CN105366674A - Preparation method of rich mesoporous high-specific surface area activated carbon - Google Patents
Preparation method of rich mesoporous high-specific surface area activated carbon Download PDFInfo
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- CN105366674A CN105366674A CN201410428179.0A CN201410428179A CN105366674A CN 105366674 A CN105366674 A CN 105366674A CN 201410428179 A CN201410428179 A CN 201410428179A CN 105366674 A CN105366674 A CN 105366674A
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Abstract
The invention relates to a preparation method of rich mesoporous high-specific surface area activated carbon. The problems that in the prior art, process is complex and production cost is high are mainly solved. One weight part of activated carbon powder is heated to 700-1000 DEG C from the room temperature in the nitrogen atmosphere, then 0.01-0.15 weight part of carbon dioxide is secondarily activated for 10 minutes to 2.5 hours in the minute atmosphere and is then cooled to the room temperature in the nitrogen atmosphere, and then rich mesoporous high-specific surface area activated carbon is prepared. According to the technical scheme, the problems are solved, and the method can be used for industrial production of adsorption, catalysis and energy storage materials.
Description
Technical field
The present invention relates to a kind of preparation method being rich in mesopore active carbon with high specific surface area.
Background technology
Gac raw materials abundance, cheap, be widely used in absorption, be separated, purify, the field such as catalysis and energy storage.Current commercial gac specific surface area is less, and form primarily of micropore, only containing a small amount of mesopore and macropore, but be used as to be separated the sorbent material of macromolecular substance, support of the catalyst and electrochemical capacitor electrode material etc. and need that there is larger specific surface area and higher mesoporous.
About being rich in mesopore, the preparation of active carbon with high specific surface area has many reports, is broadly divided into three kinds, i.e. direct activation method, catalytic activation method and template.
Direct activation method needs to use chemical activating agent usually, disclose a kind of high-specific surface area as document CN201110210608.3 and be rich in the preparation method of the mangosteen shell gac of mesopore, it adopts potassium oxalate to make activator, at 700 ~ 900 DEG C, the discarded mangosteen shell of activation obtains the gac being rich in mesopore, but its specific surface area is less, only 1100m
2about/g.Due to chemical activating agent severe corrosive at high temperature, therefore activation equipment requires higher, and reaction product must through pickling and washing removing residue chemical reagent, and cause complex process, production cost is high, and environment friendly is poor.
Catalytic activation method changes speed and the selectivity of priming reaction by adding catalyzer in presoma, thus prepares the gac of mesopore prosperity.As document CN99106067.9 discloses a kind of coal-based mesopore activated carbon manufacture method, it take coal as raw material, the mode of mechanically mixing or dipping is adopted to add the transistion metal compounds such as Fe, Co, Ni of 0.5 ~ 15% wherein, obtained specific surface area 1100 ~ 1600m after steam activation
2the mesopore activated carbon of/g, mesoporous 20 ~ 50%.Although the method significantly improves mesoporous and the Carbon yield of gac, the use of transition-metal catalyst adds the postprocessing working procedures of raw materials cost and production, causes production cost to rise.
Template normally deposits organic precursor in porous molecular screen template, removes template again and obtain mesopore activated carbon after charing.As document CN200610134271.1 disclose a kind of with asphaltene class material for the method for ordered structure mesoporous carbon prepared by raw material, its with mesoporous melecular sieves SBA-15 for template, with the by product asphaltene class material in coal direct liquefaction process for carbon source, obtained powdery mesoporous carbon after polymerization, charing, the demoulding.The mesoporous carbon structure that the method prepares is orderly, pore size uniform, controllable, but its raw material subject range is narrow, technique is loaded down with trivial details, preparation cost is higher, is not suitable for suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists complex process, problem that production cost is high, provides a kind of preparation method being rich in mesopore, active carbon with high specific surface area newly.The method has the advantages that technique is simple, production cost is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of preparation method being rich in mesopore active carbon with high specific surface area, by the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 700 ~ 1000 DEG C, then re-activation process 10 minutes ~ 2.5 hours in 0.01 ~ 0.15 part of heavy carbonic acid gas/minute atmosphere, in nitrogen atmosphere, be cooled to room temperature, described in namely obtaining, be rich in mesopore active carbon with high specific surface area.
In technique scheme, preferably, described active carbon powder is coconut shell based activated carbon.
In technique scheme, preferably, described re-activation treatment temp is 750 ~ 950 DEG C.
In technique scheme, preferably, described carbon dioxide atmosphere be 0.02 ~ 0.12 part of weight/minute.
In technique scheme, preferably, the described re-activation treatment time is 0.5 ~ 2 hour.
In the present invention, to have the gac of certain initial hole for raw material, carry out re-activation with appropriate carbonic acid gas, carbonic acid gas and carbon react, and the original micropore size of gac is broadened, and pore volume increases, thus effectively improve its specific surface area; Part adjacent cells is fused into mesopore because hole wall complete reaction disappears, and its mesoporous is improved.Therefore can be prepared by processing parameters such as control activation temperature, activator level and soak times and be rich in mesopore active carbon with high specific surface area.
Compared with prior art, re-activation technique of the present invention is simple, and without the need to using chemical reagent and expensive specific equipment, production cost is lower, is easy to commercial introduction application; Prepared gac has larger specific surface area and higher mesoporous simultaneously, can be widely used in the fields such as absorption, catalysis and energy storage material.
Below by embodiment, the invention will be further elaborated.
Embodiment
[embodiment 1]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 750 DEG C, then re-activation process 2 hours in per minute 0.1 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1037m
2/ g, mesoporous is 22.7%.
[embodiment 2]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 850 DEG C, then re-activation process 2 hours in per minute 0.08 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1210m
2/ g, mesoporous is 27.8%.
[embodiment 3]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 900 DEG C, then re-activation process 2 hours in per minute 0.02 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1173m
2/ g, mesoporous is 23.2%.
[embodiment 4]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 900 DEG C, then re-activation process 2 hours in per minute 0.1 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1518m
2/ g, mesoporous is 39.2%.
[embodiment 5]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 950 DEG C, then re-activation process 1 hour in per minute 0.1 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1607m
2/ g, mesoporous is 34.9%.
[embodiment 6]
By the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 900 DEG C, then re-activation process 0.5 hour in per minute 0.12 part of heavy carbon dioxide atmosphere, is cooled to room temperature in nitrogen atmosphere.The BET specific surface area of obtained gac is 1359m
2/ g, mesoporous is 29.5%.
Claims (5)
1. one kind is rich in the preparation method of mesopore active carbon with high specific surface area, by the active carbon powder of 1 part heavy in nitrogen atmosphere from room temperature to 700 ~ 1000 DEG C, then re-activation process 10 minutes ~ 2.5 hours in 0.01 ~ 0.15 part of heavy carbonic acid gas/minute atmosphere, in nitrogen atmosphere, be cooled to room temperature, described in namely obtaining, be rich in mesopore active carbon with high specific surface area.
2. be rich in the preparation method of mesopore active carbon with high specific surface area according to claim 1, it is characterized in that described active carbon powder is coconut shell based activated carbon.
3. be rich in the preparation method of mesopore active carbon with high specific surface area according to claim 1, it is characterized in that described re-activation treatment temp is 750 ~ 950 DEG C.
4. be rich in the preparation method of mesopore active carbon with high specific surface area according to claim 1, it is characterized in that described carbon dioxide atmosphere be 0.02 ~ 0.12 part of weight/minute.
5. be rich in the preparation method of mesopore active carbon with high specific surface area according to claim 1, it is characterized in that the described re-activation treatment time is 0.5 ~ 2 hour.
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| CN201410428179.0A CN105366674A (en) | 2014-08-27 | 2014-08-27 | Preparation method of rich mesoporous high-specific surface area activated carbon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106190317A (en) * | 2016-07-22 | 2016-12-07 | 新奥科技发展有限公司 | The preparation method of coal gasifier, gasification system and activated coke |
| CN107055503A (en) * | 2017-02-28 | 2017-08-18 | 广西秀美壮乡能源环保有限公司 | A kind of preparation method of Mesoporous Carbon Materials |
| CN110668439A (en) * | 2019-11-01 | 2020-01-10 | 海南星光活性炭有限公司 | Preparation method of coconut shell activated carbon for extracting gold |
| CN113522233A (en) * | 2020-04-17 | 2021-10-22 | 中国石油化工股份有限公司 | Purifying agent, preparation method and application thereof, and purifying method |
Citations (3)
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| CN101239329A (en) * | 2008-03-10 | 2008-08-13 | 中国林科院林产化工研究所江苏省溧阳市活性炭联合工厂 | Method for preparing palladium catalyst carrier special-purpose active carbon |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
| CN103787331A (en) * | 2014-02-28 | 2014-05-14 | 东北林业大学 | Preparation method of pitch-based spherical activated carbon with rich meso pores |
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2014
- 2014-08-27 CN CN201410428179.0A patent/CN105366674A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101239329A (en) * | 2008-03-10 | 2008-08-13 | 中国林科院林产化工研究所江苏省溧阳市活性炭联合工厂 | Method for preparing palladium catalyst carrier special-purpose active carbon |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
| CN103787331A (en) * | 2014-02-28 | 2014-05-14 | 东北林业大学 | Preparation method of pitch-based spherical activated carbon with rich meso pores |
Non-Patent Citations (1)
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| JUAN F. GONZA´LEZ ET AL.,: "Porosity Development in Activated Carbons Prepared from Walnut Shells by Carbon Dioxide or Steam Activation", 《INDUSTRIAL&ENGINEERING CHEMISTRY RESEARCH》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106190317A (en) * | 2016-07-22 | 2016-12-07 | 新奥科技发展有限公司 | The preparation method of coal gasifier, gasification system and activated coke |
| CN106190317B (en) * | 2016-07-22 | 2020-10-27 | 新奥科技发展有限公司 | Coal gasification furnace, coal gasification system and preparation method of active coke |
| CN107055503A (en) * | 2017-02-28 | 2017-08-18 | 广西秀美壮乡能源环保有限公司 | A kind of preparation method of Mesoporous Carbon Materials |
| CN107055503B (en) * | 2017-02-28 | 2019-03-12 | 江苏丽鑫实业有限公司 | A kind of production method of Mesoporous Carbon Materials |
| CN110668439A (en) * | 2019-11-01 | 2020-01-10 | 海南星光活性炭有限公司 | Preparation method of coconut shell activated carbon for extracting gold |
| CN113522233A (en) * | 2020-04-17 | 2021-10-22 | 中国石油化工股份有限公司 | Purifying agent, preparation method and application thereof, and purifying method |
| CN113522233B (en) * | 2020-04-17 | 2023-09-29 | 中国石油化工股份有限公司 | Purifying agent, preparation method and application thereof and purifying method |
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Application publication date: 20160302 |