CN102275911A - Microporous active carbon and preparation method by chemical agent aperture regulation and control - Google Patents
Microporous active carbon and preparation method by chemical agent aperture regulation and control Download PDFInfo
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Abstract
The invention provides a microporous active carbon preparation method by chemical aperture regulation and control. First, a fruit casing is dried and mixed with a chemical agent diluted solution according to a low dipping ratio; the fruit casing is fully dipped and dried at a certain temperature. A mixture is slowly heated to an activation temperature under an inert atmosphere and insulted for a while; after the activation, the mixture is cooled and treated with washing, pickling, washing and drying to obtain a microporous normal distribution concentrated fruit casing base active carbon. The invention has advantages of low dipping ratio, small usage amount of chemical agent, low activation temperature and high product rate, so as to realize low coasts and a simple preparation technology. Meanwhile, the prepared active carbon has greatly concentrated and adjustable microporous apertures and significant added value, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of microporous type absorbent charcoal material and preparation method thereof, be specifically related to the low consumed short-cut method that chemical method regulation and control aperture prepares shell base microporous type gac.
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Background technology
Wood activated charcoal is owing to the feature of its raw material, and conventional activation back aperture distributes than dispersion.In the gac professional purpose, the molecular sieve type gac that micropore size distributes and concentrates, high efficiency has huge potential application prospect at aspects such as super capacitor material, lithium ion battery, blood purifications, is the research focus of current advanced raw material of wood-charcoal material.
Present chemical method generally is that the phosphoric acid that adopts is activator phosphorus wood than generally about 4:1, macroporous type gac during 600 ℃ of activation about 1 hour prepare.But the microporous type gac generally then more adopts the activation of physics method to prepare if will prepare, with the physics method---and water vapour, CO
2Be restructured as the master with high temperature, do not see the method report of chemical agent activation regulation and control micropore size as yet.But physics method yield of activation is low general many below 10%, and temperature required height is many more than 1000 ℃, so raw material and energy consumption height.Simultaneously, under high temperature like this, aperture size is difficult to control.Therefore, it is low to explore resources and energy consumption, and the technology of aperture easy-regulating becomes the difficult problem that aperture control prepares the micropore gac.
People such as the Yang Kunbin of Kunming University of Science and Technology (Yang Kunbin, Peng Jinhui, Zhang Libo, Deng. the steam activation legal system is equipped with the pore structure feature [J] of cocoanut active charcoal. the charcoal element, 2010,1: 8-13. Yang Kun is refined, Peng Jinhui, full in summer should, Deng. CO2 activation preparation coconut husk matrix activated carbon [J]. charcoal element, 2010,1: 20-23.) with the coconut husk be raw material, be activator with water vapour and carbonic acid gas respectively, prepare the gac of micropore prosperity.When water vapour consumption and carbonic acid gas consumption are comparatively suitable, in condition and range, improve activation temperature and prolong soak time, help the formation of micropore, but along with the raising of activation temperature and the prolongation of soak time, yield reduces constantly.The yield that physical activation method prepares gac low (below 10%), and temperature required height (more than 900 ℃) are so raw material and energy consumption height.Simultaneously, at high temperature, aperture size is difficult to control.
People such as the Liu Junli of China Forests Science Academe Forests Chemical Industry Research Institute (Liu Junli, Gu Kelong. pyroprocessing is to the influence [J] of activated carbon pore structure. chemistry of forest product and industry, 1999,19 (3): 37-40.) with starch be raw material, metal hydroxides is an activator, at 800~900 ℃ of activation 2h, the raw material gac that obtains obtains final gac at 1100 ℃ of oxygen barrier thermal treatment 4h.The average pore radius of gained gac is reduced to 1.5 nm by 2.5 nm.Utilizing high temperature to reform is a kind of method of adjusting micropore, but the temperature of reaction height, power consumption is big, and the time is long, the cost height, the industrialization difficulty is bigger.
People such as the Ma Rong of China Mining University (Ma Rong, Zhang Lifang, Zhang Shuanquan, Deng. Taixi anthracite prepares the experimental study [J] of micropore gac. novel charcoal material, 2004,19 (1): 57-61.) studied the test conditions that under nitrate and two kinds of additive effects of potassium-containing compound, prepares the micropore gac with Taixi anthracite.Drawn the optimum level combination: the mass ratio of additive nitrate and potassium-containing compound is 2:1,5 ℃/min of charing heat-up rate, 920 ℃ of activation temperatures, soak time 3.5 h.Discover, it is that the gac that 6% additive makes all is being greatly improved aspect micropore pore volume and the total pore volume that the same terms adds down massfraction: the micropore pore volume is from 0.1847 ml/g height to 0.3299 ml/g, and always pore volume is brought up to 0.5128 ml/g from 0.2186 ml/g.The catalyzer difference that the utilization of catalysis aperture control method is added, soak time and temperature different can be regulated and control out the gac of special pore size distribution.But inevitably can the lingering section metallic element in the micropore gac that the catalytic activation method makes, when this gac is used for liquid phase adsorption, metallic element may enter solution with ionic species, bring secondary pollution, especially but very harmful in the purification of food, tap water and medicine is used.Although can reduce metal content by acid-alkali washing, brought environmental pollutions such as waste water, waste gas simultaneously, complicated operation, cost increases.
People such as Kyotani (the T KYOTANI of reaction Science Institute of northeastern Japan university, T NAGA I, S I NOU E.Formation o f new type of porous carbon by carbonization in zeolite Nanochannels[J] .Chem Mater, 1997,9 (2): be carbon source 609-6l5.) with vinyl cyanide (AC) and furfuryl alcohol (FA), zeolite is prepared the micropore charcoal with three-dimensional regular structure as template.The disadvantage of utilizing template to prepare gac is the removal of template, has increased high expense.This kind method cost height is unfavorable for suitability for industrialized production.
In sum, adopt physics method and catalysis method regulation activity charcoal micropore to distribute usually, too high but shortcoming is an activation temperature, yield is too low, and actual application value is little; It is high that high temperature transfers the hole that temperature of reaction is required, and increased energy requirement, the distribution in wayward aperture under the high temperature; The gac meeting remnant metal ion of hole preparation is transferred in catalysis, and is unfavorable to some liquid phase adsorption; Template is adjusted micropore has increased great amount of cost when processing template.Therefore, it is low to explore resources and energy consumption, and the technology of aperture easy-regulating becomes the difficult problem that aperture control prepares the micropore gac.
Summary of the invention
In order to solve the cost of manufacture height that prior art exists, the product yield is low, the nonadjustable shortcoming in aperture, the invention provides a kind of chemical method aperture control and prepare the microporous type process of active carbon, the preparation method is simply quick, product yield height, cost is low, and micropore distributes and concentrates, and micropore size is controlled.
Technical scheme of the present invention is: a kind of chemical agent aperture control prepares the microporous type process of active carbon, comprises the steps:
The first step, the shell screening: with the shell oven dry, fragmentation, sieving out particle diameter is the shell particle of 0.6mm-1.0mm;
Second step, the lower concentration dip treating of chemical agent: the mass ratio according to shell particle and pure chemistry medicament is (0.2~0.6): 1 ratio, and the shell particle flooded in the chemical agent solution of mass concentration 5 ~ 60% be dried to the moisture evaporate to dryness more than 24 hours again and obtain chemical agent shell mixture;
In the 3rd step, low-temperature activation: exsiccant chemical agent shell mixture temperature rise rate with 1 ℃~10 ℃/min under nitrogen atmosphere is warming up to warm 350 ℃ eventually of activation by 200 ℃, and constant temperature activated in 4~5 hours then, after activation is finished, cooling, washing, dry the flourishing activated carbon product of micropore; The microporosity 60~90% of micropore gac, specific surface area 50~2700m
2/ g, yield 30~50%, iodine sorption value is 245~2050mg/g, methylene blue adsorption value is 45~90mL/g.
The flow velocity of nitrogen: 0.5L~4L/min.
Described chemical agent is any one in potassium hydroxide, phosphoric acid or the zinc chloride.
Drying temperature in the 3rd step is 30~200 ℃.
Described shell is arbitrary in oil tea shell, coconut husk, the apricot shell.
The chemical agent aperture control prepares the flourishing active fruit shell carbon of micropore of microporous type process of active carbon preparation, and grain graininess is even, and particle diameter is 0.6~1.0mm, the microporosity 60~90% of micropore gac, specific surface area 50~2700m
2/ g, yield 30~50%, iodine sorption value is 245~2050mg/g, methylene blue adsorption value is 45~90mL/g.
Beneficial effect:
1. adopt chemical activation method to produce the microporous type gac, the yield of product is much higher than physics method that tradition adopts brings up to 30 ~ 50% by original 10%, and chemical agent is reduced to (0.2~0.6) than the addition of the 4:1 of common chemical method: 1, significantly reduced the usage quantity of activator.Activation temperature also is reduced to present be no more than 350 ℃ by about 600 ℃ of chemical method, about 1000 ℃ high temperature of physics method, has saved the energy.And technology is simple, and cost is low, is convenient to industrializing implementation.
2. the micropore of the gac for preparing is very flourishing, and normal distribution is concentrated, and microporosity reaches 60~90%, mean pore size 1.6nm, specific surface area 1500~2700m
2/ g, yield 30 ~ 60%, iodine sorption value is 245~2050mg/g, methylene blue adsorption value is 45~90mL/g.
3. the pore size of gac of the present invention, micropore distribution, specific surface area, pore volume can be passed through chemical agent H
3PO
4, ZnCl
2The addition of the aqueous solution, the temperature rise rate in the reactivation process, activation temperature, soak time are controlled.
Description of drawings
Fig. 1 phosphoric acid method aperture control micropore gac pore size distribution curve.
The N of Fig. 2 phosphoric acid method aperture control micropore gac
2Adsorption curve.
Fig. 3 chemical method aperture control prepares the surface topography of microporous type gac.
Fig. 4 temperature rise rate is to the influence of microporosity.
Fig. 5 activation temperature is to the influence of microporosity.
Fig. 6 phosphoric acid addition is to the influence of microporosity.
Fig. 7 zinc chloride addition is to the influence of microporosity.
The pore size distribution of the different impregnating ratio gacs of Fig. 8.
The sorption isotherm of the different impregnating ratio gacs of Fig. 9.
Figure 10 chemical method aperture control prepares the surface topography of microporous type gac.
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Embodiment
The chemical method aperture control prepares the microporous type process of active carbon, comprises the steps:
The first step, shell screening: with the shell oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
Second step, the lower concentration dip treating of chemical agent: with dense chemical agent be configured to mass concentration be 5-60% than dilute solution, mixes with the shell particle, flood more than 24 hours, be dried to the moisture evaporate to dryness again.Chemical agent solution, the mass ratio of shell particle and chemical agent are (0.1~1): 2 ~ 3, and drying temperature can adopt 30 ℃~200 ℃ conventional dryings.
The 3rd step: low-temperature activation: exsiccant chemical agent shell mixture is warming up to eventually temperature of activation with certain temperature rise rate under nitrogen atmosphere, after activation is finished, gets the flourishing activated carbon product of micropore through steps such as the cooling of routine, washing, oven dry.The flow velocity of nitrogen gas: 0.5L~4L/min, 1 ℃ of-10 ℃/min of heat-up rate; During activation, temperature is warming up to warm 500 ℃ eventually of activation by 200, and constant temperature activated in 0.1~5 hour then.The microporosity 40-100% of micropore gac, specific surface area 50~2700m
2/ g, yield 30-60%, iodine sorption value are 245~2050mg/g, methylene blue adsorption value is 45~90mL/g.
The shell that adopts in the method for the present invention can comprise air-dry samples such as oil tea shell, coconut husk, apricot shell, and grain diameter is 0.6~1.0mm.Chemical agent is potassium hydroxide, phosphoric acid, water or wherein several arbitrarily arbitrarily than mixture, perhaps is zinc chloride.The preparation of chemical agent solution can be adopted zinc chloride: the mass ratio of water is 5%~60% ratio, or phosphoric acid: the mass ratio of water is 5%~60% ratio, or potassium hydroxide aqueous solution.The mass ratio of shell and pure chemistry medicament can adopt (0.1~1): 3, and the drying temperature scope of shell and chemical mixtures material is at 30 ℃~200 ℃, and to the moisture evaporate to dryness, chemical agent fully is impregnated into material.
The pore size of gac of the present invention, micropore distribution, specific surface area, pore volume can be passed through chemical agent H
3PO
4, ZnCl
2Deng the addition of the aqueous solution, the temperature rise rate in the reactivation process, activation temperature, soak time are controlled.Activate by lower temperature: exsiccant chemical agent shell mixture is warming up to activation temperature eventually with certain temperature rise rate under inert atmosphere.After activation is finished, cooling, washing, dry the flourishing activated carbon product of micropore.Activation test-results such as Fig. 4-shown in Figure 7.
The present invention is as follows to the testing method that prepared chemical agent aperture control prepares the specific surface area of microporous type gac and absorption property:
The mensuration of (1) micropore distribution, specific surface area, pore volume: gac is to the mensuration of nitrogen adsorption isotherm, according to the BET formula calculated specific surface area under the employing liquid nitrogen condition.
(2) surface topography adopts the S-4800 type awkward silence at a meeting photo-emission electron microscopy observation of FDAC (Hitachi) company.
(3) mensuration of iodine sorption value and methylene blue adsorption value: the mensuration of iodine sorption value is carried out according to GB/T 12496.8-1999 " mensuration of wood activated charcoal test method iodine sorption value "; The mensuration of methylene blue adsorption value is carried out according to GB/T 12496.9-1999 " mensuration of wood activated charcoal test method methylene blue adsorption value ".
(1) shell screening: with the coconut husk oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
(2) the lower concentration dip treating of chemical agent: it is 20% solution that zinc chloride is mixed with mass concentration, mixes according to mass ratio 0.2:1 with coconut husk according to pure zinc chloride, floods 24 hours, dry down at 100 ℃.
(3) low-temperature activation: exsiccant zinc chloride coconut husk mixture is warming up to 400 ℃ with 5 ℃/min under nitrogen atmosphere, keeps 60mins, the activation finish after, the cooling, the washing, dry activated carbon sample.The microporosity 80% of gac, specific surface area 370m
2/ g, yield 60%, iodine sorption value is 355mg/g, methylene blue adsorption value is 30ml/g.
Embodiment 2
(1) shell screening: with the coconut husk oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
(2) the lower concentration dip treating of chemical agent: it is 20% solution that zinc chloride is mixed with mass concentration, mixes according to mass ratio 0.4:1 with coconut husk, floods 24 hours, dry down at 100 ℃.
(3) low-temperature activation: exsiccant zinc chloride coconut husk mixture is warming up to 400 ℃ with 5 ℃/min under nitrogen atmosphere, keeps 60mins, the activation finish after, the cooling, the washing, dry activated carbon sample.The microporosity 75% of gac, specific surface area 670m
2/ g, yield 54%, iodine sorption value is 455mg/g, methylene blue adsorption value is 50ml/g.
Embodiment 3
(1) shell screening: with the coconut husk oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
(2) the lower concentration dip treating of chemical agent: it is 20% solution that zinc chloride is mixed with mass concentration, mixes according to mass ratio 0.6:1 with coconut husk, floods 24 hours, dry down at 100 ℃.
(3) low-temperature activation: exsiccant zinc chloride coconut husk mixture is warming up to 400 ℃ with 5 ℃/min under nitrogen atmosphere, keeps 60mins, the activation finish after, the cooling, the washing, dry activated carbon sample.The microporosity 90% of gac, specific surface area 770m
2/ g, yield 47%, iodine sorption value is 655mg/g, methylene blue adsorption value is 60ml/g.
Embodiment 4
(1) shell screening: with the coconut husk oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
(2) the lower concentration dip treating of chemical agent: it is 20% solution that zinc chloride is mixed with mass concentration, mixes according to mass ratio 0.6:1 with coconut husk, floods 24 hours, dry down at 100 ℃.
(3) low-temperature activation: exsiccant zinc chloride coconut husk mixture is warming up to 400 ℃ with 3 ℃/min under nitrogen atmosphere, keeps 60mins, the activation finish after, the cooling, the washing, dry activated carbon sample.The microporosity 95% of gac, specific surface area 1070m2/g, yield 52%, iodine sorption value is 1055mg/g, methylene blue adsorption value is 80ml/g.
Embodiment 5
(1) shell screening: with the coconut husk oven dry, the particle of 0.6mm-1.0mm is sieved out in fragmentation.
(2) the lower concentration dip treating of chemical agent: it is 20% solution that zinc chloride is mixed with mass concentration, mixes according to mass ratio 0.6:1 with coconut husk, floods 24 hours, dry down at 100 ℃.
(3) low-temperature activation: exsiccant zinc chloride coconut husk mixture is warming up to 350 ℃ with 3 ℃/min under nitrogen atmosphere, keeps 60mins, the activation finish after, the cooling, the washing, dry activated carbon sample.The microporosity 95% of gac, specific surface area 1150m
2/ g, yield 54%, iodine sorption value is 1174mg/g, methylene blue adsorption value is 70ml/g.
Embodiment 6
Change the chemical agent among the embodiment 5 into phosphoric acid, all the other obtain the microporosity 96% of activated carbon sample, specific surface area 1168m with embodiment 5
2/ g, yield 53%, iodine sorption value is 1201mg/g, methylene blue adsorption value is 70ml/g.
Embodiment 7
Change the drying temperature among the embodiment 5 into 80 ℃, all the other obtain the microporosity 96% of activated carbon sample, specific surface area 1210m with embodiment 5
2/ g, yield 54%, iodine sorption value is 1274mg/g, methylene blue adsorption value is 60ml/g.
Embodiment 8
Make the raw material among the embodiment 7 into the oil tea shell, all the other obtain the microporosity 91% of gac, specific surface area 1050m with embodiment 7
2/ g, yield 51%, iodine sorption value is 974mg/g, methylene blue adsorption value is 90ml/g.
Embodiment 9
Make the raw material among the embodiment 7 into the apricot shell, all the other obtain the microporosity 92% of gac, specific surface area 1047m with embodiment 7
2/ g, yield 52%, iodine sorption value is 874mg/g, methylene blue adsorption value is 80ml/g.
Claims (6)
1. a chemical agent aperture control prepares the microporous type process of active carbon, it is characterized in that, comprises the steps:
The first step, the shell screening: with the shell oven dry, fragmentation, sieving out particle diameter is the shell particle of 0.6mm-1.0mm;
Second step, the lower concentration dip treating of chemical agent: the mass ratio according to shell particle and pure chemistry medicament is (0.2~0.6): 1 ratio, and the shell particle flooded in the chemical agent solution of mass concentration 5 ~ 60% be dried to the moisture evaporate to dryness more than 24 hours again and obtain chemical agent shell mixture;
In the 3rd step, low-temperature activation: exsiccant chemical agent shell mixture temperature rise rate with 1 ℃~10 ℃/min under nitrogen atmosphere is warming up to warm 350 ℃ eventually of activation by 200 ℃, and constant temperature activated in 4~5 hours then, after activation is finished, cooling, washing, dry the flourishing activated carbon product of micropore; The microporosity 60~90% of micropore gac, specific surface area 50~2700m
2/ g, yield 30~50%, iodine sorption value is 245~2050mg/g, methylene blue adsorption value is 45~90mL/g.
2. chemical agent aperture control as claimed in claim 1 prepares the microporous type process of active carbon, it is characterized in that the flow velocity of nitrogen: 0.5L~4L/min.
3. chemical agent aperture control as claimed in claim 1 prepares the microporous type process of active carbon, it is characterized in that, described chemical agent is any one in potassium hydroxide, phosphoric acid or the zinc chloride.
4. chemical agent aperture control as claimed in claim 1 prepares the microporous type process of active carbon, it is characterized in that, the drying temperature in the 3rd step is 30~200 ℃.
5. chemical agent aperture control as claimed in claim 1 prepares the microporous type process of active carbon, it is characterized in that, described shell is arbitrary in oil tea shell, coconut husk, the apricot shell.
6. the flourishing active fruit shell carbon of micropore for preparing the preparation of microporous type process of active carbon as the arbitrary described chemical agent aperture control of claim 1~5, it is characterized in that grain graininess is even, particle diameter is 0.6~1.0mm, the microporosity 60~90% of micropore gac, specific surface area 50~2700m
2/ g, yield 30~50%, iodine sorption value is 245~2050mg/g, methylene blue adsorption value is 45~90ml/g.
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