CN102689901A - Method for fast drying high specific surface area activated carbon - Google Patents
Method for fast drying high specific surface area activated carbon Download PDFInfo
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- CN102689901A CN102689901A CN2012101608091A CN201210160809A CN102689901A CN 102689901 A CN102689901 A CN 102689901A CN 2012101608091 A CN2012101608091 A CN 2012101608091A CN 201210160809 A CN201210160809 A CN 201210160809A CN 102689901 A CN102689901 A CN 102689901A
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- specific surface
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Abstract
The invention discloses a method for fast drying high specific surface area activated carbon. The method comprises the steps of: uniformly mixing a carbon precursor with KOH (potassium hydroxide) or NaOH (sodium hydroxide) by the mass ratio of 1 to 3-8, activating the mixture for 0.5-2 hours under N2 (nitrogen) atmosphere at 800-950 DEG C, naturally cooling the mixture to the room temperature, washing the obtained crude product to neutral by deionized water, obtaining a water activated material after centrifugally separating or extruding and filtering, and dipping for 0.5-2 hours at 30-50 DEG C by the volume ratio of the water activated material to organic solvent being 1 to 0.5-3, obtaining the activated material containing a solvent by centrifugally separating or extruding and filtering, and drying the activated material containing the solvent to obtain the product. The method disclosed by the invention has the advantages of simple operation, easiness in control and feasibility in large-scale production.
Description
Technical field
The invention belongs to a kind of preparation process of active carbon, relate to a kind of method of rapid drying active carbon with high specific surface area specifically.
Background technology
The preparation patent of active carbon with high specific surface area is a lot; But the overwhelming majority only simply replaces " drying " to the dry link in its preparation process, how not to offer some clarification on drying and drying efficiency: as Chinese invention patent 200710008973 " is the method for feedstock production high-adsorption active carbon with the petroleum coke " be with the petroleum coke be raw material after with product cooling, washing, drying product; And for example Chinese invention patent 200610139415 " with the method for preparing low ash high specific surface area active carbon from coconut shell slag " then discloses a kind of method with preparing low ash high specific surface area active carbon from coconut shell slag; The deliming coconut-shell slag obtains active carbon after charing, activation, promptly obtain Powdered active carbon with high specific surface area after active carbon washing to neutrality, the oven dry; Chinese invention patent 200610038065 " a kind of preparation method of high specific surface area active charcoal based on formaldehyde-phenol resin " is that activated material is cooled off under inert atmosphere for another example; Wash earlier, pickling then is washed to neutrality at last; Drying promptly obtains the active carbon with high specific surface area of powdery.
Chinese invention patent 200610123444 " a kind of preparation method of high specific area anthrax active carbon " discloses a kind of preparation method of high specific area anthrax active carbon; Clearly activated material is washed with distillation earlier; Use pickling and alkali cleaning more repeatedly; Using zero(ppm) water to be washed till the pH value afterwards is 6～7, at 100～150 ℃ of down dry 10～15h, makes coal mass active carbon again; Chinese invention patent 200610034388 " a kind of preparation method of high superficial area bamboo active carbon " also is to activated material dry 10～15h under 100～150 ℃, makes bamboo absorbent charcoal.Can find out by above-mentioned two patents, during the dry consumption energy consumption of activated material.
Summary of the invention
The method that the purpose of this invention is to provide a kind of rapid drying active carbon with high specific surface area.
Preparing method of the present invention is following:
Contain carbon matrix precursor and KOH or NaOH by mass ratio 1: (3-8) behind the uniform mixing, in 800-950 ℃ of following N
2Activation 0.5-2h in the atmosphere; Naturally cool to room temperature afterwards; The thick product with deionized water that obtains is washed to neutral, through obtaining moisture activated material after spinning or the press filtration, is 1 according to moisture activated material with the volume of organic solvent ratio: (0.5-3) flood 0.5-2h down at 30-50 ℃; Obtain containing the activated material of solvent afterwards through spinning or press filtration, the activated material that contains solvent is carried out the drying back obtain product.
Aforesaid drying is air draught drying, constant pressure and dry or drying under reduced pressure.
As stated, adopting air draught exsiccant temperature is 50-90 ℃, and be 2-4h time of drying, the flow of air: according to the volume ratio that contains activating solvent material and air is 1: (5-10);
As stated, adopting the temperature of constant pressure and dry is 80-100 ℃, and be 5-12h time of drying;
As stated, adopting the temperature of drying under reduced pressure is 50-80 ℃, and be 2-3h time of drying, and vacuum tightness is 0.05-0.09MPa;
As stated, the organic solvent of employing is ethanol or acetone;
As stated, containing carbon matrix precursor is: refinery coke, coal, resin, agricultural crop straw carbide or shell class carbide etc.
Advantage of the present invention:
After adopting organic solvent with the replacement of the water in the gac duct, can greatly shorten the exsiccant time and significantly reduce drying temperature.The condensable recovery of the solvent that evaporates in the drying process, recycling causes the cost of this gac to descend.The present invention is easy and simple to handle in addition, is easy to control and large-scale production.
Embodiment
Embodiment 1
Refinery coke and KOH press behind the mass ratio 1:8 uniform mixing in 800 ℃ of following N
2Activation 0.5h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:3 floods 0.5h down at 50 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through press filtration afterwards.According to the volume ratio that contains ethanol activated material and air is that 1:10 adopts air draught dry, and drying temperature is 90 ℃, and be 2h time of drying, can obtain the product that specific surface area reaches 3410m2/g.
Embodiment 2
Resol and NaOH press behind the mass ratio 1:3 uniform mixing in 950 ℃ of following N
2Activation 2h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material after the spinning is that 1:0.5 floods 2h down at 30 ℃ according to the volume ratio of activated material and acetone, obtains containing the activated material of acetone afterwards through spinning.Being 100 ℃ in temperature adopts the dry 5h of method of constant pressure and dry can obtain the product that specific surface area reaches 2150m2/g down.
Embodiment 3
Hard coal and KOH press behind the mass ratio 1:5 uniform mixing in 850 ℃ of following N
2Activation 0.5h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:2 floods 1h down at 40 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through press filtration afterwards.In vacuum tightness is that dry 2h can obtain the product that specific surface area reaches 3320m2/g under 0.09MPa, temperature were 50 ℃.
Embodiment 4
Corn straw carbide and NaOH press behind the mass ratio 1:6 uniform mixing in 900 ℃ of following N
2Activation 1.5h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:0.5 floods 2h down at 50 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through press filtration afterwards.According to the volume ratio that contains ethanol activated material and air is that 1:5 adopts air draught dry, and drying temperature is 50 ℃, and be 4h time of drying, can obtain the product that specific surface area reaches 2580m2/g.
Embodiment 5
Coconut husk carbide and KOH press behind the mass ratio 1:4 uniform mixing in 830 ℃ of following N
2Activation 1h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material after the spinning is that 1:2 floods 2h down at 40 ℃ according to the volume ratio of activated material and acetone, obtains containing the activated material of acetone afterwards through spinning.Being 80 ℃ in temperature adopts the dry 12h of method of constant pressure and dry can obtain the product that specific surface area reaches 2860m2/g down.
Embodiment 6
Cotton stalk carbide and KOH press behind the mass ratio 1:5 uniform mixing in 850 ℃ of following N
2Activation 0.5h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:1 floods 1h down at 50 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through press filtration afterwards.In vacuum tightness is that dry 3h can obtain the product that specific surface area reaches 3320m2/g under 0.05MPa, temperature were 80 ℃.
Embodiment 7
Resol and NaOH press behind the mass ratio 1:5 uniform mixing in 850 ℃ of following N
2Activation 3h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material after the spinning is that 1:0.5 floods 2h down at 40 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through spinning afterwards.According to the volume ratio that contains ethanol activated material and air is that 1:8 adopts air draught dry, and drying temperature is 80 ℃, and be 3h time of drying, can obtain the product that specific surface area reaches 2340m2/g.
Embodiment 8
Coconut husk carbide and KOH press behind the mass ratio 1:5 uniform mixing in 850 ℃ of following N
2Activation 1.5h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material after the spinning is that 1:2 floods 1h down at 35 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through spinning afterwards.Being 90 ℃ in temperature adopts the dry 8h of method of constant pressure and dry can obtain the product that specific surface area reaches 3130m2/g down.
Embodiment 9
Cotton stalk carbide and NaOH press behind the mass ratio 1:6 uniform mixing in 950 ℃ of following N
2Activation 1h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:1 floods 0.5h down at 50 ℃ according to the volume ratio of activated material and acetone, obtains containing the activated material of acetone afterwards through press filtration.In vacuum tightness is that dry 2h can obtain the product that specific surface area reaches 2840m2/g under 0.07MPa, temperature were 70 ℃.
Embodiment 10
Refinery coke and NaOH press behind the mass ratio 1:8 uniform mixing in 900 ℃ of following N
2Activation 1h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:2.5 floods 0.5h down at 50 ℃ according to the volume ratio of activated material and acetone, obtains containing the activated material of acetone afterwards through press filtration.According to the volume ratio that contains acetone activated material and air is that 1:7 adopts air draught dry, and drying temperature is 70 ℃, and be 3h time of drying, can obtain the product that specific surface area reaches 2750m2/g.
Embodiment 11
Resol and KOH press behind the mass ratio 1:5 uniform mixing in 850 ℃ of following N
2Activation 1h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material after the spinning is that 1:1 floods 2h down at 30 ℃ according to activated material and alcoholic acid volume ratio, obtains containing the alcoholic acid activated material through spinning afterwards.Being 90 ℃ in temperature adopts the dry 10h of method of constant pressure and dry can obtain the product that specific surface area reaches 3210m2/g down.
Embodiment 12
Hard coal and NaOH press behind the mass ratio 1:8 uniform mixing in 900 ℃ of following N
2Activation 2h in the atmosphere cools to room temperature afterwards naturally, and the thick product of acquisition is extremely neutral with a large amount of deionized water wash.Moisture activated material behind the press filtration is that 1:2 floods 1h down at 40 ℃ according to the volume ratio of activated material and acetone, obtains containing the activated material of acetone afterwards through press filtration.In vacuum tightness is that dry 2h can obtain the product that specific surface area reaches 2950m2/g under 0.06MPa, temperature were 80 ℃.
Claims (7)
1. the method for a rapid drying active carbon with high specific surface area is characterized in that comprising the steps:
Contain carbon matrix precursor and KOH or NaOH by mass ratio 1:3-8 uniform mixing after, in 800-950 ℃ of following N
2Activation 0.5-2h in the atmosphere; Naturally cool to room temperature afterwards; The thick product with deionized water washing of acquisition through obtaining moisture activated material after spinning or the press filtration, is down flooded 0.5-2h for 1:0.5-3 at 30-50 ℃ according to moisture activated material and volume of organic solvent ratio to neutrality; Obtain containing the activated material of solvent afterwards through spinning or press filtration, the activated material that contains solvent is carried out the drying back obtain product.
2. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 1 is characterized in that described drying is air draught drying, constant pressure and dry or drying under reduced pressure.
3. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 2; It is characterized in that described employing air draught exsiccant temperature is 50-90 ℃; Be 2-4h time of drying, the flow of air: the volume ratio according to solvent-laden activated material and air is 1:5-10.
4. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 2, the temperature that it is characterized in that described employing constant pressure and dry is 80-100 ℃, be 5-12h time of drying.
5. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 2, the temperature that it is characterized in that described employing drying under reduced pressure is 50-80 ℃, and be 2-3h time of drying, and vacuum tightness is 0.05-0.09MPa.
6. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 1 is characterized in that described organic solvent is ethanol or acetone.
7. the method for a kind of rapid drying active carbon with high specific surface area as claimed in claim 1 is characterized in that the described carbon matrix precursor that contains is refinery coke, coal, resin, agricultural crop straw carbide or shell class carbide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101608091A CN102689901A (en) | 2012-05-23 | 2012-05-23 | Method for fast drying high specific surface area activated carbon |
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| CN2012101608091A CN102689901A (en) | 2012-05-23 | 2012-05-23 | Method for fast drying high specific surface area activated carbon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649267A (en) * | 2015-03-06 | 2015-05-27 | 方大炭素新材料科技股份有限公司 | Preparation method of activated carbon for making supercapacitors |
| CN107244670A (en) * | 2016-03-29 | 2017-10-13 | 四川大学 | A kind of bigger serface carbon material and preparation method thereof and for super capacitor material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001019904A1 (en) * | 1999-09-15 | 2001-03-22 | Tda Research, Inc. | Mesoporous carbons and polymers |
| CN1884062A (en) * | 2006-07-10 | 2006-12-27 | 山西中良煤化工科技有限公司 | Process of continuous preparation of activated carbon with high specific surface area |
| CN101985358A (en) * | 2010-11-09 | 2011-03-16 | 同济大学 | Method for quickly preparing carbon-silicon dioxide composite aerogel |
-
2012
- 2012-05-23 CN CN2012101608091A patent/CN102689901A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001019904A1 (en) * | 1999-09-15 | 2001-03-22 | Tda Research, Inc. | Mesoporous carbons and polymers |
| CN1884062A (en) * | 2006-07-10 | 2006-12-27 | 山西中良煤化工科技有限公司 | Process of continuous preparation of activated carbon with high specific surface area |
| CN101985358A (en) * | 2010-11-09 | 2011-03-16 | 同济大学 | Method for quickly preparing carbon-silicon dioxide composite aerogel |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649267A (en) * | 2015-03-06 | 2015-05-27 | 方大炭素新材料科技股份有限公司 | Preparation method of activated carbon for making supercapacitors |
| CN107244670A (en) * | 2016-03-29 | 2017-10-13 | 四川大学 | A kind of bigger serface carbon material and preparation method thereof and for super capacitor material |
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Application publication date: 20120926 |