CN102627276A - Method for preparing nutshell activated carbon by pyrolyzing activation technology and activated carbon - Google Patents
Method for preparing nutshell activated carbon by pyrolyzing activation technology and activated carbon Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000004913 activation Effects 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title abstract description 9
- 238000000197 pyrolysis Methods 0.000 claims abstract description 123
- 239000002994 raw material Substances 0.000 claims abstract description 80
- 238000001179 sorption measurement Methods 0.000 claims abstract description 49
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 25
- 239000011630 iodine Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- 238000010792 warming Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 238000005554 pickling Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 235000013399 edible fruits Nutrition 0.000 claims description 11
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 235000011869 dried fruits Nutrition 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 6
- 235000005074 zinc chloride Nutrition 0.000 abstract description 5
- 239000011592 zinc chloride Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 244000060011 Cocos nucifera Species 0.000 description 46
- 235000013162 Cocos nucifera Nutrition 0.000 description 46
- 239000010903 husk Substances 0.000 description 44
- 238000006243 chemical reaction Methods 0.000 description 22
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 21
- 229960000907 methylthioninium chloride Drugs 0.000 description 21
- 238000002203 pretreatment Methods 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 14
- 238000009413 insulation Methods 0.000 description 14
- 230000007935 neutral effect Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 238000012216 screening Methods 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000003610 charcoal Substances 0.000 description 7
- 239000002023 wood Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000274 adsorptive effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 244000082204 Phyllostachys viridis Species 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000037452 priming Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 235000001122 chang geng bian tao Nutrition 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention provides a method for preparing nutshell activated carbon by a pyrolyzing activation technology and activated carbon. The method takes fragmented dry nutshells as raw materials, which are pyrolyzed under a pyrolysis temperature, and then pickled, washed, and dried so as to obtain activated carbon. Specifically, the raw materials are put in a ceramic pyrolysis reactor first, and the ceramic pyrolysis reactor is filled with air and sealed completely, then pyrolysis is carried out under a pyrolysis temperature of 700-1000DEG C for 1-10h. The prepared activated carbon has a specific surface area of 500-2300m<2>/g, a yield of 5-40%, and an iodine adsorption value of 470-1930mg/g. The one-step pyrolyzing activation method provided in the invention for preparing nutshell activated carbon with high adsorption performance needs no water vapor, phosphoric acid or zinc chloride and other activating agents. The prepared product has high yield and excellent adsorption performance. And the preparation technology is green, clean, and has short process as well as low cost.
Description
Technical field
The present invention relates to a kind of gac and preparation method thereof, especially relate to a kind of simple and convenient process for preparing of cleanliness without any pollution of gac of good adsorption performance.
Background technology
Preparation method of active carbon adopts chemical activation method and physical activation method usually at present, and chemical activation method need use chemical agents such as a large amount of phosphoric acid, zinc chloride, be prone to produce waste water and waste gas, and etching apparatus is serious; Physical activation method needs a large amount of high-temperature vapors or stack gas, and energy consumption is high, and the time is long, and the product yield is lower.Therefore, exploitation technology fast and convenient, energy-saving and cost-reducing, with low cost becomes the key of Preparation of Activated Carbon.
A meeting equality people of South China Science & Engineering University and Xiamen University (Zhang Huiping, Ye Liyi, Yang Lichun. phosphoric acid activation method prepares wood activated charcoal research [J]. chemistry of forest product and industry; 2004,24 (4): 49-52.) with phosphoric acid be acvator, the preparation wood activated charcoal; In scope of experiment; The impregnating ratio of selecting phosphoric acid activation method to produce wood activated charcoal is 100-150%, and activation temperature is about 500 ℃, and soak time 60-90min is more suitable.The specific surface area of the resulting gac of preparation reaches 1536m under optimum relatively experiment condition
2/ g.People such as the Li Bing of Northwest University (Li Bing, Li Yang, Xu Ningxia; Deng. zinc chloride activation method prepares amygdalus pedunculata pall gac [J]. Northwest University's journal (natural science edition) 2010; 40 (5) :) utilize zinc chloride activation method to prepare the flat walnut gac of long handle, in experiment condition, optimised process is 50% for the liquor zinci chloridi massfraction; Activation temperature is 600 ℃, and soak time is 90min.The specific surface area that can make gac is 1633.08 m
2/ g, its iodine sorption value are 883.78 mg/g, and methylene blue adsorption value is 165 mg/g.Chemical activation method prepares gac, owing to use a large amount of chemical reagent, equipment is produced certain corrosion, and environment is caused secondary pollution.
People such as the Wang Xiufang of South China Science & Engineering University (Wang Xiufang, Zhang Huiping, Chen Huan the admire preparation and the sign [J] of .KOH activation method high-specific surface area activated carbon from bamboo. functional materials, 2006, (4): 675-679.), utilize KOH to prepare active carbon with high specific surface area.They are raw material with the bamboo, and KOH is an acvator, in impregnating ratio 1.0, and 800 ℃ of soak time 2h of activation temperature, the specific surface area of resulting activated carbon product and pore volume can reach 2996m
2/ g and 1.64cm
3/ g.The gac added value of this method preparation is high, particularly has broad application prospects in the electrode materials field of double layer capacitor in adsorbing domain.But there are high, the problems such as etching apparatus is serious, subsequent disposal complicacy of production cost in this method.
People such as the Li Qin of Southeast China University (Li Qin, Jin Baosheng, Huang Yaji; Deng. steam activation prepares the experimental study [J] of biomass active charcoal. Southeast China University's journal, 2009,35 (9): 1008-1011.) with water vapour be acvator; With rice husk, corn cob, Pericarppium arachidis hypogaeae is raw material, the preparation gac.Result of study finds that corn cob is the material of the preparation gac of the best in 3 kinds of raw materials, and at 800 ℃ of following activation 90min, can obtain specific surface area is 924.48m
2The gac of/g.People such as Shi Zhiqiang (Shi Zhiqiang, Wang Chengyang, Du Yuan, etc. the preparation of alkyd resin based micropore charcoal and electric double layer capacitance characteristic [J]. University Of Tianjin's journal, 2007,40 (8): 911-915.) with resol be raw material, CO
2Be acvator, under the situation of nitrogen protection, be warming up to 700 ℃ of pyrolysis certain hours, change logical CO subsequently
2, and be warming up to 950 ℃ of activation 7h, and obtaining alkyd resin based micropore charcoal, this charcoal specific surface area can reach 2246m
2/ g.Physical activation method prepares gac, and active rate is low, and power consumption is high, and the product yield is low.
In sum, the common preparation method of gac exists the chemical reagent consumption big, and three-waste pollution is high, and energy consumption is high, and yield is low, and production cost is high, different problems such as complex process, and Development and Production technology is simple, and energy-saving and cost-reducing working method is particularly important.
Summary of the invention
In order to solve the acvators such as need water vapour, carbonic acid gas or high-temperature flue gas that existing gac physics method production technology exists; Shortcomings such as energy consumption is high, and the product yield is low, the present invention provides a kind of pyrolysis activation to prepare the method and the gac of active fruit shell carbon; Preparation technology is simply quick; The product yield is high, and cost is low, and absorption property is good.
Technical scheme of the present invention is: a kind of pyrolysis activation method prepares the method for active fruit shell carbon; With the dry shell after the fragmentation is that raw material carries out pyrolysis under pyrolysis temperature, and pyrolysis is after obtain gac after the pickling, washing, drying, and raw material places earlier in the ceramic pyrolysis reactor; With being full of air in the ceramic pyrolysis reactor; Airtight fully, and then under 700 ~ 1000 ℃ pyrolysis temperature pyrolysis 1 ~ 10h, the gac specific surface area 500-2300m of preparation
2/ g, yield 5-40%, iodine sorption value are 470-1930mg/g.
Dried fruit capsomere after the fragmentation directly is 0.85mm-22.0mm.
The volume of raw material accounts for 6.6 ~ 65.7% of ceramic pyrolysis reactor volume.
Temperature rise rate with 1 ℃ of-10 ℃/min is warming up to pyrolysis temperature.
The gac that the method that described pyrolysis activation method prepares active fruit shell carbon obtains, specific surface area 500-2300m
2/ g, yield 5-40%, iodine sorption value are 470-1930mg/g.
Beneficial effect
1. the pyrolysis activation prepares the high absorption property active fruit shell carbon, and cost is low, and technology is easy, and the product yield is high.
2. the pore texture of gac is flourishing, and absorption property is good.
3. the present invention adopts the airtight preparation gac of ceramic pyrolysis reactor, and the accumulation of heat of ceramic pyrolysis reactor is effective, and the inner raw material in back that heats up can self-activation, need not to add any acvators such as water vapour, phosphoric acid and zinc chloride, cleanliness without any pollution in the preparation process.
4. the used shell of the present invention can be coconut husk, oil tea shell, nut-shell etc., can turn waste into wealth.
5. the absorption property of gac of the present invention, specific surface area, pore volume can be passed through raw material reaction amount, raw material stoving temperature, raw material particle size, airtight pre-treatment, and the temperature rise rate in the pyrolytic process, pyrolysis temperature, pyrolysis time are controlled.
Description of drawings
Fig. 1 prepares the N2 adsorption desorption graphic representation of high absorption property cocoanut active charcoal for the pyrolysis activation method.
Fig. 2 prepares the BJH method pore size distribution curve figure of high absorption property cocoanut active charcoal for the pyrolysis activation method.
Fig. 3 prepares the H-K method micropore size scatter chart of high absorption property cocoanut active charcoal for direct pyrolysis activation method.
Fig. 4 is the figure that influences of pyrolysis temperature contrast table area.
Fig. 5 is the figure that influences of pyrolysis time contrast table area.
Fig. 6 is the figure that influences of temperature rise rate contrast table area.
Fig. 7 is the figure that influences of material quantity contrast table area.
Fig. 1 be 10g (13.15ml) coconut husk raw material in the 100ml pyrolysis reactor, the pyrolysis activation temperature is 1000 ℃, soaking time is 6h, the specific surface area figure of preparation gac gained.This adsorption isothermal line of Fig. 1 curve display is
type, shows that this gac is the microporous type sorbent material.Under extremely low relative pressure, the adsorptive capacity of sample sharply increases, and greater than 0.1 o'clock, adsorptive capacity reached capacity basically at relative pressure, and along with the increase of relative pressure, adsorptive capacity slightly increases, and is a platform basically.Fig. 2 and Fig. 3 are the graph of pore diameter distribution that calculates with BJH method and H-K method respectively.Fig. 2 and Fig. 3 show that this activated carbon capillary is flourishing, and atomic hole (aperture < 0.7 nm) distributes more concentrated, and peak value appears at 0.47 nm place.Middle macropore is less relatively.
Fig. 4～Fig. 7 is respectively the influence of different pyrolysis temperatures, pyrolysis time, temperature rise rate and raw material reaction amount contrast table area.As shown in the figure, along with the increase of pyrolysis temperature, the prolongation of pyrolysis time, the specific surface area of gac constantly increases; Improve temperature rise rate, the specific surface area of gac also increases; But the raw material reaction amount increases, and specific surface area reduces.This is because of the raising along with pyrolysis temperature, the prolongation of pyrolysis time, and raw material pyrolytic reaction and self-activation reaction are more abundant, and hole forms abundanter, shows that specific surface area increases.Temperature rise rate causes the heat transmission rapid fast, helps reaming.Along with the increase of raw material reaction amount, the raw material accumulating amount is big, and the pyrolysis priming reaction is restricted, and pyrolysis reactor inner air amount reduces the carrying out that also can influence priming reaction.
Embodiment
The present invention is following to the testing method of the absorption property of prepared active fruit shell carbon and specific surface area:
(1) mensuration of iodine sorption value and methylene blue adsorption value: sample carries out according to " wood activated charcoal TP " GB/T 12496. 8-1999 " mensuration of wood activated charcoal TP iodine sorption value " and GB/T 12496. 10-1999 " mensuration of wood activated charcoal TP methylene blue adsorption value " the adsorptive value detection of iodine and methylene blue.
(2) mensuration of specific surface area: utilize the mensuration of gac, according to the BET formula calculated specific surface area to nitrogen adsorption isotherm.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the ceramic pyrolysis reactor of 100ml, can adopt clay or other enclosed materials that the slit is shut.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 700 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 24.4% of gac, specific surface area 558m
2/ g, iodine sorption value are 767mg/g, and methylene blue adsorption value does<15mlg.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the ceramic pyrolysis reactor of 100ml, can adopt clay or other enclosed materials that the slit is shut.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 800 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 22.3% of gac, specific surface area 704m
2/ g, iodine sorption value are 892mg/g, and methylene blue adsorption value is 30ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 18.3% of gac, specific surface area 994m
2/ g, iodine sorption value are 1295mg/g, and methylene blue adsorption value is 135 ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 1000 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 18.0% of gac, specific surface area 1043m
2/ g, iodine sorption value are 1279mg/g, and methylene blue adsorption value is 195ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 2h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 24.1% of gac, specific surface area 718m
2/ g, iodine sorption value are 902mg/g, and methylene blue adsorption value is 60ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 6h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 11.8% of gac, specific surface area 1283m
2/ g, iodine sorption value are 1480mg/g, and methylene blue adsorption value is 375ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 8h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 9.41% of gac, specific surface area 1723m
2/ g, iodine sorption value are 1629mg/g, and methylene blue adsorption value is 375ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus; Temperature rise rate with 10 ℃/min is warming up to 1000 ℃ of pyrolysis temperatures; And insulation certain hour 6h, treat that pyrolysis finishes, and takes out sample; To neutral, be activated carbon sample through pickling, washing after the drying.The yield 11.9% of gac, specific surface area 1696m
2/ g, iodine sorption value are 1789mg/g, and methylene blue adsorption value is 345ml/g.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 2 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 25.9% of gac, specific surface area 747 m
2/ g, iodine sorption value are 921mg/g, and methylene blue adsorption value does<15mlg.Temperature rise rate slowly then makes the mitigation that the heat transmission is carried out, and pore-creating speed reduces, and the mesopore amount is lower than the micropore amount, show that directly methylene blue adsorption value is low on.
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 5 ℃/min, and insulation certain hour 6h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 22.5% of gac, specific surface area 883 m
2/ g, iodine sorption value are 1057mg/g, and methylene blue adsorption value is 60ml/g.
Embodiment 11
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 30g (39.45ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 25.9% of gac, specific surface area 603m
2/ g, iodine sorption value are 786mg/g, and methylene blue adsorption value is 15ml/g.
Embodiment 12
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 200ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 17.7% of gac, specific surface area 1175m
2/ g, iodine sorption value are 1314mg/g, and methylene blue adsorption value is 195ml/g.
Embodiment 13
(1) raw material crushing: with raw material crushing, 20-22mm is got in screening, in 120 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 23.0% of gac, specific surface area 912m
2/ g, iodine sorption value are 1097mg/g, and methylene blue adsorption value is 60ml/g.
Embodiment 14
(1) raw material crushing: with air-dry coconut husk raw material crushing, the 0.85-2.00mm particle is got in screening, in 180 ℃ of oven dry down.
(2) airtight pre-treatment before the reaction: 10g (13.15ml) coconut husk raw material is placed the pyrolysis reactor of 100ml, airtight.
(3) pyrolysis: the airtight pyrolysis reactor that the coconut husk raw material is housed is placed High Temperature Furnaces Heating Apparatus, be warming up to 900 ℃ of pyrolysis temperatures with the temperature rise rate of 10 ℃/min, and insulation certain hour 4h; Treat that pyrolysis finishes; Take out sample, to neutral, be activated carbon sample after the drying through pickling, washing.The yield 20.8% of gac, specific surface area 1209m
2/ g, iodine sorption value are 1374mg/g, and methylene blue adsorption value is 135ml/g.
Embodiment 15
Make the raw material among the embodiment 3 into the oil tea shell, all the other obtain the yield 23.0% of activated carbon sample, specific surface area 624m with embodiment 3
2/ g, iodine sorption value are 859mg/g, and methylene blue adsorption value is 157.5ml/g.
Embodiment 16
Make the raw material among the embodiment 3 into nut-shell, all the other obtain the yield 23.3% of activated carbon sample, specific surface area 718m with embodiment 3
2/ g, iodine sorption value are 864mg/g, and methylene blue adsorption value is 60ml/g.
Claims (5)
1. a pyrolysis activation method prepares the method for active fruit shell carbon, is that raw material carries out pyrolysis under pyrolysis temperature with the dry shell after the fragmentation, and pyrolysis is after obtain gac after the pickling, washing, drying; It is characterized in that; Raw material places earlier in the ceramic pyrolysis reactor, and is with being full of air in the ceramic pyrolysis reactor, airtight fully; And then under 700 ~ 1000 ℃ pyrolysis temperature pyrolysis 1 ~ 10h, the gac specific surface area 500-2300m of preparation
2/ g, yield 5-40%, iodine sorption value are 470-1930mg/g.
2. pyrolysis activation method as claimed in claim 1 prepares the method for active fruit shell carbon, it is characterized in that, the dried fruit capsomere after the pulverizing directly is 0.85mm-22.0mm.
3.. pyrolysis activation method as claimed in claim 1 prepares the method for active fruit shell carbon, it is characterized in that, the volume of raw material accounts for 6.6 ~ 65.7% of ceramic pyrolysis reactor volume.
4. pyrolysis activation method as claimed in claim 1 prepares the method for active fruit shell carbon, it is characterized in that, is warming up to pyrolysis temperature with the temperature rise rate of 1 ℃ of-10 ℃/min.
5. the gac that obtains of the described pyrolysis activation method of claim 1 ~ 4 method for preparing active fruit shell carbon is characterized in that specific surface area 500-2300m
2/ g, yield 5-40%, iodine sorption value are 470-1930mg/g
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