CN101397136A - Method for preparing high specific surface area granular activated carbon by physical activation process - Google Patents
Method for preparing high specific surface area granular activated carbon by physical activation process Download PDFInfo
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- CN101397136A CN101397136A CNA2008102335305A CN200810233530A CN101397136A CN 101397136 A CN101397136 A CN 101397136A CN A2008102335305 A CNA2008102335305 A CN A2008102335305A CN 200810233530 A CN200810233530 A CN 200810233530A CN 101397136 A CN101397136 A CN 101397136A
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- surface area
- specific surface
- active carbon
- gas
- high specific
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001994 activation Methods 0.000 title 1
- 235000013162 Cocos nucifera Nutrition 0.000 claims abstract description 17
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 17
- 230000004913 activation Effects 0.000 claims abstract description 14
- 230000005855 radiation Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000010903 husk Substances 0.000 claims description 14
- 239000005539 carbonized material Substances 0.000 claims description 11
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 15
- 238000003763 carbonization Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000004907 flux Effects 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The invention provides a method for preparing grain active carbon with high specific surface area by a physical activation method, comprising the steps as follows: firstly, coconut shell is carbonized under high temperature; subsequently, the crushed and screened carbonization material is arranged in a microwave radiation device; by controlling activation temperature and adjusting activation time and activation gas flux, the raw material is activated so as to gain the grain active carbon product with the specific surface area more than 2200m<2>/g. The method utilizes high-temperature carbonization to improve the micro-pore structure of the carbonization material of the coconut shell, is beneficial for improving the orderly structure of the carbonization material of the coconut shell, reduces the burning of the carbon during the carbonization process and improves the yield of the active carbon product; the prepared active carbon is the grain active carbon, and the applicable range is improved.
Description
One, technical field
The present invention relates to the method that a kind of physical activation method prepares high specific surface area granular activated carbon, belong to technical field of material.
Two, background technology
Gac is a kind of porous carbon material, has a wide range of applications in fields such as chemical industry, environmental protection, metallurgy, electronics and the energy.In recent years, along with science and technology development, the activated carbon application field constantly enlarges, and absorption property has been proposed new, higher requirement, under the general requirements of " high absorption, multi-functional, high strength ", occurred the increasing trend of special-purpose activated charcoal demand.Active carbon with high specific surface area adopts the chemical activation method to be prepared from usually at present, prepares 2000m with activators such as KOH, NaOH
2The height ratio specific surface area active carbon that/g is above makes fields such as its electrode that can be applied to double layer capacitor, Chu Qing, storage methane.But this method has corrodibility to equipment, and prepared gac mostly is the Powdered intensity that do not have, for its application brings certain limitation; Also need after having activated simultaneously product is carried out pickling and washing, this just brings secondary pollutants such as waste water, causes environmental pollution.Though and physical activation method does not produce pollution to environment, when the gac of preparation high-specific surface area, often need long time just can make its specific surface area reach 2000m at present
2More than/the g, this just causes prepared by physical method to have the energy consumption height that active carbon with high specific surface area needs, and the time is long, and the yield of products obtained therefrom is low, has reduced raw material availability, causes the significantly raising of its production cost.
In the patent No. is 200510010670.2 patent, a kind of " producing the method for active carbon with high specific surface area " disclosed, be raw material with the tobacco rod, KOH is an activator, with carrying out pickling, washing and oven dry after the microwave radiation, obtains activated carbon product.This method has stronger corrodibility to equipment on the one hand owing to added reagent such as pharmaceutical chemicals, needs on the other hand its product pickling and washing, brings secondary pollution.
In " the coconut husk charcoal prepares the research of active carbon with high specific surface area " that Su Wei etc. delivered in " chemistry of forest product with industry " the 2nd phase in 2006 with water vapour and CO
2Be common activated gas, prepare gac stage by stage, this legal system is equipped with specific surface area greater than 2000m
2The above gac of/g needs the time more than 10 hours at least, and yield is lower than 19.4%.Can find out from document: this method needs in preparation process mixed gas (water vapour and CO
2) accurately control in the ratio of different steps, this has brought certain degree of difficulty for preparation process.In the patent No. is in the patent of 200510010669.X, the method of a kind of " the waste tobacco stalk treated manufacturing gac of physics method " is disclosed, with the tobacco rod is raw material, water vapour is activated gas, though required time is shorter, but its product only can reach the requirement of activated carbon product commonly used, does not reach the application requiring in the fields such as electrode, Chu Qing, storage methane of double layer capacitor far away, and yield also lower (being lower than 30%).
Compare with above-mentioned technology, activated gas used in the present invention is water vapour and CO
2Gas has overcome chemical activation method to the corrosion of equipment and the pollution of environment; Needing with coconut husk carbonized material behind the process high temperature carbonization to raw material is raw material, the yield height (greater than 40%) of activated carbon product, the utilization that helps improving raw material resources; Adopt microwave as heating source,, realize it, and prepared gac is particulate state, improved range of application temperature controlling by adjusting microwave power.
Three, summary of the invention
The object of the present invention is to provide a kind of physical activation method to prepare the method for high specific surface area granular activated carbon; at first coconut husk is at high temperature carried out charing; to carry out subsequently fragmentation, the screening after carbonized material place microwave radiation device; by the control activation temperature; regulate soak time and activated gas flow; raw material is carried out activation treatment, and obtaining specific surface area is 2200m
2The granulated active carbon product that/g is above.
The present invention realizes that by following processing step Fig. 1 is its process flow sheet.
(1) with coconut husk in charring furnace 800~1200 ℃ of following charings 1~3 hour;
(2) the coconut husk carbonized material after the charing is carried out fragmentation, screening, getting particle diameter is 4~30 purpose particles;
(3) the coconut husk carbonized material after the fragmentation places microwave radiation device, when being heated to 800~950 ℃, feeding activated gas and activates, and obtains the active carbon with high specific surface area product.
Wherein when being activated gas with water vapour, its flow is 0.5~4L/min.Kg (the water vapour flow of per kilogram charcoal per minute); With CO
2During for activated gas, its flow is 1~5L/min.Kg (CO of per kilogram charcoal per minute
2Airshed); With CO
2When being activated gas with the mixed gas of water vapour, CO
2With the ratio of water vapour be 5~1:1, its flow is 0.5~6L/min.Kg (mixed gas flow of per kilogram charcoal per minute).
The present invention has the following advantages:
(1) adopts water vapour, CO
2A kind of or mixed gas be activated gas, do not produce the three wastes, environmentally safe, little to equipment corrosion;
(2) utilize high temperature carbonization, improve the microvoid structure of coconut husk carbonized material, for the preparation active carbon with high specific surface area provides the raw material with comparatively flourishing pore texture; Help improving the ordered structure of coconut husk carbonized material, reduce the ablation of charcoal in reactivation process, improve the yield of activated carbon product;
(3) utilize internal heating and the selectivity heat characteristic of microwave to material, overcome material temperature inside gradient, help the diffusion of activated gas in material inside, fast reaction speed, shorten soak time, reach energy-saving and cost-reducing, help the reaction of active site and activated gas, effectively promote the formation of hole, improved the yield of gac;
(4) prepared gac is a granulated active carbon, has improved its range of application;
Four, embodiment
Embodiment 1: get the coconut husk carbonized material 200g behind the high temperature carbonization, place microwave radiation device, be heated to 900 ℃, feed water vapour, its water vapour flow is 0.5L/min, activates after 1.25 hours, obtains having the activated carbon product of high-specific surface area.Its yield is 42.2%, and iodine sorption value is 1569.47mg/g, and specific surface area is 2279m
2/ g, pore volume is 1.212cm
3/ g.
Embodiment 2: get the coconut husk carbonized material 150g behind the high temperature carbonization, place microwave radiation device, be heated to 850 ℃, feed CO
2, CO wherein
2Flow is 0.6L/min, activates after 3 hours, obtains having the activated carbon product of high-specific surface area.Its yield, iodine sorption value, specific surface area and pore volume are respectively 49.2%, 1456.37mg/g, 2203m
2/ g and 1.255cm
3/ g.
Embodiment 3: get the coconut husk carbonized material 250g behind the high temperature carbonization, place microwave radiation device, be heated to 900 ℃, feed water vapour and CO
2Mixed gas, CO wherein
2With the ratio of water vapour be 3:1, mixed gas flow is 0.8L/min, activates after 1 hour, obtains having the activated carbon product of high-specific surface area.Its yield is 50.6%, and iodine sorption value is 1485.03mg/g, and specific surface area is 2250m
2/ g, pore volume is 1.157cm
3/ g.
Claims (2)
1. a physical activation method prepares the method for high specific surface area granular activated carbon, it is characterized in that: realize as follows,
(1) with coconut husk in charring furnace 800~1200 ℃ of following charings 1~3 hour;
(2) the coconut husk carbonized material after the charing is carried out fragmentation, screening, getting particle diameter is 4~30 purpose particles;
(3) the coconut husk carbonized material after the fragmentation places microwave radiation device, when being heated to 800~950 ℃, feeding activated gas and activates, and obtains the high specific surface area granular activated carbon product.
2. physical activation method according to claim 1 prepares the method for high specific surface area granular activated carbon, it is characterized in that: described activated gas is water vapour and CO
2A kind of in the gas, or both gas mixtures, when being activated gas with water vapour, its flow is 0.5~4L/min.Kg; With CO
2During for activated gas, its flow is 1~5L/min.Kg; With CO
2When being activated gas with the mixed gas of water vapour, CO
2With the ratio of water vapour be 5~1: 1, its flow is 0.5~6L/min.Kg.
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Cited By (26)
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CN101830461A (en) * | 2010-05-24 | 2010-09-15 | 浙江省林业科学研究院 | Method for making active carbon with powdery wooden materials by using one-step physical method and carbon activation furnace |
CN102205960A (en) * | 2011-04-29 | 2011-10-05 | 河南省核力科技发展有限公司 | Method for preparing activated carbon electrode material for super capacitor |
CN102580679A (en) * | 2012-01-13 | 2012-07-18 | 昆明理工大学 | Method for preparing modified microwave activated carbon sorbent |
CN102616778A (en) * | 2012-04-06 | 2012-08-01 | 昆明理工大学 | Method for preparing mesoporous activated carbon by regenerating waste coal-based activated carbon through microwave heating |
CN102786050A (en) * | 2012-07-16 | 2012-11-21 | 太仓市联林活性炭厂 | Method for preparing microporous cocoanut active charcoal by pyrolysis and activation |
CN102874803A (en) * | 2011-07-12 | 2013-01-16 | 栾清杨 | Preparation technology of active carbon for active carbon sheet materials |
CN104649266A (en) * | 2015-02-04 | 2015-05-27 | 昆明理工大学 | Preparation method of active carbon with high specific surface area made from bamboo wood |
CN104692380A (en) * | 2015-02-04 | 2015-06-10 | 昆明理工大学 | Preparation method of Ageratina-adenophora-base high-specific-area activated carbon |
WO2015106720A1 (en) * | 2014-01-20 | 2015-07-23 | 中盈长江国际新能源投资有限公司 | Method for producing super activated charcoal from biomass power plant ash |
CN102600850B (en) * | 2012-01-13 | 2016-06-22 | 昆明理工大学 | A kind of preparation method of the catalyst of elimination cos and Carbon bisulfide simultaneously |
CN105948036A (en) * | 2016-04-26 | 2016-09-21 | 湘潭大学 | Preparation method and application of porous active carbon material with radix puerariae-based interconnected hierarchical aperture structure |
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CN107381567A (en) * | 2017-09-15 | 2017-11-24 | 江苏科力特环保科技有限公司 | A kind of method of physical vapor method production activated carbon |
CN107500287A (en) * | 2017-08-04 | 2017-12-22 | 北海和荣活性炭科技有限责任公司 | A kind of production method of active carbon with high specific surface area |
CN107572518A (en) * | 2016-07-04 | 2018-01-12 | 现代自动车株式会社 | Method for preparing activated carbon |
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CN112871132A (en) * | 2019-11-29 | 2021-06-01 | 中国石油天然气集团有限公司 | Carbonyl activated carbon particles and preparation method and application thereof |
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-
2008
- 2008-11-04 CN CNA2008102335305A patent/CN101397136A/en active Pending
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CN108751190A (en) * | 2018-06-26 | 2018-11-06 | 阜南县胜天新能源开发有限公司 | A method of improving cocoanut active charcoal comprehensive utilization ratio |
CN112871132A (en) * | 2019-11-29 | 2021-06-01 | 中国石油天然气集团有限公司 | Carbonyl activated carbon particles and preparation method and application thereof |
CN113443627A (en) * | 2021-07-13 | 2021-09-28 | 四川泷邦净水材料有限公司 | Preparation and use method of activated carbon for purifying manganese sulfate solution |
CN113493203A (en) * | 2021-07-27 | 2021-10-12 | 福建省鑫森炭业股份有限公司 | Preparation method of activated carbon for regeneration treatment of kidney dialysate and activated carbon |
CN115784171A (en) * | 2022-11-23 | 2023-03-14 | 无锡日月水处理有限公司 | Method for recovering and treating waste sulfuric acid |
CN115784171B (en) * | 2022-11-23 | 2023-07-07 | 无锡日月水处理有限公司 | Recovery treatment method of waste sulfuric acid |
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