, sulfuric acid or its mixed acid solution.
4. the production method of a biomass-based activated carbon for super capacitors as claimed in claim 1, it is characterized in that: described activator is potassium hydroxide, sodium hydroxide or phosphoric acid.
5. the production method of a biomass-based activated carbon for super capacitors as claimed in claim 1 is characterized in that: after the sugar acid solution polycondensation and carbonization, filter gained filtrate, after the adjustment acid concentration, return the hydrolyzing process recycle.
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| CN 201110062358 CN102205963A (en) | 2011-03-16 | 2011-03-16 | Method for preparing activated carbon for biomass-based super capacitor |
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| CN 201110062358 CN102205963A (en) | 2011-03-16 | 2011-03-16 | Method for preparing activated carbon for biomass-based super capacitor |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102568851A (en) * | 2012-01-19 | 2012-07-11 | 山东理工大学 | Rice hull multi-stage porous carbon counter electrode of dye sensitized solar cell and preparation method |
| CN102709066A (en) * | 2012-07-03 | 2012-10-03 | 吉林大学 | Water system symmetrical electrochemical capacitor based on rice husk porous carbon |
| CN103274391A (en) * | 2013-06-26 | 2013-09-04 | 吉林大学 | Preparation method of alkali soluble water heat carbon |
| CN103539118A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for supercapacitor |
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN104307480A (en) * | 2014-11-18 | 2015-01-28 | 成都理想财富投资咨询有限公司 | Preparing method for printing and dyeing sewage treatment magnetic particles |
| CN104477908A (en) * | 2014-12-26 | 2015-04-01 | 海南大学 | Method for preparing activated carbon with chitosan used as raw material and obtainedactivated carbon |
| CN105129770A (en) * | 2015-08-31 | 2015-12-09 | 吉林大学 | Morphological control method for functional hydrothermal carbon |
| WO2016072932A1 (en) * | 2014-11-04 | 2016-05-12 | National University Of Singapore | Activated carbon, hydrochar and processes for making same |
| CN107098332A (en) * | 2017-06-26 | 2017-08-29 | 东北大学 | A kind of method that high temperature cabonization organic matter prepares carbon-based absorbing material |
| CN107403698A (en) * | 2017-09-11 | 2017-11-28 | 湖南农业大学 | A kind of application that the method for activated carbon and its activated carbon of preparation are prepared using biomass |
| CN107555424A (en) * | 2017-08-31 | 2018-01-09 | 西南大学 | A kind of preparation method of porous class graphene active carbon material and products thereof and application |
| CN110240158A (en) * | 2019-07-02 | 2019-09-17 | 天津工业大学 | A kind of method for preparation of active carbon based on phytic acid and saccharide compound |
| CN110577222A (en) * | 2019-10-21 | 2019-12-17 | 中国矿业大学 | Activated carbon and preparation method and application thereof |
| CN113415803A (en) * | 2021-08-12 | 2021-09-21 | 中国科学院生态环境研究中心 | Waste treatment method |
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| CN1919730A (en) * | 2006-09-13 | 2007-02-28 | 海南大学 | Method of preparing low ash high specific surface area active carbon from coconut shell slag |
| CN101811692A (en) * | 2010-05-05 | 2010-08-25 | 吉林大学 | New method for comprehensive utilization of straw resource |
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2011
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| CN1919730A (en) * | 2006-09-13 | 2007-02-28 | 海南大学 | Method of preparing low ash high specific surface area active carbon from coconut shell slag |
| CN101811692A (en) * | 2010-05-05 | 2010-08-25 | 吉林大学 | New method for comprehensive utilization of straw resource |
Non-Patent Citations (1)
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| 《高等学校化学学报》 20000331 郭玉鹏 等 由稻壳制备高比表面积活性炭 335-338 1-5 第21卷, 第3期 * |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102568851A (en) * | 2012-01-19 | 2012-07-11 | 山东理工大学 | Rice hull multi-stage porous carbon counter electrode of dye sensitized solar cell and preparation method |
| CN102709066A (en) * | 2012-07-03 | 2012-10-03 | 吉林大学 | Water system symmetrical electrochemical capacitor based on rice husk porous carbon |
| CN103663448B (en) * | 2012-09-19 | 2017-08-01 | 天津普兰纳米科技有限公司 | Preparation method, gained carbon material and its application of carbon material |
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN103274391A (en) * | 2013-06-26 | 2013-09-04 | 吉林大学 | Preparation method of alkali soluble water heat carbon |
| CN103539118B (en) * | 2013-10-30 | 2015-12-30 | 中国第一汽车股份有限公司 | A kind of method for preparation of active carbon for ultracapacitor |
| CN103539118A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for supercapacitor |
| WO2016072932A1 (en) * | 2014-11-04 | 2016-05-12 | National University Of Singapore | Activated carbon, hydrochar and processes for making same |
| CN104307480A (en) * | 2014-11-18 | 2015-01-28 | 成都理想财富投资咨询有限公司 | Preparing method for printing and dyeing sewage treatment magnetic particles |
| CN104477908A (en) * | 2014-12-26 | 2015-04-01 | 海南大学 | Method for preparing activated carbon with chitosan used as raw material and obtainedactivated carbon |
| CN105129770A (en) * | 2015-08-31 | 2015-12-09 | 吉林大学 | Morphological control method for functional hydrothermal carbon |
| CN107098332A (en) * | 2017-06-26 | 2017-08-29 | 东北大学 | A kind of method that high temperature cabonization organic matter prepares carbon-based absorbing material |
| CN107555424A (en) * | 2017-08-31 | 2018-01-09 | 西南大学 | A kind of preparation method of porous class graphene active carbon material and products thereof and application |
| CN107403698A (en) * | 2017-09-11 | 2017-11-28 | 湖南农业大学 | A kind of application that the method for activated carbon and its activated carbon of preparation are prepared using biomass |
| CN107403698B (en) * | 2017-09-11 | 2019-04-09 | 湖南农业大学 | A kind of application preparing the method for activated carbon and its active carbon of preparation using biomass |
| CN110240158A (en) * | 2019-07-02 | 2019-09-17 | 天津工业大学 | A kind of method for preparation of active carbon based on phytic acid and saccharide compound |
| CN110577222A (en) * | 2019-10-21 | 2019-12-17 | 中国矿业大学 | Activated carbon and preparation method and application thereof |
| CN113415803A (en) * | 2021-08-12 | 2021-09-21 | 中国科学院生态环境研究中心 | Waste treatment method |
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Application publication date: 20111005 |