CN101209840A - Method for preparing high specific area anthrax active carbon - Google Patents
Method for preparing high specific area anthrax active carbon Download PDFInfo
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- CN101209840A CN101209840A CNA2007101856527A CN200710185652A CN101209840A CN 101209840 A CN101209840 A CN 101209840A CN A2007101856527 A CNA2007101856527 A CN A2007101856527A CN 200710185652 A CN200710185652 A CN 200710185652A CN 101209840 A CN101209840 A CN 101209840A
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Abstract
The invention provides a method for preparing coal activated carbon with high specific surface area. High metamorphosed coal and low metamorphosed coal are grinded respectively and then mixed according to a weight ratio of 1:1-10. The coal blending sample is mixed with KOH according to a weight ratio of 1:1-6, then N2 is input for protection, the temperature is heated to 400 to 600 DEG C by a speed of 2-8 DEG C/min, the constant temperature lasts for 1-2 hours, then is heated to 800 to 950 DEG C by the same speed and constant temperature lasts for 1-2 hours again, and is cooled down to room temperature; the mixture is washed by water till the PH value is 7-7.5, dipped with hydrochloric acid for 2-3 times, then washed by distilled water to be neutral and dried; a coal based activated carbon with high specific surface area is obtained. The invention has the advantages of wide raw material source, low price and higher specific surface area than 2500m<2>/g.
Description
Technical field
The invention belongs to a kind of method for preparing high specific area anthrax active carbon.
Background technology
The present Application Areas of active carbon with high specific surface area is more and more wideer, and especially the medium as clean fuel storage aspects such as following H2 and Sweet natural gases has advantageous advantage, so its preparation is the focus that people study always.The height of specific surface area is particularly important as gas storage to it, and the essential condition that the gac price also is it to come into the market.Adopt aboundresources, cheap coal the concrete remarkable advantages of starting raw material as the preparation active carbon with high specific surface area.
At present, adopting coal is physical activation method as the feedstock production process of active carbon overwhelming majority, and prepared gac specific surface area generally is no more than 1500m
2/ g is not suitable as the suitable media that stores above-mentioned gas.Expect the gac that the cost low specific surface area is high, can only adopt the method for chemical activation at present, disclose a kind of method of Sweet natural gas absorption super-activated carbon as patent 200510122081.This gac is that raw material mixes with coal dust, activator and coal tar, feeds superheated vapo(u)r under sealed state, obtains in a 800-830 ℃ of constant temperature 2-2.5 hour charing-activation-molecular sieveization;
Patent 200610098623 is pulverized high sulphur coal, be warmed up to 350~450 ℃ by weight 1: 4~8 after mixing with the KOH activator, constant temperature 1 hour is follow-up continuously to be warmed up to 750~850 ℃ and to activate, and constant temperature 100 minutes is made product through after a series of conventional processing;
97123209 of patents are pressed carbon raw material with carbon raw material and KOH: KOH=1: 1~5 (weight ratio) is through pulverizing at N
2Protection is packed into down and is heated to 400 ℃ in the closed reactor, keeps 1 hour, continues to be heated to 800 ℃, and priming reaction maintenance 1 hour obtains gac;
It is raw material that 55 pages of coal conversion the 27th the 4th phases of volume provide with high-sulfur, low-rank coal, adopts the method that adds the prepared active carbon with high specific surface area of KOH chemical activation after the saltpetre preoxidation;
Studied the 55th page of novel charcoal material the 13rd the 4th phase of volume that dipping KOH method has made specific surface area greater than 1500m to the operation of active carbon from coal absorption property in the active carbon from coal production technique
2The gac of/g.
What aforesaid method adopted all is that single coal is carried out activation treatment, although adopt chemical activation method, the generally not super 2500m of the specific surface area of the gac that makes
2/ g, and the specific surface area general requirement of gac that is applied to gas storage is at 2500m
2Could increase the adsorptive capacity of gas on gac significantly more than the/g.
Summary of the invention
The purpose of this invention is to provide a kind of raw material sources extensive, cheap be that the specific surface area of raw material is greater than 2500m with the coal
2The preparation method of active carbon of/g.
Owing to is the gac of raw material production with single coal, its pore structure and absorption property respectively have characteristics: with the bituminous coal of low metamorphic grade is that the gac mesopore of raw material production is abundanter, with the activated carbon capillary prosperity that is raw material production of high metamorphic grade hard coal; Add AI in the feed coal
2O
3, SiO
2, Fe
2O
3, CaO, MgO, K
2O, Na
2O etc. have certain influence, wherein Fe to reactivation process
2O
3, CaO, MgO, K
2O and Na
2O etc. have certain katalysis to reactivation process.Therefore, if two kinds of different coals of metamorphic grade are mixed according to a certain percentage, and under the KOH effect, can make the carbide of two kinds of coals that crosslinking reaction and polyreaction just take place before liquid phase forms, directly generation is unbodied solid-state, becomes the plain presoma of awkward graphitized charcoal; In addition, two kinds of coals have also changed the content of above-mentioned inorganic oxide in coal after mixing, and the absorption property of final prepared gac is also had certain positive effect.
The method for preparing high specific area anthrax active carbon of the present invention is as follows:
(1) coal with high metamorphic grade and low metamorphic grade grinds respectively, gets the coal dust of particle diameter between the 30-150 order after the screening, and be 1 by the coal weight ratio of high metamorphic grade and low metamorphic grade: 1-10 mixes, and obtains the coal blending sample; And then be 1 by coal blending sample: KOH: the weight ratio of 1-6 mixes, and obtains compound sample;
(2) compound sample is placed in the activation furnace, feeds N
2Protect, be raised to 400-600 ℃ with the temperature rise rate of 2-8 ℃/min, constant temperature 1-2h continues to be raised to 800-950 ℃ with same temperature rise rate afterwards, and constant temperature 1-2h drops to room temperature naturally again, obtains activated material;
(3) activated material is washed with water to after pH value is 7-7.5, uses salt acid dipping 2-3 time instead, uses distilled water wash afterwards instead to neutral, is drying to obtain high specific area anthrax active carbon.
The coal of aforesaid high metamorphic grade is a hard coal.
The coal of aforesaid low metamorphic grade is weakly caking coal, coking coal, meager coal etc.
Advantage of the present invention:
(1) adopts high rotten and low rotten two kinds of coals, can obtain specific surface area greater than 2500m
2The gac of the high pore structure prosperity of/g;
The collocation of the different coals of (2) two kinds of prices is expected to reduce the raw materials cost of final gained gac, the cost of especially high rotten coal (as reducing anthracitic consumption);
(3) the inventive method is simple, only needs two kinds of coals are directly mixed to activate to get final product.
Embodiment
Embodiment 1: hard coal and weakly caking coal are ground respectively, get the coal dust of particle diameter between the 30-80 order after the screening, by hard coal: the weakly caking coal weight ratio is to mix at 1: 10; And then be that 1: 6 weight ratio mixes by coal blending sample: KOH; Compound sample is placed in the activation furnace, feeds N
2Protect, be raised to 400 ℃ with the temperature rise rate of 8 ℃/min, constant temperature 2h continues to be raised to 800 ℃ with same temperature rise rate afterwards, and constant temperature 1h drops to room temperature naturally again; Activated material is washed with water to after the pH value is 7.2, uses the salt acid dipping instead 3 times, uses distilled water wash afterwards instead to neutral, drying.The specific surface area of gained gac is 2650m
2/ g.
Comparative Examples 1: with single hard coal is that raw material experimentizes, and other condition is with embodiment 1.The specific surface area of gained gac is 2220m
2/ g.
Embodiment 2: hard coal and coking coal are ground respectively, get the coal dust of particle diameter between the 50-100 order after the screening, according to hard coal: the coking coal weight ratio is to mix at 10: 1; And then be that 1: 5 weight ratio mixes by coal sample: KOH; Compound sample is placed in the activation furnace, feeds N2 and protects, and is raised to 600 ℃ with the temperature rise rate of 5 ℃/min, and constant temperature 1h continues to be raised to 900 ℃ with same temperature rise rate afterwards, and constant temperature 1h drops to room temperature naturally again; Activated material with tap water wash be 7.5 to the pH value after, use the salt acid dipping instead 2 times, use distilled water wash afterwards instead to neutral, drying.The specific surface area of gained gac is 2960m
2/ g.
Comparative Examples 2: with single hard coal is that raw material experimentizes, and other condition is with embodiment 2.The specific surface area of gained gac is 2610m
2/ g.
Embodiment 3: hard coal and meager coal are ground respectively, get the coal dust of particle diameter between the 100-150 order after the screening, according to high hard coal: the meager coal weight ratio is to mix at 1: 1; And then be that 1: 4 weight ratio mixes by coal sample: KOH; Compound sample is placed in the activation furnace, feeds N2 and protects, and is raised to 400 ℃ with the temperature rise rate of 2 ℃/min, and constant temperature 2h continues to be raised to 950 ℃ with same temperature rise rate afterwards, and constant temperature 1h drops to room temperature naturally again; Activated material with tap water wash be 7.3 to the pH value after, use the salt acid dipping instead 3 times, use distilled water wash afterwards instead to neutral, drying.The specific surface area of gained gac is 3230m
2/ g.
Comparative Examples 3: with single hard coal is that raw material experimentizes, and other condition is with embodiment 3.The specific surface area of gained gac is 2850m
2/ g.
Embodiment 4: hard coal and weakly caking coal are ground respectively, get the coal dust of particle diameter between the 120-150 order after the screening, according to hard coal: the weakly caking coal weight ratio is to mix at 3: 2; And then be that 1: 5 weight ratio mixes by coal sample: KOH; Compound sample is placed in the activation furnace, feeds N2 and protects, and is raised to 500 ℃ with the temperature rise rate of 5 ℃/min, and constant temperature 1h continues to be raised to 900 ℃ with same temperature rise rate afterwards, and constant temperature 2h drops to room temperature naturally again; Activated material with tap water wash be 7.1 to the pH value after, use the salt acid dipping instead 2 times, use distilled water wash afterwards instead to neutral, drying.The specific surface area of gained gac is 3550m
2/ g.
Comparative Examples 4: with single hard coal is that raw material experimentizes, and other condition is with embodiment 4.The specific surface area of gained gac is 2940m
2/ g.
Claims (3)
1. a method for preparing high specific area anthrax active carbon is characterized in that comprising the steps:
(1) coal with high metamorphic grade and low metamorphic grade grinds respectively, gets the coal dust of particle diameter between the 30-150 order after the screening, and be 1 by the coal weight ratio of high metamorphic grade and low metamorphic grade: 1-10 mixes, and obtains the coal blending sample; And then be 1 by coal blending sample: KOH: the weight ratio of 1-6 mixes, and obtains compound sample;
(2) compound sample is placed in the activation furnace, feeds N2 and protects, and is raised to 400-600 ℃ with the temperature rise rate of 2-8 ℃/min, and constant temperature 1-2h continues to be raised to 800-950 ℃ with same temperature rise rate afterwards, and constant temperature 1-2h drops to room temperature naturally again, obtains activated material;
(3) activated material is washed with water to after pH value is 7-7.5, uses salt acid dipping 2-3 time instead, uses distilled water wash afterwards instead to neutral, is drying to obtain high specific area anthrax active carbon.
2. a kind of method for preparing high specific area anthrax active carbon as claimed in claim 1, the coal that it is characterized in that described high metamorphic grade is a hard coal.
3. a kind of method for preparing high specific area anthrax active carbon as claimed in claim 1, the coal that it is characterized in that described low metamorphic grade is weakly caking coal, coking coal or meager coal.
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102432004A (en) * | 2011-09-22 | 2012-05-02 | 煤炭科学研究总院 | Active carbon for deeply purifying drinking water and preparation method thereof |
CN102689899A (en) * | 2012-05-23 | 2012-09-26 | 中国科学院山西煤炭化学研究所 | A preparation method for improving specific surface area of activated carbon |
CN103172065A (en) * | 2013-04-12 | 2013-06-26 | 宁夏大学 | Production technology for preparing pea coal activated carbon by chemical activation method |
CN104291333A (en) * | 2014-09-10 | 2015-01-21 | 重庆大学 | Method for preparing stone coal based mesoporous activated carbon with high specific surface area |
CN104891487A (en) * | 2015-04-30 | 2015-09-09 | 山东大学 | Method for rapidly preparing powdery active coke |
CN105056888A (en) * | 2015-08-07 | 2015-11-18 | 沧州绿源水处理有限公司 | Preparation method of composite coal-based adsorbing material |
CN105217625A (en) * | 2015-09-16 | 2016-01-06 | 中国矿业大学(北京) | Take weak caking coal as the agglomerated activated carbon prepared of major ingredient coal blending and method for making and application |
CN105984869A (en) * | 2015-01-30 | 2016-10-05 | 克州生产力促进中心(有限公司) | Method for preparing ethylenediamine modified activated carbon |
CN106241800A (en) * | 2016-08-30 | 2016-12-21 | 宁夏华辉活性炭股份有限公司 | The specially method for preparation of active carbon of effect absorption tetrafluoride charcoal |
CN108217649A (en) * | 2018-02-06 | 2018-06-29 | 韩笑峰 | A kind of coal activated carbon stove preparing active carbon method |
CN111217369A (en) * | 2020-03-10 | 2020-06-02 | 国家能源集团宁夏煤业有限责任公司 | Benzene protection active carbon and preparation method thereof |
CN112876310A (en) * | 2021-02-05 | 2021-06-01 | 内蒙古博大实地化学有限公司 | Compound fertilizer containing soil conditioning performance and preparation method thereof |
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2007
- 2007-12-24 CN CNA2007101856527A patent/CN101209840A/en active Pending
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102432004A (en) * | 2011-09-22 | 2012-05-02 | 煤炭科学研究总院 | Active carbon for deeply purifying drinking water and preparation method thereof |
CN102689899A (en) * | 2012-05-23 | 2012-09-26 | 中国科学院山西煤炭化学研究所 | A preparation method for improving specific surface area of activated carbon |
CN102689899B (en) * | 2012-05-23 | 2014-02-19 | 中国科学院山西煤炭化学研究所 | A preparation method for improving specific surface area of activated carbon |
CN103172065A (en) * | 2013-04-12 | 2013-06-26 | 宁夏大学 | Production technology for preparing pea coal activated carbon by chemical activation method |
CN104291333A (en) * | 2014-09-10 | 2015-01-21 | 重庆大学 | Method for preparing stone coal based mesoporous activated carbon with high specific surface area |
CN105984869A (en) * | 2015-01-30 | 2016-10-05 | 克州生产力促进中心(有限公司) | Method for preparing ethylenediamine modified activated carbon |
CN104891487A (en) * | 2015-04-30 | 2015-09-09 | 山东大学 | Method for rapidly preparing powdery active coke |
CN105056888A (en) * | 2015-08-07 | 2015-11-18 | 沧州绿源水处理有限公司 | Preparation method of composite coal-based adsorbing material |
CN105217625A (en) * | 2015-09-16 | 2016-01-06 | 中国矿业大学(北京) | Take weak caking coal as the agglomerated activated carbon prepared of major ingredient coal blending and method for making and application |
CN106241800A (en) * | 2016-08-30 | 2016-12-21 | 宁夏华辉活性炭股份有限公司 | The specially method for preparation of active carbon of effect absorption tetrafluoride charcoal |
CN106241800B (en) * | 2016-08-30 | 2018-08-03 | 宁夏华辉活性炭股份有限公司 | The specially method for preparation of active carbon of effect absorption carbon tetrafluoride |
CN108217649A (en) * | 2018-02-06 | 2018-06-29 | 韩笑峰 | A kind of coal activated carbon stove preparing active carbon method |
CN111217369A (en) * | 2020-03-10 | 2020-06-02 | 国家能源集团宁夏煤业有限责任公司 | Benzene protection active carbon and preparation method thereof |
CN112876310A (en) * | 2021-02-05 | 2021-06-01 | 内蒙古博大实地化学有限公司 | Compound fertilizer containing soil conditioning performance and preparation method thereof |
CN112876310B (en) * | 2021-02-05 | 2022-06-21 | 内蒙古博大实地化学有限公司 | Compound fertilizer containing soil conditioning performance and preparation method thereof |
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Open date: 20080702 |