CN104150478A - Green cycle process for preparing activated carbon material for supercapacitors by using rice husks - Google Patents
Green cycle process for preparing activated carbon material for supercapacitors by using rice husks Download PDFInfo
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Abstract
The invention discloses a green cycle process for preparing an activated carbon material for supercapacitors by using rice husks, and belongs to the technical field of comprehensive utilization of resources and electrochemical supercapacitors. The method comprises the following steps: carbonizing rice husks under the protection of inert gas so as to obtain a carbonized product, adding alkali into the carbonized product, and sequentially activating, washing, filtrating and drying so as to obtain high-specific-capacitance rice husk charcoal; adding hydrochloric acid into filtrate for acidifying, and sequentially aging, filtrating, washing and drying so as to obtain nano-silica; carrying out impurity removal, concentration, primary refining, secondary refining and electrolysis on the filtrate so as to obtain dilute alkali liquor, evaporating and crystallizing the dilute alkali liquor so as to obtain alkali, taking the obtained alkali as an activator used in the activation process, and taking water obtained in the process of evaporation as water for washing, so that the cyclic utilization of alkali and water is realized. According to the invention, capacitance charcoal capable of being used for the supercapacitors is prepared by using cheap rice husks; silicon-containing waste liquid can be converted into nano-silica, so that the green conversion of high-value-added rice husks is realized, therefore, the green cycle process has a high economic benefit.
Description
Technical field
The invention belongs to comprehensive utilization of resources and electric chemical super capacitor technical field, refer more particularly to a kind of green circulatory technique of being prepared activated carbon for super capacitors material by rice husk.
Background technology.
Ultracapacitor, as a kind of novel energy storage device, because it has the features such as power density is large, efficiency for charge-discharge is high, have extended cycle life, has been subject to people's extensive concern.Electrode materials is the important factor that determines ultracapacitor performance.Gac, owing to having good electrology characteristic, aboundresources, price that structure is various and suitable, has become the electrode material for super capacitor that has commercial competitiveness most.Gac, generally taking carbon containing precursor as raw material, prepares through high temperature carbonization, activation.Carbonization process is in fact the enrichment process of charcoal, has just formed preliminary pore texture.The absorbent charcoal material with excellent properties depends primarily on its presoma and activation method.Presoma prepared by gac mainly contains coal, oil, timber, polymkeric substance and biological material.Biomass source is wide, has recyclability, more and more by people are paid attention to.
The waste that rice husk produces as the paddy course of processing, quantity is very huge.Rice husk effectively utilizes significant for resource, environment and social development.The correlative study of preparing gac with rice husk has become a focus.In recent years, many patent reports prepare the method for activated carbon for super capacitors material taking rice husk as raw material.
Patent CN102431993A discloses a kind of method of preparing mesoporous activated carbon for supercapacitors material taking rice husk as raw material, the method is taking rice husk as carbon source, zinc chloride is activator, obtain Mesoporous Carbon Materials by Microwave-assisted firing zinc chloride activation rice husk, prepared gac has higher middle pore distribution, and the electrode materials that sets it as electrochemical capacitor has good fast charging and discharging performance.Patent CN102205963A discloses a kind of preparation method who prepares activated carbon for super capacitors taking rice husk as raw material, rice husk is obtained to sugar acid solution with certain density mineral acid hydrolysis, prepare hydro-thermal carbon by polycondensation and carbonization, prepare activated carbon for super capacitors with activator activation hydro-thermal carbon, the gac of acquisition has higher ratio electric capacity.But, these patents exist activator and water consumption high, the problem such as discharging of waste liquid amount is large, and preparation cost is high, and environmental pollution is serious.Prepared by rice husk in order to solve that cost in electric capacity charcoal process is high, the large problem of waste discharge amount, patent CN101804988A discloses a kind of method of utilizing rice husk to prepare gac simultaneously to reclaim silicon-dioxide, in the method, generate water glass by reacting with rice hull ash after raw material sodium carbonate pyrolytic decomposition, after water-soluble, obtain water glass and gac, water glass generates silicon-dioxide with the carbon dioxide reaction passing into, and has realized the recycle of sodium carbonate.Patent CN101920966A discloses a kind of method of utilizing rice hull ash to prepare gac and porous nano silica, rice hull ash alkali under subcarbonate is molten, after filtration, in filtrate, add dispersion agent to prepare porous nano silica, filter residue adds activator, activation obtains active carbon with high specific surface area, and this patent has realized the recycle of the molten silicon process of rice hull ash carbonate used.But these patents have only been paid close attention to the comprehensive utilization of rice husk composition, the gac of preparation can not be used for ultracapacitor, and water consumption is high, the large problem of discharging of waste liquid amount does not also solve.
Summary of the invention
Technical scheme of the present invention is as follows:
A green circulatory technique of being prepared activated carbon for super capacitors material by rice husk, mainly comprises the following steps:
(1) rice husk is cleaned, is dried, is ground;
(2) rice husk above-mentioned steps (1) being obtained carries out charing under nitrogen or argon shield, obtains rice hull carbon compound;
(3) carbide above-mentioned steps (2) being obtained and potassium hydroxide or sodium hydroxide activator in mass ratio 1:1-5 mix, and add water to mix, and dry, and activate;
(4) activation products are added in 50-100 DEG C of water and soak, filter, wash neutrality with boiling water, filter, after 100-120 DEG C of dry 12-24h, be ground to 150-300 order and obtain high specific capacitance rice husk matrix activated carbon material;
(5) filtrate in above-mentioned steps (4) is reclaimed, adjustment temperature is 50-100 DEG C, adding concentration is that 2%-20% hydrochloric acid soln carries out acidifying, controlling hydrochloric acid rate of addition is 0.1-1ml/min, control terminal pH=3-9, digestion time 0.5-5h, filters, washs, is dried, and obtains nano silicon product;
(6) by filtering the filtrate purifying that obtains, refining in above-mentioned steps (5), obtain Repone K or sodium chloride solution;
(7) above-mentioned steps (6) is obtained to Repone K or sodium chloride solution and utilize the waste heat evaporation that produces in above-mentioned steps (3), be concentrated into saturatedly, obtain saturated Repone K or sodium chloride solution, the distilled water that evaporation obtains reclaims for subsequent use;
(8) the saturated Repone K or the sodium chloride solution that above-mentioned steps (7) are obtained carry out primary purification and secondary refining, obtain the saturated Repone K of secondary or sodium chloride solution;
(9) saturated Repone K above-mentioned steps (8) being obtained or sodium chloride solution adopt ion-exchange membrane electrolyzer electrolysis, obtain potassium hydroxide or sodium hydroxide solution;
(10) by the potassium hydroxide obtaining in above-mentioned steps (9) or sodium hydroxide solution evaporation, crystallization, dry, obtain solid potassium hydroxide or sodium hydroxide, as the alkali activator recycle in step (3), the distilled water that evaporation obtains reclaims for subsequent use;
(11) bath water for step (4), (5) by the distilled water obtaining in above-mentioned steps (7) and step (10), realizes the recycle of water in preparation process.
Carbonization temperature described in step (2) is 350 DEG C-550 DEG C, carbonization time 0.5-2h.
The described activation condition of step (3) is: control 2-15 DEG C/min of heat-up rate, at 600-900 DEG C, activate 0.5-4h.
Beneficial effect: the advantage that the present invention has is: the high-quality rice husk matrix activated carbon and the nano silicon that can be used for ultracapacitor except can utilize rice husk to prepare simultaneously, realize outside rice husk comprehensive utilization of resources, also solve waste water pollution problem in the preparation process of existing rice husk matrix activated carbon, set up green circulatory technique, reduced production cost.
Brief description of the drawings
Fig. 1 is prepared the green circulatory process flow sheet of activated carbon for super capacitors material by rice husk.
Embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1:
(1) rice husk is cleaned, is dried, is ground;
(2) rice husk after above-mentioned steps (1) is ground is under nitrogen protection, and charing 2h at 450 DEG C, obtains rice hull carbon compound;
(3) carbide above-mentioned steps (2) being obtained and KOH in mass ratio 1:3 mix, and add a certain amount of water to mix, and dry, and control 10 DEG C/min of heat-up rate, at 750 DEG C, activate 1h;
(4) activation products are added in 90 DEG C of water and soak, filter, wash neutrality with boiling water, after 100 DEG C of dry 12h, obtain rice husk matrix activated carbon material, specific surface area 3235cm2/g, mean pore size 2.0nm, the ratio electric capacity of the rice hull carbon of preparation in 6M KOH solution is 331F/g, under current density 1A/g, after 2000 cycle charge-discharges, is 93.5% than electric capacity conservation rate, in the time that current density increases to 10A/g by 1A/g, electric capacity conservation rate is 67.2%;
(5) filtrate in above-mentioned steps (4) being reclaimed, is that at 70 DEG C, to add concentration be that 5% hydrochloric acid soln carries out acidifying in temperature, and controlling hydrochloric acid rate of addition is 0.2ml/min, controls terminal pH=6.5, digestion time 2h.Filter, washing, dry, the nano silicon that obtain median size and be 56nm, purity and be 99.5%, whiteness is 99.7%;
(6) filtrate in above-mentioned steps (5) is added to precipitation agent BaCl successively
2, K
2cO
3, KOH removes the SO containing in filtrate
4 2-, Ca
2+, Mg
2+, obtain the aqueous solution that contains Repone K;
(7) aqueous solution evaporate that above-mentioned steps (6) obtained contain Repone K, be concentrated into saturatedly, obtain saturated potassium chloride solution, the distilled water that evaporation obtains reclaims for subsequent use;
(8) saturated potassium chloride solution above-mentioned steps (7) being obtained is carried out primary purification and secondary refining, obtains secondary saturated potassium chloride solution;
(9) saturated potassium chloride solution above-mentioned steps (8) being obtained adopts ion-exchange membrane electrolyzer electrolysis, and electrolyzer anode chamber produces chlorine, and negative electrode generates hydrogen, obtains potassium hydroxide solution in cathodic area;
(10) by the potassium hydroxide solution evaporation obtaining in above-mentioned steps (9), crystallization, dry, obtain solid potassium hydroxide, the potassium hydroxide rate of recovery is 97.2%, can be used as the potassium hydroxide activator recycle in step (3), the distilled water that evaporation obtains reclaims for subsequent use;
(11) bath water for step (4), (5) by the distilled water obtaining in above-mentioned steps (6) and step (10), the water rate of recovery is 91.6%.
Embodiment 2
(1) rice husk is cleaned, is dried, is ground;
(2) rice husk after above-mentioned steps (1) is ground is under argon shield, and charing 2h at 450 DEG C, obtains rice hull carbon compound;
(3) carbide above-mentioned steps (2) being obtained and NaOH in mass ratio 1:4 mix, and add a certain amount of water to mix, and dry, and control 10 DEG C/min of heat-up rate, at 800 DEG C, activate 2h;
(4) activation products are joined in the water of 90～100 DEG C and soak, filter, wash neutrality with boiling water, after 120 DEG C of dry 12h, obtain rice husk matrix activated carbon material, specific surface area 2753cm2/g, mean pore size 2.3nm, the rice hull carbon of preparation is at 1M H
2sO
4in record material ratio electric capacity be 305F/g, under current density 1A/g, after 10000 cycle charge-discharges, be 96.8% than electric capacity conservation rate, in the time that current density increases to 10A/g by 1A/g, electric capacity conservation rate is 70.1%;
(5) filtrate in above-mentioned steps (4) is reclaimed, carry a temperature and be that at 80 DEG C, to add concentration be that 10% hydrochloric acid soln carries out acidifying, controlling hydrochloric acid rate of addition is 0.5ml/min, controls terminal pH=8.5, digestion time 2h.Filter, washing, dry, the nano silicon that obtain median size and be 87nm, purity and be 99.3%, whiteness is 99.6%;
(6) filtrate in above-mentioned steps (5) is added to precipitation agent BaCl successively
2, K
2cO
3, KOH removes the SO containing in filtrate
4 2-, Ca
2+, Mg
2+, obtain the aqueous solution that contains sodium-chlor;
(7) aqueous solution evaporate that above-mentioned steps (6) obtained contain sodium-chlor, be concentrated into saturatedly, obtain saturated nacl aqueous solution, the distilled water that evaporation obtains reclaims for subsequent use;
(8) saturated nacl aqueous solution above-mentioned steps (7) being obtained carries out primary purification and secondary refining, obtains secondary saturated nacl aqueous solution;
(9) saturated nacl aqueous solution above-mentioned steps (8) being obtained adopts ion-exchange membrane electrolyzer electrolysis, and electrolyzer anode chamber produces chlorine, and negative electrode generates hydrogen, obtains sodium hydroxide solution in cathodic area;
(10) by the sodium hydroxide solution evaporation obtaining in above-mentioned steps (9), crystallization, dry, obtain solid sodium hydroxide, the sodium hydroxide rate of recovery is 95.3%, can be used as the sodium hydroxide activator recycle in step (3), the distilled water that evaporation obtains reclaims for subsequent use;
(11) bath water for step (4), (5) by the distilled water obtaining in above-mentioned steps (6) and step (10), the water rate of recovery is 90.7%.
Claims (3)
1. a green circulatory technique of being prepared activated carbon for super capacitors material by rice husk, mainly comprises the following steps:
(1) rice husk is cleaned, is dried, is ground;
(2) rice husk above-mentioned steps (1) being obtained carries out charing under nitrogen or argon shield, obtains rice hull carbon compound;
(3) carbide above-mentioned steps (2) being obtained and potassium hydroxide or sodium hydroxide activator in mass ratio 1:1-5 mix, and add water to mix, and dry, and activate;
(4) activation products are added in 50-100 DEG C of water and soak, filter, wash neutrality with boiling water, filter, after 100-120 DEG C of dry 12-24h, be ground to 150-300 order and obtain high specific capacitance rice husk matrix activated carbon material;
(5) filtrate in above-mentioned steps (4) is reclaimed, adjustment temperature is 50-100 DEG C, adding concentration is that 2%-20% hydrochloric acid soln carries out acidifying, controlling hydrochloric acid rate of addition is 0.1-1ml/min, control terminal pH=3-9, digestion time 0.5-5h, filters, washs, is dried, and obtains nano silicon product;
It is characterized in that, further comprising the steps of:
(6) by filtering the filtrate purifying that obtains, refining in above-mentioned steps (5), obtain Repone K or sodium chloride solution;
(7) above-mentioned steps (6) is obtained to Repone K or sodium chloride solution and utilize the waste heat evaporation that produces in above-mentioned steps (3), be concentrated into saturatedly, obtain saturated Repone K or sodium chloride solution, the distilled water that evaporation obtains reclaims for subsequent use;
(8) the saturated Repone K or the sodium chloride solution that above-mentioned steps (7) are obtained carry out primary purification and secondary refining, obtain the saturated Repone K of secondary or sodium chloride solution;
(9) saturated Repone K above-mentioned steps (8) being obtained or sodium chloride solution adopt ion-exchange membrane electrolyzer electrolysis, obtain potassium hydroxide or sodium hydroxide solution;
(10) by the potassium hydroxide obtaining in above-mentioned steps (9) or sodium hydroxide solution evaporation, crystallization, dry, obtain solid potassium hydroxide or sodium hydroxide, as the alkali activator recycle in step (3), the distilled water that evaporation obtains reclaims for subsequent use;
(11) bath water for step (4), (5) by the distilled water obtaining in above-mentioned steps (7) and step (10), realizes the recycle of water in preparation process.
2. a kind of green circulatory technique of being prepared activated carbon for super capacitors material by rice husk according to claim 1, is characterized in that: described carbonization temperature is 350 DEG C-550 DEG C, carbonization time 0.5-2h.
3. a kind of green circulatory technique of being prepared activated carbon for super capacitors material by rice husk according to claim 1, is characterized in that: described activation condition is: control 2-15 DEG C/min of heat-up rate, at 600-900 DEG C, activate 0.5-4h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668566A (en) * | 2016-03-11 | 2016-06-15 | 宁国市万泉电器有限公司 | Method for preparing activated carbon for capacitor through pine nut shells |
| CN105692610A (en) * | 2016-03-11 | 2016-06-22 | 宁国市万泉电器有限公司 | Preparation method of activated carbon for capacitor |
| CN105819441A (en) * | 2016-03-11 | 2016-08-03 | 宁国市万泉电器有限公司 | Method for preparing active carbon used for capacitors |
| US20170349488A1 (en) * | 2016-06-07 | 2017-12-07 | Council Of Scientific & Industrial Research | Novel Multifunctional Material for Workability of Geopolymeric System and its Process Thereof |
| CN107445163A (en) * | 2017-09-08 | 2017-12-08 | 常州可赛成功塑胶材料有限公司 | A kind of preparation method of bacteriostatic activated carbon |
| CN109292751A (en) * | 2018-11-05 | 2019-02-01 | 福州大学 | A kind of preparation method and application of silicon doping charcoal |
| CN118016885A (en) * | 2024-02-01 | 2024-05-10 | 江西金糠新材料科技有限公司 | Positive electrode active material additive and preparation method and application thereof |
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| CN101804988A (en) * | 2010-05-05 | 2010-08-18 | 吉林大学 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
| CN102229429A (en) * | 2011-03-28 | 2011-11-02 | 蚌埠鑫源石英材料有限公司 | Renewable energy silicon energy storing and circulating system |
| CN102431993A (en) * | 2011-09-22 | 2012-05-02 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor by using rice hulls as raw materials |
| CN103408009A (en) * | 2013-04-27 | 2013-11-27 | 吉林大学 | Preparation method for coproduction of high-specific-capacitance active carbon and nano silicon dioxide from rice hull |
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| CN101804988A (en) * | 2010-05-05 | 2010-08-18 | 吉林大学 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
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| CN102431993A (en) * | 2011-09-22 | 2012-05-02 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor by using rice hulls as raw materials |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668566A (en) * | 2016-03-11 | 2016-06-15 | 宁国市万泉电器有限公司 | Method for preparing activated carbon for capacitor through pine nut shells |
| CN105692610A (en) * | 2016-03-11 | 2016-06-22 | 宁国市万泉电器有限公司 | Preparation method of activated carbon for capacitor |
| CN105819441A (en) * | 2016-03-11 | 2016-08-03 | 宁国市万泉电器有限公司 | Method for preparing active carbon used for capacitors |
| US20170349488A1 (en) * | 2016-06-07 | 2017-12-07 | Council Of Scientific & Industrial Research | Novel Multifunctional Material for Workability of Geopolymeric System and its Process Thereof |
| US10023497B2 (en) * | 2016-06-07 | 2018-07-17 | Council Of Scientific & Industrial Research | Multifunctional material for workability of geopolymeric system and its process thereof |
| CN107445163A (en) * | 2017-09-08 | 2017-12-08 | 常州可赛成功塑胶材料有限公司 | A kind of preparation method of bacteriostatic activated carbon |
| CN109292751A (en) * | 2018-11-05 | 2019-02-01 | 福州大学 | A kind of preparation method and application of silicon doping charcoal |
| CN109292751B (en) * | 2018-11-05 | 2021-09-28 | 福州大学 | Preparation method and application of silicon-doped biochar |
| CN118016885A (en) * | 2024-02-01 | 2024-05-10 | 江西金糠新材料科技有限公司 | Positive electrode active material additive and preparation method and application thereof |
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