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CN100402422C - Method capable of reducing energy consumption of reaction for preparing super active carbon - Google Patents

Method capable of reducing energy consumption of reaction for preparing super active carbon Download PDF

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Publication number
CN100402422C
CN100402422C CNB2006100861491A CN200610086149A CN100402422C CN 100402422 C CN100402422 C CN 100402422C CN B2006100861491 A CNB2006100861491 A CN B2006100861491A CN 200610086149 A CN200610086149 A CN 200610086149A CN 100402422 C CN100402422 C CN 100402422C
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China
Prior art keywords
reaction
temperature
energy consumption
vacuum pump
reactor
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Expired - Fee Related
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CNB2006100861491A
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Chinese (zh)
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CN1915808A (en
Inventor
李永昕
薛冰
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Jiangsu University
Jiangsu Polytechnic University
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Jiangsu Polytechnic University
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Abstract

This invention discloses a method for preparing activated carbon with reduced energy consumption. The method comprises: (1) placing a mixture of carbon-containing precursor and KOH or NaOH at a weight ratio of 1 : (3-7) in a vacuum reactor, sealing, and evacuating with a vacuum pump to a pressure of -(0.03-0.09) Mpa; (2) heating from room temperature to 650-750 deg.C, reacting for 0.5-1 h, and cooling naturally to room temperature; (3) shutting the vacuum pump, taking out the product, washing with water and drying to obtain activated carbon. The adoption of the underpressure reaction condition can lower the reaction temperature and shorten the reaction time. Since the method does not adopt protective atmosphere, the volatile components of the precursor can rapidly and completely volatilize from the surface even the inner of the precursor, thus forming activated carbon with larger specific surface area. The method has such advantages as low reaction temperature, short reaction time, no protective atmosphere and large specific surface area of the obtained activated carbon.

Description

A kind of method that can reduce energy consumption of reaction for preparing super active carbon
Technical field
The present invention relates to a kind of preparation process of active carbon, provide a kind of method that can reduce energy consumption of reaction for preparing super active carbon specifically.
Background technology
General to adopt chemical activation method be that activator prepares super-activated carbon with KOH, but in this reaction process, contains the effusion of will volatilizing of light constituent in the carbon precursor, and these fugitive constituents mainly are that some boiling points are at the tarry cut below 500 ℃, water vapour, CO, CO 2, CH 4And H 2Deng.If they can be discharged from reaction system fast, then will certainly shorten the reaction times and reduce temperature of reaction, thereby reduce energy consumption of reaction, but up to the present, lot of domestic and foreign document etc. all is to carry out activation treatment to containing carbon precursor under the high temperature more than 800 ℃, with rare gas element such as N 2With Ar gas etc. as protective atmosphere, under nearly normal pressure, reacting, cause the above-mentioned fugitive constituent of mentioning to be difficult for overflowing smoothly, Fan Ying balance also is unfavorable for moving to the direction of generation product like this, has caused the increase of energy consumption of reaction.If in operating process, adopt the method for decompression to disequilibrate, molecular balance is moved to the product direction, also avoid using simultaneously rare gas element as protection gas, so just can reduce reaction cost, but this method also there is not bibliographical information at present.
Summary of the invention
Purpose of the present invention just provides a kind of preparation method that can reduce energy consumption of reaction with the super-activated carbon of reduction reaction cost; be exactly to adopt the method for decompression to disequilibrate specifically; molecular balance is moved to the product direction; simultaneously also avoid using rare gas element as protection gas, to reduce reaction cost.
Principle of the present invention is as follows: the volatile gases that produces in the reaction process can be discharged from reactive system by the method for decompression vacuum pumping, impels the balance of reaction to move to the product direction like this.Simultaneously, owing to be to react under negative pressure, the boiling point of fugitive constituent gas can reduce greatly, and the temperature that is used to like this react also can reduce, and protective atmosphere also can be avoided in addition, thereby can reduce the cost of reaction.
The present invention realizes as follows:
It is that 1: 3~1: 7 mixture is put in the vacuum reactor by mass ratio that reaction mass is promptly contained carbon precursor and KOH or NaOH, sealing back open vacuum pump bleed up to pressure for-0.03MPa~-0.09MPa, be elevated to 650~750 ℃ temperature of reaction afterwards gradually from room temperature, and under this temperature, stopped 0.5~1 hour, naturally cooling, treat to close vacuum pump when temperature drops to nearly room temperature, take out material and carry out washing and drying, obtain target product.
Wherein the reaction mass presoma comprises refinery coke, pitch coke, coconut husk carbide, farm crop carbide or hard coal.
The invention has the advantages that: owing to adopt decompression method; temperature of reaction can suitably reduce; reaction times also can shorten; unprotect atmosphere; biggest advantage just is that fugitive constituent is fast neatly from containing carbon precursor surface even inner the effusion; produce more active channel, can obtain the higher gac of specific surface area.
Embodiment
Embodiment 1 is enclosed within the reactor after refinery coke and KOH are mixed by 1: 4 mass ratio, open vacuum pump, pressure in the reactor is evacuated to-0.09MPa by normal pressure, begins to be raised to 500 ℃ this moment and stopped 1 hour, continue to be warmed up to 750 ℃ of reactions 0.5 hour afterwards again from envrionment temperature.Naturally after the cooling, close vacuum pump, take out material, surveying its specific surface area behind washing and drying is 3010m 2/ g.
Comparative Examples 1 is put in the normal pressure reactor after refinery coke and KOH are mixed by 1: 4 mass ratio, is raised to 500 ℃ from envrionment temperature with the temperature rise rate of 5 ℃/min then and stops 1 hour, continues to be warmed up to 750 ℃ of reactions 0.5 hour afterwards again.Naturally after the cooling, take out material, surveying its specific surface area behind washing and drying is 2310m 2/ g.
Embodiment 2 is enclosed within the reactor after pitch coke and KOH are mixed by 1: 7 mass ratio, open vacuum pump, pressure in the reactor is evacuated to-0.03MPa by normal pressure, begins to be raised to 500 ℃ this moment and stopped 1 hour, continue to be warmed up to 650 ℃ of reactions 1 hour afterwards again from envrionment temperature.Naturally after the cooling, close vacuum pump, take out material, surveying its specific surface area behind washing and drying is 3380m 2/ g.
Comparative Examples 2 is put in the normal pressure reactor after pitch coke and KOH are mixed by 1: 7 mass ratio, is raised to 500 ℃ from envrionment temperature then and stops 1 hour, continues to be warmed up to 650 ℃ of reactions 1 hour afterwards again.Naturally after the cooling, take out material, surveying its specific surface area behind washing and drying is 2610m 2/ g.
Embodiment 3 is enclosed within the reactor after coconut husk carbide and KOH are mixed by 1: 3 mass ratio, open vacuum pump, pressure in the reactor is evacuated to-0.09MPa by normal pressure, begins to be raised to 500 ℃ this moment and stopped 1 hour, continue to be warmed up to 700 ℃ of reactions 0.5 hour afterwards again from envrionment temperature.Naturally after the cooling, close vacuum pump, take out material, surveying its specific surface area behind washing and drying is 2830m 2/ g.
Comparative Examples 3 is put in the normal pressure reactor after coconut husk carbide and KOH are mixed by 1: 3 mass ratio, is raised to 500 ℃ from envrionment temperature then and stops 1 hour, continues to be warmed up to 700 ℃ of reactions 0.5 hour afterwards again.Naturally after the cooling, take out material, surveying its specific surface area behind washing and drying is 2120m 2/ g.
Embodiment 4 is enclosed within the reactor after farm crop carbide and NaOH are mixed by 1: 6 mass ratio, open vacuum pump, pressure in the reactor is evacuated to-0.05MPa by normal pressure, begins to be raised to 500 ℃ this moment and stopped 1 hour, continue to be warmed up to 750 ℃ of reactions 1 hour afterwards again from envrionment temperature.Naturally after the cooling, close vacuum pump, take out material, surveying its specific surface area behind washing and drying is 2430m 2/ g.
Comparative Examples 4 is put in the normal pressure reactor after farm crop carbide and NaOH are mixed by 1: 6 mass ratio, is raised to 500 ℃ from envrionment temperature then and stops 1 hour, continues to be warmed up to 750 ℃ of reactions 1 hour afterwards again.Naturally after the cooling, take out material, surveying its specific surface area behind washing and drying is 1820m 2/ g.
Embodiment 5 is enclosed within the reactor after hard coal and NaOH are mixed by 1: 4 mass ratio, open vacuum pump, pressure in the reactor is evacuated to-0.06MPa by normal pressure, begins to be raised to 500 ℃ this moment and stopped 1 hour, continue to be warmed up to 700 ℃ of reactions 1 hour afterwards again from envrionment temperature.Naturally after the cooling, close vacuum pump, take out material, surveying its specific surface area behind washing and drying is 2240m 2/ g.
Comparative Examples 5 is put in the normal pressure reactor after hard coal and NaOH are mixed by 1: 4 mass ratio, is raised to 500 ℃ from envrionment temperature then and stops 1 hour, continues to be warmed up to 700 ℃ of reactions 1 hour afterwards again.Naturally after the cooling, take out material, surveying its specific surface area behind washing and drying is 1960m 2/ g.

Claims (2)

1. method that can reduce energy consumption of reaction for preparing super active carbon, its feature comprises the steps:
(1) be that the mixture that 1: 3~1: 7 reaction mass promptly contains carbon precursor and KOH or NaOH is put into vacuum reactor with mass ratio, the sealing back open vacuum pump bleed up to pressure for-0.03MPa~-0.09MPa;
(2) subsequently temperature of reactor is elevated to 500 ℃ gradually from room temperature, and under this temperature, stopped 1 hour; Continue elevated temperature to 650~750 ℃ afterwards, and under this temperature, reacted 0.5~1 hour;
(3) cooling is naturally subsequently treated to close vacuum pump when temperature drops to nearly room temperature, takes out material and carries out washing and drying, obtains target product.
2. a kind of method that can reduce energy consumption of reaction for preparing super active carbon as claimed in claim 1 is characterized by reaction mass and contains carbon precursor and comprise refinery coke, pitch coke, coconut husk carbide, farm crop carbide or hard coal.
CNB2006100861491A 2006-09-04 2006-09-04 Method capable of reducing energy consumption of reaction for preparing super active carbon Expired - Fee Related CN100402422C (en)

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CN100402422C true CN100402422C (en) 2008-07-16

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* Cited by examiner, † Cited by third party
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CN102733291B (en) * 2011-12-23 2014-12-31 上海浦东路桥建设股份有限公司 Regeneration method of asphalt mixture modifier for absorbing automobile exhaust

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1382625A (en) * 2002-06-09 2002-12-04 陈文照 Process for preparing activated carbon from bamboo
JP2003040611A (en) * 2002-06-20 2003-02-13 Osaka Gas Co Ltd Method for producing activated carbon
JP2003073111A (en) * 2002-06-20 2003-03-12 Osaka Gas Co Ltd Method for producing activated carbon
CN1406866A (en) * 2001-09-06 2003-04-02 张惠欣 Method for producing activaled carbon with high specific surface from refinery coke
US20030179537A1 (en) * 2001-09-11 2003-09-25 Masako Tanaka Activated carbon, method for production thereof and use thereof
CN1792785A (en) * 2005-12-29 2006-06-28 上海交通大学 Process for preparing forming active carbod by biomess derived carbonaceous medium phase

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1406866A (en) * 2001-09-06 2003-04-02 张惠欣 Method for producing activaled carbon with high specific surface from refinery coke
US20030179537A1 (en) * 2001-09-11 2003-09-25 Masako Tanaka Activated carbon, method for production thereof and use thereof
CN1382625A (en) * 2002-06-09 2002-12-04 陈文照 Process for preparing activated carbon from bamboo
JP2003040611A (en) * 2002-06-20 2003-02-13 Osaka Gas Co Ltd Method for producing activated carbon
JP2003073111A (en) * 2002-06-20 2003-03-12 Osaka Gas Co Ltd Method for producing activated carbon
CN1792785A (en) * 2005-12-29 2006-06-28 上海交通大学 Process for preparing forming active carbod by biomess derived carbonaceous medium phase

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Assignee: Changzhou Ke Feng Chemical Co., Ltd.

Assignor: Jiangsu Polytechnic University

Contract fulfillment period: 2008.7.8 to 2014.7.7 contract change

Contract record no.: 2009320000228

Denomination of invention: Method capable of reducing energy consumption of reaction for preparing super active carbon

Granted publication date: 20080716

License type: Exclusive license

Record date: 2009.3.5

LIC Patent licence contract for exploitation submitted for record

Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.7.8 TO 2014.7.7; CHANGE OF CONTRACT

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Granted publication date: 20080716

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