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CN1186043A - Method for producing activated carbon with high specific surface area from asphalt - Google Patents

Method for producing activated carbon with high specific surface area from asphalt
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Publication number
CN1186043A
CN1186043ACN96123525ACN96123525ACN1186043ACN 1186043 ACN1186043 ACN 1186043ACN 96123525 ACN96123525 ACN 96123525ACN 96123525 ACN96123525 ACN 96123525ACN 1186043 ACN1186043 ACN 1186043A
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Prior art keywords
specific surface
surface area
activated carbon
high specific
asphalt
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CN96123525A
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CN1048955C (en
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刘朗
乔文明
查庆芳
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

A process for preparing activated carbon having superhigh specific surface area with asphalt includes such technological steps as non-melting treatment of high-softening-point asphalt by oxidizing with air at 260-360 deg.C, mixing with KOH as activater in wt. ratio of 1 : (1-10), alkaline activating at 600-900 deg.C in inertial gas atmosphere for 0.5-2 hr, cooling and washing. Its specific surface area is 2500-3600 sq.m/g and its ash content is less than 0.1 Wt.%. Its other advantages include simple process, low cost and low impurities conten in raw material.

Description

Method by the bitumen production activated carbon with high specific surface area
The invention belongs to the preparation of gac.
Conventional gac generally is that raw material prepares with the coal and since the impurity ash oontent height of coal cause gac impurity ash oontent height, specific surface area is low and absorption property is not good.Can not satisfy the needs of the key areas such as recovery of food, medicine, senior environmental protection, military affairs, chemical industry, catalysis, noble metal.Thereby, be badly in need of exploitation and have the novel absorption material that the impurity ash oontent is low, the specific surface area high absorption property is good.The preparation of relevant activated carbon with high specific surface area is a unusual active subject in recent years.U.S. Pat 3624004 and US4082694 provide with refinery coke and coal and have been raw material, are activator with KOH, and (its BET specific surface is greater than 2500m to adopt chemical activation method to prepare activated carbon with high specific surface area2/ g) method.Cost height and impurity ash oontent owing to refinery coke in aforesaid method are higher, so the impurity ash oontent of prepared activated carbon with high specific surface area higher (1.5wt%); With the coal is raw material, though cost can reduce the impurity ash oontent of prepared activated carbon with high specific surface area higher (2wt%).And we know, the height of impurity ash oontent is the important indicator of its performance height in the gac, and it directly influences gac application in a lot of fields.A kind of gac of excellent property is good adsorption performance not only, and its impurity ash oontent should be low as far as possible.U.S. Pat 5143889 is a raw material with the mesophase pitch microballoon, also adopts similar activation method to make the BET specific surface area greater than 3000m2The activated carbon with high specific surface area of/g.But because the mesophase pitch microballoon prepares by coal tar thermal treatment, yield too low (10%), thereby increased the cost of prepared activated carbon with high specific surface area greatly.In the method, mesophase pitch microballoon and activator mix also need add entry and acetone, have strengthened the corrosion of activation equipment, have increased manufacturing cost, are unfavorable for its widespread use.
The purpose of this invention is to provide a kind of is raw material with pitch, and preparation has the method for active carbon with superhigh specific surface area.Gac impurity ash oontent by this method preparation is low, and good adsorption performance and price are lower.
Method by the bitumen production activated carbon with high specific surface area of the present invention, carry out as follows:
(1) with high softening point bitumen under 260-360 ℃ through atmospheric oxidation melt processed not,
(2) then with the alkaline activation agent with 1: the part by weight of 1-10 mixes, in inert atmosphere
Handled 0.5-2 hour in 600-900 ℃ of following alkaline activation,
(3) get product after cooling, washing, the drying.
Being suitable for the employed pitch of present method is high softening point bitumen, and softening temperature is preferably 200-350 ℃, and carbon content is greater than 80wt%.High softening point bitumen can be obtained after general atmospheric oxidation thermal treatment by plurality of raw materials such as petroleum residual oil, coal tar, medium temperature coal pitch.
Described alkaline activation agent can be KOH.
The atmospheric oxidation that present method adopted not melt processed and activation treatment is processing method commonly used in this field.
Compared with the prior art method of the present invention has following advantage:
1. be the feedstock production activated carbon with high specific surface area with pitch, its BET specific surface area is 2500-3600m2/ g can prepare the activated carbon with high specific surface area that hangs down impurity ash content (less than 0.2wt%).
2. can control the value volume and range of product of the oxygen-containing functional group of asphalt surface by the infusible processing parameter of control pitch, thereby can control the priming reaction active site, the surface chemical structure and the surface physics structure of control activated carbon with high specific surface area are to meet the different needs.
3. present device and technological operation are simple, and the cost of making the asphaltic base activated carbon with high specific surface area is low, helps widespread use.
The present invention is described in detail for the embodiment that provides below.
Embodiment 1
With the petroleum residual oil is raw material, after 300-400 ℃ of underpressure distillation 1-6 hour, (softening temperature is 250 ℃ to make high softening point bitumen, carbon content is 93.3wt%, ash content divides 0.04wt%), high softening point bitumen is pulverized, get three grade 74-100 microns, 65-74 micron, 40-65 micron, carry out not melt processed (heat-up rate is 2 ℃/minute) of oxidation then, the whole temperature of oxidation is 320 ℃) back standby.
Embodiment 2
Get not molten asphalt 2 grams of 74-100 micron among the embodiment 1, after mixing with 8 gram alkaline activation agent KOH, the reactor of packing into, (heat-up rate is 10 ℃/minute, and whole temperature is 900 ℃ to carry out charing and activation treatment in nitrogen atmosphere, soak time is 1 hour), take out activation products behind the cool to room temperature, through dilute hydrochloric acid washing, water washing (to remove alkaline matter), after the drying, make the asphaltic base active carbon with superhigh specific surface area, its BET specific surface area is 2666m2/ g, the activation yield is 28.8wt%, ash oontent is 0.03wt%.
Embodiment 3
Get not molten asphalt 2 grams of 65-74 micron among the embodiment 1, after mixing with 8 gram KOH, the reactor of packing into.Other condition is with embodiment 2.Prepared asphaltic base activated carbon with high specific surface area BTE specific surface area is 3021m2/ g, the activation yield is 24.7wt%, ash oontent is 0.04wt%.
Embodiment 4
Get not molten asphalt 2 grams of 40-65 micron among the embodiment 1, after mixing with 8 gram KOH, the reactor of packing into.Other condition is with embodiment 2, and the active BTE specific surface area of prepared asphaltic base superhigh specific surface area is 3646m2/ g, the activation yield is 20.5wt%, ash oontent is 0.05wt%.
Embodiment 5
Get not molten asphalt 2 grams of 74-100 micron among the embodiment 1, after KOH mix with 4 grams, the reactor of packing into, (heat-up rate is 10 ℃/minute to carry out charing and activation treatment in nitrogen atmosphere, whole temperature is 600 ℃, and soak time is 1 hour), take out activation products behind the cool to room temperature, after dilute hydrochloric acid washing, water washing, drying, making the BET specific surface area is 709m2The asphalt based active carbon of/g, the activation yield is 41.4wt%, ash oontent is 0.024wt%.
Analytical procedure calculation formula in the above-mentioned data is:
The BET surface-area: measure with ASAP absorption instrument, method is according to nitrogen adsorption isothermal line data under the low temperature (77K), by the BET Equation for Calculating.Ash content:The activation yield:
Figure A9612352500052

Claims (3)

1. method by the bitumen production activated carbon with high specific surface area is characterized in that carrying out as follows:
(1) with high softening point bitumen under 260-360 ℃ through atmospheric oxidation melt processed not,
(2) then with the alkaline activation agent with 1: the part by weight of 1-10 mixes, in inert atmosphere
Handled 0.5-2 hour in 600-900 ℃ of following alkaline activation,
(3) get product after cooling, washing, the drying.
2. the method for claim 1, the softening temperature that it is characterized in that described high softening point bitumen is 200-300 ℃.
3. the method for claim 1, the heat-up rate of melt processed is 0.5-5 ℃/minute to it is characterized in that carrying out not by described high softening point bitumen in oxidizing atmosphere, oxidation temperature eventually is 260-360 ℃.
CN96123525A1996-12-241996-12-24Method for producing activated carbon with high specific surface area from asphaltExpired - Fee RelatedCN1048955C (en)

Priority Applications (1)

Application NumberPriority DateFiling DateTitle
CN96123525ACN1048955C (en)1996-12-241996-12-24Method for producing activated carbon with high specific surface area from asphalt

Applications Claiming Priority (1)

Application NumberPriority DateFiling DateTitle
CN96123525ACN1048955C (en)1996-12-241996-12-24Method for producing activated carbon with high specific surface area from asphalt

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Publication NumberPublication Date
CN1186043Atrue CN1186043A (en)1998-07-01
CN1048955C CN1048955C (en)2000-02-02

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
CN1091073C (en)*1998-12-252002-09-18中国科学院山西煤炭化学研究所Preparation of active carbon adsorbing and storing methane
CN102963891A (en)*2012-11-142013-03-13湖北华强科技有限责任公司Active carbon with low ash content and ultrahigh specific surface area and preparation method of active carbon
CN103272533A (en)*2013-06-082013-09-04中国科学院山西煤炭化学研究所Pitch sphere oxidative stabilization method
CN104583120A (en)*2012-07-262015-04-29关西热化学株式会社 Activated carbon with high active surface area
CN104556029A (en)*2014-12-212015-04-29沈阳工程学院Preparation of active carbon and fuel oil by use of petroleum residue and tar residue together
CN104927890A (en)*2015-06-092015-09-23中国科学院山西煤炭化学研究所Large-scale pitch sphere oxidation non-fusible preparation process and device
CN104944425A (en)*2015-07-022015-09-30神华集团有限责任公司Preparation method of active carbon
CN107804849A (en)*2017-12-052018-03-16中国石油化工股份有限公司A kind of preparation method of petroleum asphalt based active carbon and its asphalt based active carbon of preparation
CN109850864A (en)*2019-01-222019-06-07陕西理工大学A method of by the synthetic microporous carbon of pitch

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
EP1565404A2 (en)2002-11-132005-08-24Showa Denko K.K.Active carbon, production method thereof and polarizable electrode

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
US4082694A (en)*1975-12-241978-04-04Standard Oil Company (Indiana)Active carbon process and composition
JPH0915711A (en)*1995-06-301997-01-17Fuji Photo Optical Co LtdData imprinting device for camera

Cited By (12)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
CN1091073C (en)*1998-12-252002-09-18中国科学院山西煤炭化学研究所Preparation of active carbon adsorbing and storing methane
CN104583120A (en)*2012-07-262015-04-29关西热化学株式会社 Activated carbon with high active surface area
CN102963891A (en)*2012-11-142013-03-13湖北华强科技有限责任公司Active carbon with low ash content and ultrahigh specific surface area and preparation method of active carbon
CN103272533A (en)*2013-06-082013-09-04中国科学院山西煤炭化学研究所Pitch sphere oxidative stabilization method
CN104556029A (en)*2014-12-212015-04-29沈阳工程学院Preparation of active carbon and fuel oil by use of petroleum residue and tar residue together
CN104556029B (en)*2014-12-212017-03-08沈阳工程学院Petroleum residual oil is combined with tar slag and prepares activated carbon and fuel oil
CN104927890A (en)*2015-06-092015-09-23中国科学院山西煤炭化学研究所Large-scale pitch sphere oxidation non-fusible preparation process and device
CN104927890B (en)*2015-06-092017-03-08中国科学院山西煤炭化学研究所 Large-scale preparation process and device for oxidizing and infusible pitch pellets
CN104944425A (en)*2015-07-022015-09-30神华集团有限责任公司Preparation method of active carbon
CN107804849A (en)*2017-12-052018-03-16中国石油化工股份有限公司A kind of preparation method of petroleum asphalt based active carbon and its asphalt based active carbon of preparation
CN107804849B (en)*2017-12-052019-12-20中国石油化工股份有限公司Preparation method of petroleum asphalt-based activated carbon and asphalt-based activated carbon prepared by same
CN109850864A (en)*2019-01-222019-06-07陕西理工大学A method of by the synthetic microporous carbon of pitch

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