CN1970444A - Microwave radiation method for preparing activated carbon with high specific surface area - Google Patents
Microwave radiation method for preparing activated carbon with high specific surface area Download PDFInfo
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- CN1970444A CN1970444A CN 200610136816 CN200610136816A CN1970444A CN 1970444 A CN1970444 A CN 1970444A CN 200610136816 CN200610136816 CN 200610136816 CN 200610136816 A CN200610136816 A CN 200610136816A CN 1970444 A CN1970444 A CN 1970444A
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Abstract
The invention discloses a making method of high specific surface area activated charcoal irradiated by microwave, which comprises the following steps: selecting carbon-rich raw material with high carbon content; grinding into 100-300 order; adding activator with quality as 1-5 times as carbon-rich raw material; stirring evenly; placing in the microwave oven to irradiate; reacting raw material and activator through heating between 700 and 1000 deg.c; insulating 3-60min; fetching the product; washing; filtering; drying to obtain the product.
Description
Technical field:
The invention belongs to gac manufacturing and microwave chemical field, relate to a kind of preparation method of active carbon, particularly relate to a kind of preparation method of active carbon with high specific surface area.
Technical background:
Gac is widely used at aspects such as water treatment, purifying air, pharmacy, food-processings, and active carbon with high specific surface area also can be used for aspects such as ultracapacitor, precious metal recovery except above-mentioned application.
U.S. Pat 4082694 and Japanese Patent JP2004/013575 have announced with the refinery coke to be raw material, are the method that activator prepares active carbon with high specific surface area with KOH; It is raw material that Chinese patent 96123525.x has announced with pitch, is the method that activator prepares active carbon with high specific surface area with KOH; Chinese patent 01126708.9 and 200610017471.9 has been announced the method for preparing active carbon with high specific surface area with KOH living fossil oil coke.The method that more than prepares active carbon with high specific surface area often adopts traditional type of heating to carry out, and its reaction process time is long, activator level is big, production cost is high, energy consumption is big.
Carry out Activated Carbon Production with traditional heating mode, energy consumption height, seriously polluted, many countries have limited this method of application.Chinese patent 931146937.2 has been announced a kind of method of microwave radiation manufacturing powdered carbon, it is with wood chip and phosphoric acid or liquor zinci chloridi dipping, make gac with microwave radiation again, but this method is raw material with the wood chip, and the wood chip source is wideless, need to consume the forest reserves, this has limited the application of this method.Chinese patent 02113270.4 has been announced a kind of method of microwave radiation tobacco rod solid waste manufacturing powdered carbon, this method is pulverized the back with the tobacco rod solid waste and is carried out carrying out carry out microwave radiation heating behind the hybrid infusion with solder(ing)acid, after pickling, oven dry, obtain gac, the material cost of this method is low, but needs the long-time dipping through 4-18 hour.Chinese patent 200510010670.2 and 200510010672.1 is a raw material with the tobacco rod waste, floods through potassium hydroxide or with phosphoric acid solution respectively, is obtaining active carbon with high specific surface area through microwave radiation, but is also needing through steeping process, and the production process time is long.Chinese patent 200510010965.X is a raw material with coconut husk or nut-shell, is activator with KOH, makes active carbon with high specific surface area by microwave radiation, but this method needs charing and two processes of activation, and technology is complicated.Chinese patent 2004100220085.X has announced a kind of with brown coal slag production process of active carbon, with the brown coal slag is raw material, with KOH is that activator prepares gac, this is a kind of way that turns waste into wealth, but, brown coal slag carbon content is lower, the invalid components effect in a large amount of expensive KOH activators and the brown coal slag, the gac yield is lower, and is difficult to produce high performance active carbon.
Summary of the invention:
The purpose of this invention is to provide a kind of energy-efficient, low-cost method for preparing active carbon with high specific surface area.
Particular content of the present invention is:
Choose the high carbon-rich materials of carbon content, levigate back stirs with the certain proportion activator, put into microwave oven again and carry out irradiation, make it heating, burning and play electric arc, wash and reclaim activator then, to wash product pickling, washing, filtration, oven dry again, promptly get active carbon with high specific surface area.Described carbon-rich materials is refinery coke, pitch or their mixture; Described activator is one or more mixtures formed in sodium hydroxide, potassium hydroxide, salt of wormwood, Repone K, the Potassium peroxide; The mass ratio of described activator and carbon-rich materials is 1～5: 1; Described microwave exposure makes the temperature of charge of being made up of carbon-rich materials and activator reach 700 ℃～1000 ℃, and is incubated 5～50 minutes under this temperature.
The beneficial effect that the present invention obtains is that (1) prepares in the process of active carbon with high specific surface area at the microwave exposure carbon-rich materials, it mainly is the heating that causes carbon-rich materials and activator by microwave, and make it to react, generating active carbon with high specific surface area, preparation cycle is short, energy consumption is low; (2) cheap, the wide material sources of the carbon-rich materials that adopts, ash oontent is low, easily makes high performance active carbon with high specific surface area; (3) present method facility investment few, simple to operate, be easy to accomplish scale production; (4) activator level is few, and the carbon-rich materials scaling loss is few, changes the yield height of active carbon with high specific surface area into, and is few pollution-free to environment.
Embodiment
Embodiment 1:
Refinery coke is ground to form 200 purpose fine powders, be to mix at 1: 3 petroleum coke powder and potassium hydroxide by mass ratio then, the mill mill is even with stirring, put into the microwave oven that power is 2KW, in nitrogen atmosphere, be heated to 800 ℃, and after being incubated 10 minutes under this temperature, take out reaction product, use washed with de-ionized water.Add massfraction in the solids after the washing and be 10% hydrochloric acid soln and carry out pickling, use washed with de-ionized water again, filter, can to obtain specific surface area be 3000m in oven dry
2The active carbon with high specific surface area that/g is above.
Embodiment 2:
Pitch is ground to form 150 purpose fine powders, be to mix at 1: 4 asphalt powder and potassium hydroxide by mass ratio then, the mill mill is even with stirring, put into the microwave oven that power is 8KW, in nitrogen atmosphere, be heated to 750 ℃, and after being incubated 25 minutes under this temperature, take out reaction product, use washed with de-ionized water.Add massfraction in the solids after the washing and be 15% hydrochloric acid soln and carry out pickling, use washed with de-ionized water again, filter, can to obtain specific surface area be 2500m in oven dry
2The active carbon with high specific surface area that/g is above.
Claims (6)
1, a kind of microwave exposure prepares the method for active carbon with high specific surface area, it is characterized in that comprising being prepared as follows step: choose the high carbon-rich materials of carbon content, the pulverizing back adds a certain amount of activator and stirs; Put into microwave oven then and carry out irradiation, make raw material and activator the heating and react; Again reaction product is washed, filters, dried, can obtain active carbon with high specific surface area.
2, microwave exposure according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: described carbon-rich materials is refinery coke, pitch or their mixture, and being crushed to granularity is 100～300 orders.
3, microwave exposure according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: described activator is one or more mixtures formed in sodium hydroxide, potassium hydroxide, salt of wormwood, Repone K, the Potassium peroxide.
4, microwave exposure according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: the mass ratio of activator and carbon-rich materials is 1～5: 1.
5, microwave exposure according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: carbon-rich materials and activator are heated and make it reaction by microwave exposure.
6, the method for preparing active carbon with high specific surface area according to claim 1 or the described microwave exposure of claim 5, it is characterized in that: microwave exposure makes the temperature of charge of being made up of carbon-rich materials and activator reach 700 ℃～1000 ℃, and is incubated 3～60 minutes under this temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610136816 CN1970444A (en) | 2006-12-07 | 2006-12-07 | Microwave radiation method for preparing activated carbon with high specific surface area |
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| CN 200610136816 CN1970444A (en) | 2006-12-07 | 2006-12-07 | Microwave radiation method for preparing activated carbon with high specific surface area |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844765A (en) * | 2010-06-02 | 2010-09-29 | 天津大学 | Active carbon for preparing carbon electrode of super capacitor and preparation method thereof |
| CN102417179A (en) * | 2011-09-02 | 2012-04-18 | 安徽工业大学 | Preparation method of activated carbon material for electrochemical capacitor |
| CN102424383A (en) * | 2011-09-23 | 2012-04-25 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor |
| CN103409853A (en) * | 2013-08-22 | 2013-11-27 | 吉林大学 | Method for preparing active carbon fiber material with energy storage characteristic from polyacrylonitrile-based pre-oxidized fiber and application of active carbon fiber material |
| CN103818903A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon from coconut shells, shaddock peels and flax stalks |
| CN103818904A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon by using pinecones, rice hulls and corn stalks |
| CN103818905A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon by using hemp stalks, walnut shells and phoenix tree leaves |
| CN104828821A (en) * | 2013-07-25 | 2015-08-12 | 程俊校 | Activated carbon and preparation process thereof |
| CN106957669A (en) * | 2017-04-12 | 2017-07-18 | 中民驰远实业有限公司 | A kind of asphalt carbonization method |
| CN106986340A (en) * | 2017-04-20 | 2017-07-28 | 神华集团有限责任公司 | Super-activated carbon, and preparation method thereof |
| CN108905925A (en) * | 2018-08-23 | 2018-11-30 | 山东成达新能源科技有限公司 | Reactor and the method for preparing super-activated carbon using the reactor |
| CN109205618A (en) * | 2018-11-27 | 2019-01-15 | 佛山市光烨环保科技有限公司 | A method of super capacitor active carbon is prepared using acid-sludge pitch |
| CN109908907A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | Synthesizing gas by reforming methane with co 2 catalyst and its preparation method |
| CN109908930A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of fischer-tropsch synthetic catalyst and preparation method thereof |
| CN109908898A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of fischer-tropsch synthetic catalyst and its preparation method |
| CN111375435A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Heteropolyacid catalyst and preparation method thereof |
| CN111375434A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Supported heteropoly acid catalyst and preparation method thereof |
| CN113120902A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Preparation method of activated carbon |
| CN114709405A (en) * | 2022-04-27 | 2022-07-05 | 深圳市寒暑科技新能源有限公司 | Preparation method of biomass-based hard carbon composite material |
-
2006
- 2006-12-07 CN CN 200610136816 patent/CN1970444A/en active Pending
Cited By (30)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844765B (en) * | 2010-06-02 | 2012-01-11 | 天津大学 | Active carbon for preparing carbon electrode of super capacitor and preparation method thereof |
| CN101844765A (en) * | 2010-06-02 | 2010-09-29 | 天津大学 | Active carbon for preparing carbon electrode of super capacitor and preparation method thereof |
| CN102417179A (en) * | 2011-09-02 | 2012-04-18 | 安徽工业大学 | Preparation method of activated carbon material for electrochemical capacitor |
| CN102417179B (en) * | 2011-09-02 | 2013-10-09 | 安徽工业大学 | Preparation method of activated carbon material for electrochemical capacitor |
| CN102424383A (en) * | 2011-09-23 | 2012-04-25 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor |
| CN102424383B (en) * | 2011-09-23 | 2013-10-09 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor |
| CN104828821A (en) * | 2013-07-25 | 2015-08-12 | 程俊校 | Activated carbon and preparation process thereof |
| CN104828821B (en) * | 2013-07-25 | 2017-11-14 | 浙江旺林生物科技有限公司 | A kind of activated carbon and its preparation technology |
| CN103409853A (en) * | 2013-08-22 | 2013-11-27 | 吉林大学 | Method for preparing active carbon fiber material with energy storage characteristic from polyacrylonitrile-based pre-oxidized fiber and application of active carbon fiber material |
| CN103818905A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon by using hemp stalks, walnut shells and phoenix tree leaves |
| CN103818904A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon by using pinecones, rice hulls and corn stalks |
| CN103818903B (en) * | 2013-10-21 | 2015-09-23 | 溧阳市浙大产学研服务中心有限公司 | The method of gac prepared by a kind of Exocarpium cocois (Cocos nucifera L), pomelo peel, waste of flax |
| CN103818904B (en) * | 2013-10-21 | 2015-09-23 | 溧阳市浙大产学研服务中心有限公司 | A kind of pinecone, rice husk, corn stalk prepare the method for gac |
| CN103818903A (en) * | 2013-10-21 | 2014-05-28 | 溧阳市浙大产学研服务中心有限公司 | Method for preparing activated carbon from coconut shells, shaddock peels and flax stalks |
| CN106957669A (en) * | 2017-04-12 | 2017-07-18 | 中民驰远实业有限公司 | A kind of asphalt carbonization method |
| CN106986340A (en) * | 2017-04-20 | 2017-07-28 | 神华集团有限责任公司 | Super-activated carbon, and preparation method thereof |
| CN109908930B (en) * | 2017-12-13 | 2021-10-08 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis catalyst and preparation method thereof |
| CN109908898B (en) * | 2017-12-13 | 2021-10-08 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis catalyst and preparation method thereof |
| CN109908907A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | Synthesizing gas by reforming methane with co 2 catalyst and its preparation method |
| CN109908930A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of fischer-tropsch synthetic catalyst and preparation method thereof |
| CN109908898A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of fischer-tropsch synthetic catalyst and its preparation method |
| CN109908907B (en) * | 2017-12-13 | 2022-02-08 | 中国石油化工股份有限公司 | Catalyst for reforming methane and carbon dioxide to produce synthetic gas and its preparing process |
| CN108905925A (en) * | 2018-08-23 | 2018-11-30 | 山东成达新能源科技有限公司 | Reactor and the method for preparing super-activated carbon using the reactor |
| CN109205618A (en) * | 2018-11-27 | 2019-01-15 | 佛山市光烨环保科技有限公司 | A method of super capacitor active carbon is prepared using acid-sludge pitch |
| CN111375434A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Supported heteropoly acid catalyst and preparation method thereof |
| CN111375435A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Heteropolyacid catalyst and preparation method thereof |
| CN111375434B (en) * | 2018-12-29 | 2022-07-12 | 中国石油化工股份有限公司 | Supported heteropoly acid catalyst and preparation method thereof |
| CN111375435B (en) * | 2018-12-29 | 2023-04-07 | 中国石油化工股份有限公司 | Heteropolyacid catalyst and preparation method thereof |
| CN113120902A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Preparation method of activated carbon |
| CN114709405A (en) * | 2022-04-27 | 2022-07-05 | 深圳市寒暑科技新能源有限公司 | Preparation method of biomass-based hard carbon composite material |
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