CN102502621A - Post-treatment process for preparing super-capacitor active carbon with super-low ash content - Google Patents
Post-treatment process for preparing super-capacitor active carbon with super-low ash content Download PDFInfo
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Abstract
The invention relates to a post-treatment process for preparing super-capacitor active carbon with super-low ash content. According to the invention, by combining high-temperature and high-pressure characteristics of a hydrothermal technique, a method including the steps of alkali washing, acid washing and water washing is adopted, so that the content of ash content impurities in the active carbon is greatly reduced and the active carbon becomes a high-performance electrode material which is high in electrical conductivity and strength and is applicable to a super capacitor. A buckle type super capacitor which is manufactured by the active carbon refined by the post-treatment process has the advantages of low resistance, small leakage current and long cycling life.
Description
Technical field
The invention belongs to the processing technology field of high performance active carbon in new forms of energy and the novel material, relate generally to the Impurity removal of super capacitor gac, effectively reduce the method for ash of active carbon content, the quality of raising and stable super capacitor active carbon electrode material.
Background technology
Electrode material for super capacitor mainly contains three types of materials such as gac, MOX and conductive polymers.They respectively have relative merits, and the metal oxide materials capacity is big but cost an arm and a leg, the conductive polymers processing characteristics good and can scale operation but easily by the electrolytic solution swelling and performance descends rapidly.
Active carbon electrode material is because of low, the technical maturity of production cost, and stable performance is the super capacitance electrode material that current each major company generally adopts.The super capacitor absorbent charcoal material is different from general gac, and it has very high index request: high-ratio surface, suitable three grades of pore structures, high tap density, high conductivity, high purity.These six indexs are mutual restriction, and rationally regulating and control these indexs is the keys that obtain heavy body super capacitor gac.High quality super capacitor Preparation of Activated Carbon technology is main at present grasps in American-European and Japanese hand, and domestic have enterprise of a few family to produce out the super capacitor gac as a trial in the foreign imitation technology, but quality still can not be compared with external like product.
The principal element that influences these two indexs of high conductivity and high purity is the content of ash content.The super capacitor gac is more stricter than absorption, catalysis and food pharmaceutical grade gac to the requirement of ash oontent; External high-end super capacitor gac producer ash content control indexes is below 0.1%, and domestic super capacitor gac producer generally is controlled at below 1%.Ash content is generally inorganic oxide (SiO
2, Al
2O
3, CaO, MgO, Fe
2O
3, K
2O, Na
2O), also contain a spot of vitriol, carbonate etc.The existence of these impurity ash contents is fatal to the performance impact of super capacitor gac, it can reduce gac physical strength, increase resistance and be easy to react and cause big leakage current with electrolytic solution.Therefore the removal of ash content is the gordian technique of producing the super capacitor activated carbon, also is the technical bottleneck of the domestic gac enterprise production super capacitor gac of restriction.
The preparation of high quality super capacitor gac is a complicated technology process, need be in material choice, and carbonization-activation prepares process and exquisite control is carried out in three aspects of aftertreatment.Raw material is mainly selected the few material of high (more than the 80%) impurity of carbon content: refinery coke gac, resin base gac and plant base gacs such as coconut husk, almond.The carbonization-activation process control is not the content that the present invention pays close attention to, and the present invention mainly is conceived to the aftertreatment technology of high performance active carbon preparation.Under the prerequisite that raw material and carbonization-activation condition are confirmed, deliming is treated as the principal element that influences quality of activated carbon, and deliming has early stage, mid-term, three kinds of technologies of post-processed.Early stage, deliming was meant that the raw material of producing gac is carried out deliming to be handled.Handle being meant that the work in-process carbonized material is carried out deliming to be handled mid-term, and then activation makes gac.Post-processed promptly is that activated carbon product is carried out deliming, and what generally adopt is the method with the dilute hydrochloric acid solution washing.Handle because the material quantity of handling is bigger early stage, increased cost greatly.Handle the fewer of research mid-term, and post-processed has plurality of advantages, and volume and quality have had very big dwindling after raw material process carbonization and the activation, and such washing composition alkali that consumes can reduce with the amount of acid greatly, has reduced pollution and cost.
Domestic majority gac enterprise all is that the gac after selecting for use hydrochloric acid to activation carries out the pickling deliming; Usually can reduce by 40～80% ash content; Ash of active carbon is reduced to below 8%, but desires to make the charcoal ash content to drop to 4% or more low-level, generally depend merely on pickling and be difficult to prove effective.
Publication number 101723359A, title adopts UW and microwave radiation to combine the method for the dipping washing of hot water, hot acid in " a kind of washing methods of electrode active carbon ", reduced the active carbon electrode material ash impurities.
Publication number 101544369, title is employed in the method that the flocculation agent that adds SEPIGEL 305 or poly aluminium chloride in the rinsing liquid reduces ash of active carbon in " a kind of method of removing ash of active carbon ".
Publication number 101269810, title, " absorbent charcoal fine purification technique " employing thermokalite is washed the technology of washing with hot acid and is reduced the ash content in the gac.
Publication number 1220237; Title is employed in the Reaktionsofen of sealing in " active carbon high-temp chlorination deliming technology ", under high reducing atmosphere; Effect through chlorizating agent and catalyzer; With infiltration or fluidization mode, ash content and chlorizating agent in the gac reacted generate gaseous chloride to discharge out of the furnace, thereby reduced ash content as the sub product recovery.
Document: " research of active carbon from coal microwave heating soda acid deliming ", author Zhang Jun etc. adopt microwave heating alkali acid system to reduce the ash content of gac.
Document: " novel method of gac degree of depth deliming ", author Yang Xia etc. adopt the method for pressurization alkali acid elution to reduce the ash content of gac.
Except normal pressure heating acid wash; Mainly contain three kinds of modes in the method for the reduction ash of active carbon that more than adopts in invention and the document: heating alkali cleaning and acid wash, pressurization alkali acid elution method, high-temperature chlorination method, wherein type of heating can adopt conventional heating, UW and microwave thermal.The conventional acid washing method is the washing methods of the most frequently used gac, it simple to operate to equipment require lowly, washing lotion can totally be used but this method is difficult to be reduced to ash content below 8%.The high pressure base acid system adopts the highly compressed condition to increase running cost, high-temp chlorination deliming method used hypertoxic chlorine and chlorine have corrodibility to the requirement of equipment than higher.These methods are because the defective on the principle can only be reduced to the ash content of gac about 4%; This also has certain gap from index of high-end super capacitor gac 0.1%, makes super capacitor and uses gac so mainly take to control the method for the raw material (polymeric resin matrix, refinery coke base and coconut husk almond base) of gac on producing.High quality resin base and refinery coke matrix activated carbon cost are high, coconut husk and almond yield poorly and collect on a large scale difficult, this big limitations the development of super capacitor charcoal industry.We have invented a kind of method of under the condition of hydro-thermal, carrying out the detergent active charcoal; Used detergent concentration is low, consumption is few; And can be reduced to the ash content of refinery coke base, plant base and resin base gac below 0.1%, be reduced to active carbon from coal below 1%.Though the disposable apparatus cost of investment is big, running cost is low, and super capacitor gac added value is high, is the reasonable a kind of method for preparing extremely low ash content super capacitor gac so compare few this kind method that adopts of demand with conventional gac.
Summary of the invention
The objective of the invention is deficiency, invented a kind of hydro-thermal aftertreatment technology, make the super capacitor gac after the activation carry out degree of depth deliming to existing ash of active carbon treatment technology.
The present invention realizes through following technical scheme:
The aftertreatment technology of the extremely low ash content super capacitor gac of a kind of preparation may further comprise the steps:
In hydrothermal reaction kettle, the super capacitor gac that activation treatment is crossed carries out hydro-thermal reaction through after adding aqueous slkali soaking earlier, and washing is carried out hydro-thermal reaction through adding after acid solution soaks again; Washing, dry getting final product; The temperature of hydro-thermal reaction is 40-250 ℃, is preferably 60-180 ℃, more preferably 120 ℃; Time is 0.1-6 hour, is preferably 0.5-3 hour, more preferably 2 hours.
Also can be with adding hydro-thermal reaction after the aqueous slkali soaking in the above-mentioned technology, and add the procedural order that acid solution soaks the back hydro-thermal reaction and change.
Can also carry out hydro-thermal reaction with the optional one of which of the process that adds acid solution with adding alkaline solution in the above-mentioned technology, remaining add acid or add the alkali process then do not carry out hydro-thermal reaction, just directly immersion.
Alkali in the above-mentioned technology in the alkaline solution is a kind of in Pottasium Hydroxide, sodium hydroxide, bicarbonate of ammonia, sodium hydrogencarbonate and the yellow soda ash or their mixture; Acid in the acid solution is a kind of in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and the hydrofluoric acid or is their mixture; The concentration of alkaline solution is between 0.05mol/L-1mol/L; Be preferably 0.2mol/L-0.5mol/L, 0.3mol/L more preferably, the concentration of acid solution is between 0.1-30wt%; Be preferably 1-10wt%, 5wt% more preferably, the adding quality of acid solution and alkaline solution be quality of activated carbon 2-20 doubly; Be preferably 5-15 doubly, more preferably 8 times.
The mineral based gac (coming from coal, oil) that the super capacitor gac that above-mentioned activation treatment is crossed comprises chemically, physical method or catalytic activation method were handled, plant base gac (coming from timber, shell, fruit stone, straw) or organic polymer resin pyrolysis gac; Particularly the super capacitor gac of present main flow comprises refinery coke matrix activated carbon, coconut husk base or almond matrix activated carbon and synthetic resins matrix activated carbon.The ash oontent of the gac after the activation is between 2%-15%.Gac comprises granulated active carbon or powdered carbon, and the granulated active carbon size is 150-800 μ m, is preferably 200-320 μ m; The powdered carbon size is 1-80 μ m, is preferably 5-15 μ m.
The aqueous slkali soaking time is 3-18 hour in the above-mentioned technology; The acid solution soak time is 2-10 hour.
Modifier modification be can also before hydro-thermal reaction, add in the above-mentioned technology, hydro-thermal reaction, the gac of the capacitive property that strengthened carried out then; Properties-correcting agent contains oxygen or nitrogen acid alkali salt for what can change activated carbon surface functional group, specifically comprises: nitric acid, and potassium permanganate, phosphoric acid hydrogen amine, neutralized verdigris or nickelous nitrate etc., its mass concentration scope is 0.5%-75%.
Inner liner of reaction kettle in the above-mentioned technological process is alkaline-resisting, acid corrosion-resistant and heat-stable tetrafluoroethylene or other macromolecular material, is preferably polytetrafluoroethyllining lining.
Add hydro-thermal reaction after the aqueous slkali soaking, and add process that acid solution soaks the back hydro-thermal reaction and can look impurities composition different and the transposing order of raw material.The mineral substance gac is preferably and adds buck heat earlier, and then adds sour water heat, and plant base and resin base gac are preferably first thermokalite and wash, and then adds sour water heat.
A kind of concrete scheme in the above-mentioned technology is following:
Chemically, physical method or catalytic activation method active carbon processed, handled 3-18 hour with aqueous slkali soaking, change over to then in the hydrothermal reaction kettle 40-250 ℃ of reaction 0.1-6 hour down; Cool to room temperature; Filter, to neutral, sig water concentrates and utilizes with deionized water wash.Then will wash to the neutral gac and soak 2-10 hour, change reaction kettle then over to, 40-250 ℃ of reaction 0.1-6 hour down with acid solution.Be cooled to room temperature, to neutral, diluted acid concentrates and utilizes with deionized water wash, uses 40-80 ℃ deionized water wash 0.5-3 hour then.Centrifugal or suction filtration obtains the gac wet feed, and is dry under 150 ℃, divides grade packaged.The acid-base solution that can not utilize again is mixed to neutral to reduce pollution and processing cost.
Principle of the present invention be activated active carbon processed under hydrothermal condition with alkali and acid solution thorough mixing.Under the HTHP thermal and hydric environment, can reinforcing mass transfer dissolve with promoting; Like this alkali and acid solution can rapid osmotic to the inside of gac; Make under usual conditions, to be difficult to dissociate fast with the ash impurities such as inorganic, metal oxide, vitriol and phosphoric acid salt of alkali and acid-respons and dissolve, thereby reduce the ash content of product significantly.
Technique effect of the present invention is to make the reduction of the very big degree of ash content of super capacitor gac, has enlarged the source of super capacitor gac raw material.Beneficial effect also is to adopt the concentration of hydrothermal treatment consists mode washing composition and consumption under the situation that does not influence washing effect, significantly to reduce, and has reduced the consumption of the bronsted lowry acids and bases bronsted lowry of contaminate environment, and has improved economic benefit.
Through the later gac of present technique scheme aftertreatment, greatly reduce the content of ash contents such as inorganic impurity.Compare with existing method, this kind method can make the ash content of active carbon from coal be reduced to below 1%, and refinery coke base, plant base and resin base gac are reduced to below 0.1%.The inventive method is simple to operate, and running cost is low, and the super capacitor quality of activated carbon of preparation is high, can substitute the conventional alkali cleaning and the method for pickling fully, is used for the aftertreatment technology of super capacitor gac.
Description of drawings
Fig. 1 is the adsorption desorption isothermal map of Comparative Examples 1 and embodiment 1.
Embodiment
Below in conjunction with specific embodiment the present invention is done to further describe, so that help the reader better to understand technical scheme of the present invention, but specific embodiment is not done any qualification to scope of the present invention.
Typical process is following in the technology of the present invention:
Gac after the activation treatment → hydro-thermal alkali cleaning → hydro-thermal pickling → hot water wash → centrifugal or suction filtration → drying → classification → packing.
Embodiment 1
The coconut husk matrix activated carbon 30g of activated processing, use 280ml concentration to soak 6 hours as the potassium hydroxide solution of 0.3mol/L, change the hydrothermal reaction kettle of 1L then over to, 120 ℃ of reactions 2 hours down.Reaction finishes, and filters, with deionized water wash 3 times; The hydrochloric acid soln of putting into the gac wet feed 5wt% soaked 3 hours, changed water heating kettle over to and reacted 1 hour down for 120 ℃, filtered; With deionized water wash 3 times, reaction 1 hour in 60 ℃ of hot water is again filtered; De-ionized washing is to neutral, and 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Comparative Examples 1
The coconut husk matrix activated carbon 30g of activated processing, use 280ml concentration to be heated to 60 ℃ of washing by soaking 6 hours as the potassium hydroxide solution of 0.3mol/L, filter; Deionized water wash is to neutral; Hydrochloric acid soln with 5wt% was heated to 30 ℃ of washing by soaking 3 hours then, filtered, and deionized water wash is to neutral; 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Embodiment 2
The active carbon from coal 30g of activated processing, use 300ml concentration to soak 8 hours as the potassium hydroxide solution of 0.5mol/L, change the hydrothermal reaction kettle of 1L then over to, 150 ℃ of reactions 2 hours down.Reaction finishes, and filters, with deionized water wash 3 times; The hydrochloric acid soln of putting into the gac wet feed 5wt% soaked 6 hours, changed water heating kettle over to and reacted 1 hour down for 150 ℃, filtered; With deionized water wash 3 times, reaction 1 hour in 60 ℃ of hot water again, with deionized water wash to neutral; 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Comparative Examples 2
The active carbon from coal 30g of activated processing, use 300ml concentration to be heated to 60 ℃ of washing by soaking 8 hours as the potassium hydroxide solution of 0.5mol/L, filter; Deionized water wash is to neutral; Hydrochloric acid soln with 5wt% was heated to 30 ℃ of washing by soaking 6 hours then, filtered, and deionized water wash is to neutral; 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Embodiment 3
The transposing of the order of alkali cleaning among the embodiment 1 and pickling, all the other steps are identical, obtain the super capacitor activated carbon product.
Embodiment 4
Be changed to sodium hydroxide to the alkali among the embodiment 1, acid is changed to nitric acid, and all the other conditions are identical, obtains the super capacitor activated carbon product.
Embodiment 5
Soaking later gac with hydrochloric acid soln among the embodiment 1, with 8% potassium permanganate solution immersion 2 hours, all the other conditions were identical again, obtained under hydrothermal condition the super capacitor gac through the potassium permanganate oxidation modification.
Embodiment 6
The coconut husk matrix activated carbon 30g of activated processing, use 280ml concentration to soak 6 hours as the potassium hydroxide solution of 0.3mol/L, change the hydrothermal reaction kettle of 1L then over to, 120 ℃ of reactions 2 hours down.Reaction finishes, and filters, and with deionized water wash 3 times, puts into the gac wet feed 30 ℃ of immersions of hydrochloric acid soln 3 hours of 5wt%; Filter, 60 ℃ of hot water wash 2 hours are filtered; Spend ion-cleaning to neutral, 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Embodiment 7
The resin base gac 20g of activated processing, use 240ml concentration to soak 6 hours as the potassium hydroxide solution of 0.3mol/L, change the hydrothermal reaction kettle of 1L then over to, 100 ℃ of reactions 2 hours down.Reaction finishes, and filters, with deionized water wash 3 times; The hydrochloric acid soln of putting into the gac wet feed 5wt% soaked 3 hours, changed water heating kettle over to and reacted 1 hour down for 100 ℃, filtered; With deionized water wash 3 times, reaction 1 hour in 60 ℃ of hot water is again filtered; De-ionized washing is to neutral, and 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Embodiment 8
The refinery coke matrix activated carbon 20g of activated processing, use 240ml concentration to soak 6 hours as the potassium hydroxide solution of 0.3mol/L, change the hydrothermal reaction kettle of 1L then over to, 100 ℃ of reactions 2 hours down.Reaction finishes, and filters, with deionized water wash 3 times; The hydrochloric acid soln of putting into the gac wet feed 5wt% soaked 3 hours, changed water heating kettle over to and reacted 1 hour down for 100 ℃, filtered; With deionized water wash 3 times, reaction 1 hour in 60 ℃ of hot water is again filtered; De-ionized washing is to neutral, and 150 ℃ of dryings 2 hours obtain the super capacitor activated carbon product.
Each embodiment of table 1 and Comparative Examples detected result
Measure result's (seeing table 1) of ash content from washing the back, adopt the hydro-thermal alkali cleaning method of hydro-thermal pickling then, the ash oontent of gac is minimum, and the ash oontent result that the change washing sequence obtains is more or less the same.Of different types according to different material gac impurities, we can change washing sequence, make the deliming effect reach best.Simultaneously we see that first hydro-thermal alkali cleaning heats pickling then and also can reach hydro-thermal alkali cleaning and hydro-thermal pickling result much at one, heat pickling then considering that the preferably water thermokalite is washed under the condition of production cost.Fig. 1 is the adsorption desorption thermo-isopleth of Comparative Examples 1 and embodiment 1, can find out that the method specific surface area and the adsorptive capacity that adopt hydro-thermal to wash are bigger.
Claims (10)
1. an aftertreatment technology for preparing extremely low ash content super capacitor gac is characterized in that, may further comprise the steps:
In hydrothermal reaction kettle, the super capacitor gac that activation treatment is crossed carries out hydro-thermal reaction through after adding aqueous slkali soaking earlier, and washing is carried out hydro-thermal reaction through adding after acid solution soaks again; Washing, dry getting final product; The temperature of hydro-thermal reaction is 40-250 ℃, and the time is 0.1-6 hour.
2. treatment process according to claim 1 is characterized in that, will add hydro-thermal reaction after the aqueous slkali soaking, and adds the procedural order that acid solution soaks the back hydro-thermal reaction and changes.
3. treatment process according to claim 1 and 2 is characterized in that, adds alkaline solution and carries out hydro-thermal reaction with the optional one of which of the process that adds acid solution.
4. treatment process according to claim 3 is characterized in that, the alkali in the alkaline solution is a kind of in Pottasium Hydroxide, sodium hydroxide, bicarbonate of ammonia, sodium hydrogencarbonate and the yellow soda ash or their mixture; Acid in the acid solution is a kind of in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and the hydrofluoric acid or is their mixture,
5. treatment process according to claim 4 is characterized in that, the concentration of alkaline solution is between 0.05mol/L-1mol/L, and the concentration of acid solution is between 0.1-30wt%; The adding quality of acid solution and alkaline solution is 2-20 a times of quality of activated carbon.
6. treatment process according to claim 1; It is characterized in that; The mineral based gac that the super capacitor gac that described activation treatment is crossed comprises chemically, physical method or catalytic activation method were handled, plant base gac or organic polymer resin pyrolysis gac; The ash oontent of the gac after the activation is between 2%-15%.
7. according to claim 1 or 6 described treatment process, it is characterized in that gac comprises granulated active carbon or powdered carbon, the granulated active carbon size is 150-800 μ m, and the powdered carbon size is 1-80 μ m.
8. treatment process according to claim 5 is characterized in that concrete steps are following:
The aqueous slkali soaking time is 3-18 hour; The acid solution soak time is 2-10 hour.
9. treatment process according to claim 1 is characterized in that, before hydro-thermal reaction, adds modifier modification, carries out hydro-thermal reaction, the gac of the capacitive property that strengthened then; Described properties-correcting agent contains oxygen or nitrogen acid alkali salt for what can change activated carbon surface functional group.
10. treatment process according to claim 9 is characterized in that, described properties-correcting agent comprises: nitric acid, and potassium permanganate, phosphoric acid hydrogen amine, neutralized verdigris or nickelous nitrate, its mass concentration scope is 0.5%-75%.
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| CN103723724A (en) * | 2013-12-08 | 2014-04-16 | 夏榆凌 | Method for manufacturing high activation grade activated carbon by using crop-residue-derived carbon |
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| CN106587058A (en) * | 2016-12-21 | 2017-04-26 | 南京林业大学 | Method for recovering KOH and refining activated carbon in process of preparing super activated carbon with KOH activation method |
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| CN103723724A (en) * | 2013-12-08 | 2014-04-16 | 夏榆凌 | Method for manufacturing high activation grade activated carbon by using crop-residue-derived carbon |
| CN109071237A (en) * | 2016-01-08 | 2018-12-21 | 瓦普公司 | Low ash divides the production method of active carbon |
| CN105923633A (en) * | 2016-04-22 | 2016-09-07 | 东北电力大学 | Method for reducing ash content in process of preparing activated carbon by using straws |
| CN106587058A (en) * | 2016-12-21 | 2017-04-26 | 南京林业大学 | Method for recovering KOH and refining activated carbon in process of preparing super activated carbon with KOH activation method |
| CN106587058B (en) * | 2016-12-21 | 2019-08-09 | 南京林业大学 | A kind of KOH activation method prepares the recycling of the KOH in super-activated carbon technique and absorbent charcoal fine purification method |
| CN106946253B (en) * | 2017-03-09 | 2018-12-21 | 中国科学院山西煤炭化学研究所 | One kind being based on HNO3The preparation method of the high-specific-capacitance active carbon of hydrothermal oxidization modification |
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| CN115557497A (en) * | 2022-09-07 | 2023-01-03 | 中国科学院上海高等研究院 | High-quality activated carbon and preparation method thereof |
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