CN1824604A - Method of making special active carbon for capacitor using hard fruit shell - Google Patents

Method of making special active carbon for capacitor using hard fruit shell Download PDF

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Publication number
CN1824604A
CN1824604A CN 200510047259 CN200510047259A CN1824604A CN 1824604 A CN1824604 A CN 1824604A CN 200510047259 CN200510047259 CN 200510047259 CN 200510047259 A CN200510047259 A CN 200510047259A CN 1824604 A CN1824604 A CN 1824604A
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shell
accordance
capacitor
water
activation
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CN1318295C (en
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古可隆
李国君
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Chaoyang Senyuan Activated Carbon Co., Ltd.
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古可隆
李国君
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Abstract

The present invention relates to a method for preparing special-purpose active carbon for capacitor by using nutshell. Said method includes the following steps: selecting raw material, breaking nutshell to make its grain size be 3-5 mm; charring for 1-2 hr at 400-500 deg.C; mixing charred material and sodium hydroxide and potassium hydroxide according to the ratio of 1:1.0-2.5:0.4-1.2; activating for 2-3 hr at 700-800 deg.C; cooling activated material in water, water-washing filtrate, adding acid to make neutralization, making pH value of water-washed solution be 6-7 and drying so as to obtain the invented product.

Description

Make the method for capacitor special-purpose activated charcoal of hard fruit shell
Technical field
The present invention relates to a kind of preparation method of high-ratio surface special-purpose activated charcoal, particularly Main classification is that COIB31/08 makes the electrode of super capacitor process of active carbon with hard fruit shell.
Background of invention
Ultracapacitor is that the physical power source that begins to occur in the world the 1980s stores new technology, and the core material of electrode of super capacitor is the high-performance ultracapacitor special-purpose activated charcoal (abbreviation electrode carbon) of high-performance, high-specific surface area, appointment pore size.Electrode carbon the eighties in last century by U.S. AMOCO company exploitation, but can only commercially produce on a small quantity, Japan also begins to commercially produce on a small quantity subsequently, China began one's study from 1993, failed really to realize suitability for industrialized production so far.It is to be raw material with resin and same sex pitch that the U.S., Japan produce electrode carbon, the patent No. is 01123095.9, title " gac and production method thereof, polarizable electrode and double layer capacitor ", this technology is developed by Japan one tame enterprise, is to make the big gac of static capacity by the isotropic pitch of particulate state through thermal treatment and activation; The patent No. is 00118967.0.Title " is made the method for preparation of active carbon of electrode of super capacitor " and is disclosed a kind of gac making method of making electrode of super capacitor by University Of Tianjin, this method is to be raw material with resol, main through coking, charing, activation treatment, make required gac through washing, oven dry again.Aforesaid method particularly is that the electrode carbon of raw material production costs an arm and a leg with the resin, generally at 80～1,600,000 yuan/ton (Renminbi).This also is to be difficult to realize the major cause commercially produced in a large number.Various nucleocapsids such as present hard fruit shell such as apricot, hazel, walnut, jujube nuclear, mostly being used for fuel uses, the part industry is made active carbon in use for decoloring sugar with hard fruit shell, because technical indicators such as the void distribution that such gac can reach, specific surface area are not high, can only be used for sugar decolouring, purifying of drinking water industry, require the field that specific surface area is higher, adsorptive power is strong, void distribution can satisfy special specialty for those, such gac will can not reach far away.
Summary of the invention
The purpose of this invention is to provide a kind of is the method that raw material is made capacitor special-purpose activated charcoal with hard fruit shell, utilizes the gac of this method preparation, and specific surface area is big, and adsorptive power is good, and void distribution is reasonable; Average 10～150,000 yuan/ton (Renminbi) of cost of manufacture, this gac is the most suitable to be applied to the double layer capacitor manufacturing, is the core material of electrode of super capacitor.
In order to achieve the above object, the present invention is achieved through the following technical solutions: be that the employing hard fruit shell is a raw material, handle the method for producing the electrode for capacitors special-purpose activated charcoal through charing, activation, washing, oven dry, its technical characterictic is:
A) raw material was handled 1～2 hour in 400～500 ℃ of charings through screening, particle size after cracking to 3～5mm;
B) carbonized material is mixed by 1: 1.0～2.5: 04.～1.2 weight proportions with sodium hydroxide and potassium hydroxide, in 700～800 ℃ of activation treatment 2～3 hours;
C) will activate material and add in the water and cool off, and leach the material washing and add the acid neutralization, water lotion pH value to 6～7 can obtain finished product after the oven dry.
The present invention can also be achieved through the following technical solutions:
Be suitable for 450～480 ℃ through experiment carbonization temperature of the present invention.Adopt chemical activation technology, at activator KOH, NaOH, ZnCL, CaCL 2In the middle of to select NaOH and KOH for use be the combination activator of present method, the weight proportion of carbonized material and sodium hydroxide and potassium hydroxide for be chosen as 1: 1.5～2.0: 0.6～1.0, activation temperature is chosen as 750～800 ℃, time be 2～3 hours more suitable, when activation temperature continue to raise, soak time is long more, the comprehensive physicochemical property of gac is not to improve, but reduces, charcoal alkali proportioning will influence the formation of gac hole, and the cooled material washing adding hydrochloric acid that leaches neutralizes.Used hard fruit shell is the nucleocapsid of various hard fruits such as almond shell, coconut husk, nut-shell, hazelnut shell, peach-pit shell, jujube nucleocapsid, hawthorn seeds.
Embodiment expresses with tabular form.
Raw material variety 1000g Carbonization temperature ℃ Activation temperature ℃ Add alkali number (g) KOH+NaOH Soak time (hour) Iodine sorption value mg/g Specific surface area M 2/g
Coconut husk 480 780 800+1700 2 1300～1400 2000～2400
The almond shell 450 750 700+1600 2 1300～1500 2200～2500
Peach shell, jujube nuclear 420 700 850+1600 2 1300～1400 2000～2400
Nut-shell 450 750 850+1800 3 1400～1600 2300～2600
The hazel shell 420 720 700+2000 3 1300～1400 2200～2400
The almond shell 480 780 1000+1500 3 1500～1600 2500～2600
With almond shell 1000g fragmentation, granularity is at 3～5mm, charing is 2 hours under 450 ℃ ± 5 temperature, again carbonized material and 90% sodium hydroxide 1780g and 85% potassium hydroxide 825g (industrial goods content 80～90%) are mixed, under 750 ± 5 ℃ of temperature in rotatable activation furnace activation treatment 2 hours, will activate material and put into water rapidly and cool off, leach the material washing and add the hydrochloric acid neutralization, make the water lotion pH value reach 6～7, drying materials is ground to needs particle fineness to get final product.
Product of the present invention and resin method product contrast table
Producing country The U.S., Japan Enterprise of the present invention
Raw material technology Resin method Hard fruit shell carbonization-activation method
Used activator and proportioning Portions of resin KOH=1: 3.5～8 Apricot shell carbonized material: NaOH: KOH=1: 1.0～2.5: 0.4～1.2
The absorption index of void distribution Specific surface area: 2500～3000m 2/ g pore size distribution: 1～3nm iodine sorption value: 1600～2000mg/g Yamamoto Methylene Blue ZF absorption: 20～35ml proportion: 0.3～0.4g/ml Specific surface area: 2000～2600m 2/ g pore size distribution: 0.8～2.2nm iodine sorption value: 1300～1600mg/g Yamamoto Methylene Blue ZF absorption: 20～30ml proportion: 0.4～0.5g/ml
Average price (Renminbi) 80～1,600,000 yuan/ton 10～150,000 yuan/ton
Basic mechanical design feature Discharge time: 2 minutes and 20 seconds Discharge time: 3 minutes and 0 second
With the gac of the present invention preparation, the discharge time that is gone out by last tabular, discharge time was long more, illustrates that the gac void distribution is reasonable more as can be seen; In selected one suitable interval while of activation temperature, combination activator and suitable proportional quantity also are the key factors that improves the comprehensive physical and chemical index of gac.Product of the present invention is a domestic relevant energy enterprise probationary certificate through in recent years, and this product utmost point is applicable to the making of double electric layers supercapacitor electrode, and quality and comprehensive technical indexes are better than present world like product, and product price has competitive power.

Claims (6)

1, make the method for capacitor special-purpose activated charcoal of hard fruit shell, it is to be raw material with the waste hard shell, handles and obtains through charing, activation, washing, oven dry, it is characterized in that:
A) raw material was handled 1～2 hour in 400～500 ℃ of charings through screening, particle size after cracking to 3～5mm;
B) carbonized material is mixed by 1: 1.0～2.5: 04.～1.2 weight proportions with sodium hydroxide and potassium hydroxide, in 700～800 ℃ of activation treatment 2～3 hours;
C) will activate material and add in the water and cool off, and leach the material washing and add the acid neutralization, water lotion pH value to 6～7 can obtain finished product after the oven dry.
2, in accordance with the method for claim 1, it is characterized in that described carbonization temperature is 450～480 ℃.
3, in accordance with the method for claim 1, the weight proportion that it is characterized in that carbonized material and sodium hydroxide and potassium hydroxide is 1: 1.5～2.0: 0.6～1.0.
4, in accordance with the method for claim 1, it is characterized in that described activation temperature is 750～800 ℃.
5, in accordance with the method for claim 1, it is characterized in that neutralizing acid is a hydrochloric acid.
6, in accordance with the method for claim 1, it is characterized in that described hard fruit shell is almond shell, coconut husk, nut-shell, hazelnut shell, peach-pit shell, jujube nucleocapsid, hawthorn seeds.
CNB2005100472592A 2005-09-19 2005-09-19 Method of making special active carbon for capacitor using hard fruit shell Active CN1318295C (en)

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100396608C (en) * 2006-09-15 2008-06-25 江苏工业学院 Method of preparing high specific surface area activated carbon with rich mesoporous
WO2009015533A1 (en) * 2007-07-27 2009-02-05 Chaoyang Shenyuan Active Carbon Co. Ltd. Active carbon for capacitor and a method for preparing the same
CN100463850C (en) * 2006-09-13 2009-02-25 海南大学 Method of preparing low ash high specific surface area active carbon from coconut shell slag
CN101780952A (en) * 2010-03-26 2010-07-21 上海交通大学 Method for preparing loading functional oxide porous carbon
CN102354613A (en) * 2011-09-14 2012-02-15 中国第一汽车股份有限公司 Electrode material of supercapacitor and preparation method for electrode material
CN102874803A (en) * 2011-07-12 2013-01-16 栾清杨 Preparation technology of active carbon for active carbon sheet materials
CN103346025A (en) * 2013-06-26 2013-10-09 西北师范大学 Method for preparing super capacitor electrode materials with laver
CN104843702A (en) * 2015-04-25 2015-08-19 海南大学 Mat grass activated carbon and preparing method thereof
CN105731752A (en) * 2016-04-29 2016-07-06 东北大学 Method for preparing biochar by carrying out copyrolysis on excess sludge and hazelnut shell
CN105923634A (en) * 2016-05-06 2016-09-07 海南大学 Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon
CN105957729A (en) * 2016-05-18 2016-09-21 哈尔滨万鑫石墨谷科技有限公司 Super capacitor flexible electrode, preparation method thereof and super capacitor
CN106006630A (en) * 2016-05-19 2016-10-12 青岛大学 Method for preparing activated carbon materials
CN106145088A (en) * 2016-06-28 2016-11-23 湘潭大学 A kind of biomass porous material with carbon element and its preparation method and application
CN106904611A (en) * 2017-03-20 2017-06-30 陕西师范大学 A kind of preparation method of walnut shell activated carbon
CN109607534A (en) * 2019-01-28 2019-04-12 广西农垦糖业集团昌菱制糖有限公司 A kind of processing technology using bagasse production active carbon
CN111710536A (en) * 2020-05-20 2020-09-25 上海应用技术大学 Vanadium pentoxide/hawthorn fruit-based porous carbon composite material and preparation method and application thereof
CN115504468A (en) * 2022-09-27 2022-12-23 东莞理工学院 Modification method for improving walnut shell based active carbon toluene adsorption breakthrough time

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1511784A (en) * 2002-12-28 2004-07-14 谢仁智 Process for preparing large and medium pore high performance active carbon

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100463850C (en) * 2006-09-13 2009-02-25 海南大学 Method of preparing low ash high specific surface area active carbon from coconut shell slag
CN100396608C (en) * 2006-09-15 2008-06-25 江苏工业学院 Method of preparing high specific surface area activated carbon with rich mesoporous
WO2009015533A1 (en) * 2007-07-27 2009-02-05 Chaoyang Shenyuan Active Carbon Co. Ltd. Active carbon for capacitor and a method for preparing the same
CN101780952A (en) * 2010-03-26 2010-07-21 上海交通大学 Method for preparing loading functional oxide porous carbon
CN102874803A (en) * 2011-07-12 2013-01-16 栾清杨 Preparation technology of active carbon for active carbon sheet materials
CN102354613A (en) * 2011-09-14 2012-02-15 中国第一汽车股份有限公司 Electrode material of supercapacitor and preparation method for electrode material
CN103346025A (en) * 2013-06-26 2013-10-09 西北师范大学 Method for preparing super capacitor electrode materials with laver
CN104843702A (en) * 2015-04-25 2015-08-19 海南大学 Mat grass activated carbon and preparing method thereof
CN105731752A (en) * 2016-04-29 2016-07-06 东北大学 Method for preparing biochar by carrying out copyrolysis on excess sludge and hazelnut shell
CN105731752B (en) * 2016-04-29 2019-04-26 东北大学 A method of charcoal is prepared using excess sludge and hazelnut shell copyrolysis
CN105923634B (en) * 2016-05-06 2019-01-15 海南大学 Supercapacitor coir fibre matrix activated carbon and preparation method thereof
CN105923634A (en) * 2016-05-06 2016-09-07 海南大学 Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon
CN105957729A (en) * 2016-05-18 2016-09-21 哈尔滨万鑫石墨谷科技有限公司 Super capacitor flexible electrode, preparation method thereof and super capacitor
CN106006630A (en) * 2016-05-19 2016-10-12 青岛大学 Method for preparing activated carbon materials
CN106145088B (en) * 2016-06-28 2018-05-25 湘潭大学 A kind of biomass porous carbon material and its preparation method and application
CN106145088A (en) * 2016-06-28 2016-11-23 湘潭大学 A kind of biomass porous material with carbon element and its preparation method and application
CN106904611A (en) * 2017-03-20 2017-06-30 陕西师范大学 A kind of preparation method of walnut shell activated carbon
CN106904611B (en) * 2017-03-20 2018-06-29 陕西师范大学 A kind of preparation method of walnut shell activated carbon
CN109607534A (en) * 2019-01-28 2019-04-12 广西农垦糖业集团昌菱制糖有限公司 A kind of processing technology using bagasse production active carbon
CN111710536A (en) * 2020-05-20 2020-09-25 上海应用技术大学 Vanadium pentoxide/hawthorn fruit-based porous carbon composite material and preparation method and application thereof
CN111710536B (en) * 2020-05-20 2022-02-11 上海应用技术大学 Vanadium pentoxide/hawthorn fruit-based porous carbon composite material and preparation method and application thereof
CN115504468A (en) * 2022-09-27 2022-12-23 东莞理工学院 Modification method for improving walnut shell based active carbon toluene adsorption breakthrough time

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