CN105236405B - A kind of convenient preparation method of biomass-based nitrating activated carbon - Google Patents

A kind of convenient preparation method of biomass-based nitrating activated carbon Download PDF

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CN105236405B
CN105236405B CN201510576495.7A CN201510576495A CN105236405B CN 105236405 B CN105236405 B CN 105236405B CN 201510576495 A CN201510576495 A CN 201510576495A CN 105236405 B CN105236405 B CN 105236405B
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activated carbon
biomass
preparation
nitrating activated
bean dregs
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CN105236405A (en
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李大伟
田原宇
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The present invention relates to the convenient preparation method of a kind of biomass-based nitrating activated carbon.Its technical scheme is to comprise the following steps: first use dry method uniformly to mix with bean dregs by the mass ratio of 1.2 ~ 3.0:1 potassium carbonate; press bean dregs quality again 5% 50% add ammonium hydrogen carbonate; uniformly mix; again by mixture under noble gas is protected; it is heated to activation temperature with the heating rate of 7 20 DEG C/min; insulation, finally carries out cooling down, washing to neutral, dry, prepares nitrating activated carbon.The invention has the beneficial effects as follows: 1) manufacturing cycle is shorter, and technique is simple, and energy consumption is little, it is not necessary to the most first raw material is carried out carbonization, it is not necessary to be dried the carbon precursor containing activator, and can use higher heating rate;2) gained activated carbon contains abundant nitrogen element and bigger specific surface area;3) without using the extremely strong caustic soda of alkalescence and caustic potash in preparation process, the corrosion to equipment is significantly reduced.

Description

A kind of convenient preparation method of biomass-based nitrating activated carbon
Technical field
The present invention relates to technical field of active carbon, particularly to the convenient preparation side of a kind of biomass-based nitrating activated carbon Method.
Background technology
Nitrating activated carbon because having the surface chemical property of uniqueness and flourishing pore structure, gas absorption, electrochemistry, Greater advantage is occupied in the fields such as catalysis.The common preparation method of nitrating activated carbon has: template, post treatment method, carbonization/activation contain Nitrogen carbon matrix precursor method.In recent years, with nitrogenous biomass as carbon precursor, use carbonization/activation method to prepare nitrating activated carbon, be subject to More concern.
Such as, (the Sustainable and hierarchical porous such as Zhanquan Zhang Enteromorpha prolifera based carbon for CO2 capture, Journal of Hazardous Materials, 2012) with Entermorpha as raw material, through hydro-thermal carbonization, KOH activation, having prepared nitrogen content is 2.6wt%, specific surface area For 418m2The activated carbon of/g.(the Superior carbon-based CO such as Song Jian2 adsorbents prepared From poplar anthers, Carbon, 2014) with Poplar anthers as raw material, through conventional carbonization, KOH activation, prepare nitrogen Content is 1.26wt%, specific surface area is 3322m2The activated carbon of/g.(preparation of Semen Glycines slag base porous charcoal and the superelevation thereof such as Zhu Bo The research of electric capacity, Shandong Technology Univ's journal (natural science edition), 2014) utilize bean dregs and KOH, prepare N doping activity Charcoal.
The studies above is that the preparation of nitrating activated carbon provides invaluable experience.But, the method using these research reports, Need the most first raw material to be carried out carbonization, need the mixture of carbon precursor and alkali liquor is dried for a long time, Or need to use relatively low heating rate (≤5 DEG C/min), the manufacturing cycle causing nitrating activated carbon is long, and technique is loaded down with trivial details, or energy Consumption is big.
Summary of the invention
The purpose of the present invention is aiming at the drawbacks described above that prior art exists, it is provided that a kind of manufacturing cycle is shorter, technique The convenient preparation method of simple biomass-based nitrating activated carbon.
Its technical scheme is to comprise the following steps: first by the mass ratio of 1.2 ~ 3.0:1, potassium carbonate is used dry method with bean dregs Uniformly mix, then be not more than 1.5mm ammonium hydrogen carbonate by the 5%-50% interpolation particle diameter of bean dregs quality, uniformly mix, then By mixture under noble gas is protected, it is heated to activation temperature with the heating rate of 7-20 DEG C/min, is incubated 65-100 min, finally Carry out cooling down, washing to neutral, dry, prepare nitrating activated carbon.
The particle diameter of above-mentioned bean dregs is 0.1-3.0mm, and moisture is not higher than 7%.
Above-mentioned potassium carbonate is powdery, and the largest particles particle diameter is less than 1.0 mm.
Above-mentioned dry method, refers to mix potassium carbonate powder with biomass, is not the potassium carbonate using and being dissolved in water or alcohol.
Above-mentioned is uniform, refers to the mixture being stirred continuously potassium carbonate powder with biomass, until the most uniform.
Above-mentioned activation temperature is 570-750 DEG C.
Above-mentioned washing, refers to that the pH value washed to washing liquid is 7.0-8.0.
Above-mentioned cooling, refers to naturally cool under nitrogen protection under 100 DEG C.
Above-mentioned is dried, and refers on 110 DEG C of forced air drying 10h.
Compared with the technology of preparing of existing biomass-based nitrating activated carbon, the invention have the advantage that
1) manufacturing cycle is shorter, and technique is simple, and energy consumption is little, it is not necessary to the most first raw material is carried out carbonization, it is not necessary to right Carbon precursor containing activator is dried, and can use higher heating rate;2) gained activated carbon contains abundant nitrogen Element (nitrogen content is 1.0wt% ~ 8.0wt%) and bigger specific surface area (500m2/g~1800m2/ g);3) nothing in preparation process The extremely strong caustic soda of alkalescence and caustic potash need to be used, significantly reduce the corrosion to equipment.
Detailed description of the invention
Below in conjunction with example, the invention will be further described, but is not used in the restriction present invention:
Embodiment 1
The potassium carbonate that particle diameter is less than 0.5mm is the bean dregs of 0.2-0.9mm with particle diameter, mixes by the mass ratio of 2:1, then presses 5% addition particle diameter of bean dregs quality is the ammonium hydrogen carbonate of 0.1-1.5mm, stirs.By mixture under nitrogen protection, with 7 DEG C/heating rate of min is heated to 570 DEG C, is incubated 100min.Then, it is cooled under nitrogen protection 80 DEG C, and spends Ionized water cyclic washing, until the pH value of washing liquid is 8.0.Finally, by sample in 110 DEG C of forced air drying 15h.Gained nitrating activity The specific surface area of charcoal is 980m2/ g, nitrogen content is 4.2wt%.
Embodiment 2
The potassium carbonate that particle diameter is less than 0.3mm is the bean dregs of 0.2-0.9mm with particle diameter, mixes by the mass ratio of 1.5:1, then By the ammonium hydrogen carbonate of 50% addition 0.2-1.2mm of bean dregs quality, stir.By mixture under nitrogen protection, with 12 DEG C/ The heating rate of min is heated to 600 DEG C, is incubated 70min.Then, it is cooled under nitrogen protection 60 DEG C, and uses deionization Water cyclic washing, until the pH value weakly acidic pH of washing liquid.Finally, by sample in 110 DEG C of forced air drying 12h.Gained nitrating activated carbon Specific surface area be 830m2/ g, nitrogen content is 5.2wt%.
Embodiment 3
The potassium carbonate that particle diameter is less than 0.1mm is the bean dregs of 0.3-1.0mm with particle diameter, mixes by the mass ratio of 1.8:1, then By the ammonium hydrogen carbonate of 25% addition 0.5-1.5mm of bean dregs quality, stir.By mixture under nitrogen protection, with 15 DEG C/ The heating rate of min is heated to 650 DEG C, is incubated 50min.Then, it is cooled under nitrogen protection 70 DEG C, and uses deionization Water cyclic washing, until the pH value weakly acidic pH of washing liquid.Finally, by sample in 110 DEG C of forced air drying 12h.Gained nitrating activated carbon Specific surface area be 1080m2/ g, nitrogen content is 3.7wt%.
Embodiment 4
The potassium carbonate that particle diameter is less than 1.0mm is the bean dregs of 0.1-3.0mm with particle diameter, mixes by the mass ratio of 3:1, then presses The ammonium hydrogen carbonate of 32% addition 0.05-0.9mm of bean dregs quality, stirs.By mixture under nitrogen protection, with 20 DEG C/ The heating rate of min is heated to 750 DEG C, is incubated 65min.Then, it is cooled under nitrogen protection 80 DEG C, and uses deionization Water cyclic washing, until the pH value weakly acidic pH of washing liquid.Finally, by sample in 110 DEG C of forced air drying 12h.Gained nitrating activated carbon Specific surface area be 1180m2/ g, nitrogen content is 3.2wt%.
The above, be only the part preferred embodiment of the present invention, and any those of ordinary skill in the art all may profit Revised or be revised as the technical scheme of equivalent by the technical scheme of above-mentioned elaboration.Therefore, according to the technology of the present invention Any simple modification that scheme is carried out or substitute equivalents, belong to the greatest extent the scope of protection of present invention.

Claims (9)

1. a preparation method for biomass-based nitrating activated carbon, is characterized in that comprising the following steps:
First use dry method uniformly to mix with bean dregs by the mass ratio of 1.2 ~ 3.0:1 potassium carbonate, then press the 5%-of bean dregs quality 50% adds the ammonium hydrogen carbonate that particle diameter is not more than 1.5mm, uniformly mixes, then by mixture under noble gas is protected, with 7-20 DEG C/heating rate of min is heated to activation temperature, is incubated 65-100 min, finally carry out cooling down, wash to neutral, be dried, system Obtain nitrating activated carbon.
The preparation method of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: the grain of described bean dregs Footpath is 0.1-3.0mm, and moisture is not higher than 7%.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described carbonic acid Potassium is powdery, and the largest particles particle diameter is less than 1.0 mm.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described is dry Method, refers to mix potassium carbonate powder with biomass, is not the potassium carbonate using and being dissolved in water or alcohol.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described is equal Even, refer to the mixture being stirred continuously potassium carbonate powder with biomass, until the most uniform.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described activation Temperature is 570-750 DEG C.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described washes Wash, refer to that the pH value washed to washing liquid is 7.0-8.0.
The preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described cooling Refer to naturally cool under nitrogen protection under 100 DEG C.
The convenient preparation method of a kind of biomass-based nitrating activated carbon the most according to claim 1, is characterized in that: described It is dried and refers on 110 DEG C of forced air drying 10h.
CN201510576495.7A 2015-09-11 2015-09-11 A kind of convenient preparation method of biomass-based nitrating activated carbon Expired - Fee Related CN105236405B (en)

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CN105921106A (en) * 2016-05-17 2016-09-07 南京正森环保科技有限公司 Surface nitrogen-rich activated carbon and preparation method and application thereof
CN106179440B (en) * 2016-06-24 2019-01-04 浙江大学 N doping multi-stage porous charcoal and its preparation method and application
CN106115698B (en) * 2016-06-24 2018-05-15 浙江大学 A kind of method for preparing nitrogenous porous charcoal using the useless charcoal of recycling and products thereof and application
CN106219539A (en) * 2016-07-25 2016-12-14 句容市百诚活性炭有限公司 A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon
CN106865547A (en) * 2017-04-06 2017-06-20 合肥工业大学 A kind of preparation method of plastic biologic activated carbon and its activated carbon of acquisition
CN108940191B (en) * 2018-06-05 2021-05-11 西北农林科技大学 Sulfur-nitrogen doped porous biochar, and preparation method and application thereof
CN110467180A (en) * 2019-07-16 2019-11-19 江苏大学 A kind of preparation method of the biomass derived Carbon Materials for sodium-ion battery
CN111186837A (en) * 2020-01-07 2020-05-22 南京林业大学 Preparation method of special nitrogen-doped formed activated carbon for catalyst carrier

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JP2003034518A (en) * 2001-07-19 2003-02-07 Noriyuki Yamazaki Activated carbon and method for manufacturing it
CN1465521A (en) * 2002-07-01 2004-01-07 金车股份有限公司 Method for making active carbon utilizing coffee bean dregs
CN103030710A (en) * 2013-01-05 2013-04-10 广西大学 Resource utilization method of camellia oleifera shells
CN104386685A (en) * 2014-10-22 2015-03-04 北京化工大学 Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material

Patent Citations (4)

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JP2003034518A (en) * 2001-07-19 2003-02-07 Noriyuki Yamazaki Activated carbon and method for manufacturing it
CN1465521A (en) * 2002-07-01 2004-01-07 金车股份有限公司 Method for making active carbon utilizing coffee bean dregs
CN103030710A (en) * 2013-01-05 2013-04-10 广西大学 Resource utilization method of camellia oleifera shells
CN104386685A (en) * 2014-10-22 2015-03-04 北京化工大学 Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material

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