CN105236405A - Convenient biomass-based nitrogen-doped active carbon preparation method - Google Patents
Convenient biomass-based nitrogen-doped active carbon preparation method Download PDFInfo
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- CN105236405A CN105236405A CN201510576495.7A CN201510576495A CN105236405A CN 105236405 A CN105236405 A CN 105236405A CN 201510576495 A CN201510576495 A CN 201510576495A CN 105236405 A CN105236405 A CN 105236405A
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Abstract
The present invention relates to a convenient biomass-based nitrogen-doped active carbon preparation method. The technical scheme comprises: uniformly mixing potassium carbonate and bean residue according to a mass ratio of 1.2-3.0:1 by using a dry method, adding ammonium bicarbonate having the amount of 5-50% of the mass of the bean residue, uniformly mixing, heating the mixture under an inert gas at a heating rate of 7-20 DEG C/min to achieve an activation temperature, carrying out thermal insulation, cooling, washing to achieve a neutral state, and drying to obtain the nitrogen-doped active carbon. The method of the present invention has the following beneficial effects that: 1) the preparation cycle is short, the process is simple, the energy consumption is low, the activating agent-containing precursor is not required to be dried, and the high heating rate can be adopted; 2) the obtained active carbon is rich in nitrogen and has large specific surface area; and 3) during the preparation process, the strong alkality caustic soda and the strong alkality caustic potash are not required, such that the corrosion on the equipment is substantially reduced.
Description
Technical field
The present invention relates to technical field of active carbon, particularly a kind of convenient preparation method of biomass-based nitrating gac.
Background technology
Nitrating gac, because having unique surface chemical property and flourishing pore texture, occupies greater advantage in fields such as gas adsorption, electrochemistry, catalysis.The common preparation method of nitrating gac has: template, post treatment method, charing/activate nitrogenous carbon matrix precursor method.In recent years, with nitrogenous biomass for carbon precursor, adopt charing/activation method to prepare nitrating gac, receive more concern.
Such as, (the SustainableandhierarchicalporousEnteromorphaproliferabas edcarbonforCO such as ZhanquanZhang
2capture, JournalofHazardousmaterials, 2012) be raw material with Enteromorpha, through hydro-thermal charing, KOH activation, obtained that nitrogen content is 2.6wt%, specific surface area is 418m
2the gac of/g.(the Superiorcarbon-basedCO such as SongJian
2adsorbentspreparedfrompoplaranthers, Carbon, 2014) be raw material with Poplar anthers, through routine charing, KOH activation, obtained that nitrogen content is 1.26wt%, specific surface area is 3322m
2the gac of/g.Zhu Bo etc. (preparation of soya bean slag base porous charcoal and the research of ultra-high capacity thereof, Shandong Technology Univ's journal (natural science edition), 2014) utilize bean dregs and KOH, have obtained nitrogen-dopped activated carbon.
Above-mentioned research is that the preparation of nitrating gac provides invaluable experience.But, adopt the method for these research reports, need first to carbonize raw material before activation, need to carry out long drying to the mixture of carbon precursor and alkali lye, or need to adopt lower temperature rise rate (≤5 DEG C/min), cause the preparation cycle of nitrating gac long, technique is loaded down with trivial details, or energy consumption is large.
Summary of the invention
Object of the present invention is exactly in view of the foregoing defects the prior art has, provides a kind of preparation cycle shorter, the convenient preparation method of the simple biomass-based nitrating gac of technique.
Its technical scheme comprises the following steps: first adopt dry method to carry out Homogeneous phase mixing by the mass ratio of 1.2 ~ 3.0:1 in salt of wormwood and bean dregs; add particle diameter by the 5%-50% of bean dregs quality again and be not more than 1.5mm bicarbonate of ammonia; carry out Homogeneous phase mixing; again by mixture noble gas protection under; activation temperature is heated to the temperature rise rate of 7-20 DEG C/min; insulation 65-100min, finally carries out cooling, washing to neutral, dry, obtained nitrating gac.
The particle diameter of above-mentioned bean dregs is 0.1-3.0mm, and moisture content is not higher than 7%.
Above-mentioned salt of wormwood is powdery, and largest particle particle diameter is less than 1.0mm.
Above-mentioned dry method, refers to and is mixed with biomass by salt of wormwood powder, is not to adopt the salt of wormwood being dissolved in water or alcohol.
Above-mentioned is even, refers to the mixture constantly stirring salt of wormwood powder and biomass, until visually even.
Above-mentioned activation temperature is 570-750 DEG C.
Above-mentioned washing, refers to that washing is 7.0-8.0 to the pH value of washing lotion.
Above-mentioned cooling, refers to and naturally cools under nitrogen protection under 100 DEG C.
Above-mentioned drying, refers on 110 DEG C of forced air drying 10h.
Compared with the technology of preparing of existing biomass-based nitrating gac, advantage of the present invention is:
1) preparation cycle is shorter, and technique is simple, and energy consumption is little, without the need to first carbonizing raw material before activation, without the need to carrying out drying to the carbon precursor containing activator, and can adopt higher temperature rise rate; 2) gained gac contains abundant nitrogen element (nitrogen content is 1.0wt% ~ 8.0wt%) and larger specific surface area (500m
2/ g ~ 1800m
2/ g); 3) in preparation process without the need to adopting alkalescence extremely strong caustic soda and Pian Zhuan caustic potash flakes, significantly reduce the corrosion to equipment.
Embodiment
Below in conjunction with example, the invention will be further described, but be not used in restriction the present invention:
embodiment 1
The salt of wormwood and the particle diameter that particle diameter are less than 0.5mm are the bean dregs of 0.2-0.9mm, mix, then add by 5% of bean dregs quality the bicarbonate of ammonia that particle diameter is 0.1-1.5mm, stir by the mass ratio of 2:1.By mixture under nitrogen protection, be heated to 570 DEG C with the temperature rise rate of 7 DEG C/min, insulation 100min.Then, it is cooled to 80 DEG C under nitrogen protection, and uses deionized water repetitive scrubbing, until the pH value of washing lotion is 8.0.Finally, by sample in 110 DEG C of forced air drying 15h.The specific surface area of gained nitrating gac is 980m
2/ g, nitrogen content is 4.2wt%.
embodiment 2
The salt of wormwood and the particle diameter that particle diameter are less than 0.3mm are the bean dregs of 0.2-0.9mm, mix, then add the bicarbonate of ammonia of 0.2-1.2mm by 50% of bean dregs quality, stir by the mass ratio of 1.5:1.By mixture under nitrogen protection, be heated to 600 DEG C with the temperature rise rate of 12 DEG C/min, insulation 70min.Then, it is cooled to 60 DEG C under nitrogen protection, and uses deionized water repetitive scrubbing, until the pH value weakly acidic pH of washing lotion.Finally, by sample in 110 DEG C of forced air drying 12h.The specific surface area of gained nitrating gac is 830m
2/ g, nitrogen content is 5.2wt%.
embodiment 3
The salt of wormwood and the particle diameter that particle diameter are less than 0.1mm are the bean dregs of 0.3-1.0mm, mix, then add the bicarbonate of ammonia of 0.5-1.5mm by 25% of bean dregs quality, stir by the mass ratio of 1.8:1.By mixture under nitrogen protection, be heated to 650 DEG C with the temperature rise rate of 15 DEG C/min, insulation 50min.Then, it is cooled to 70 DEG C under nitrogen protection, and uses deionized water repetitive scrubbing, until the pH value weakly acidic pH of washing lotion.Finally, by sample in 110 DEG C of forced air drying 12h.The specific surface area of gained nitrating gac is 1080m
2/ g, nitrogen content is 3.7wt%.
embodiment 4
The salt of wormwood and the particle diameter that particle diameter are less than 1.0mm are the bean dregs of 0.1-3.0mm, mix, then add the bicarbonate of ammonia of 0.05-0.9mm by 32% of bean dregs quality, stir by the mass ratio of 3:1.By mixture under nitrogen protection, be heated to 750 DEG C with the temperature rise rate of 20 DEG C/min, insulation 65min.Then, it is cooled to 80 DEG C under nitrogen protection, and uses deionized water repetitive scrubbing, until the pH value weakly acidic pH of washing lotion.Finally, by sample in 110 DEG C of forced air drying 12h.The specific surface area of gained nitrating gac is 1180m
2/ g, nitrogen content is 3.2wt%.
The above, be only part preferred embodiment of the present invention, any those of ordinary skill in the art all may utilize the technical scheme correct of above-mentioned elaboration or are revised as equivalent technical scheme.Therefore, any simple modification of carrying out according to technical scheme of the present invention or substitute equivalents, belong to the scope of protection of present invention to the greatest extent.
Claims (9)
1. a convenient preparation method for biomass-based nitrating gac, is characterized in that comprising the following steps:
First dry method is adopted to carry out Homogeneous phase mixing by the mass ratio of 1.2 ~ 3.0:1 in salt of wormwood and bean dregs; the ammonium hydrogencarbonate of 1.5mm is not more than again by the 5%-50% interpolation particle diameter of bean dregs quality; carry out Homogeneous phase mixing; again by mixture noble gas protection under; activation temperature is heated to the temperature rise rate of 7-20 DEG C/min; insulation 65-100min, finally carries out cooling, washing to neutral, dry, obtained nitrating gac.
2. preparation according to claim 1 in the pressed active carbon method of water float, can is characterized in that: the particle diameter of described bean dregs is 0.1-3.0mm, and moisture content is not higher than 7%.
3. in the pressed active carbon method of water float, can it is characterized in that a kind of preparation according to claim 1: described salt of wormwood is powdery, and largest particle particle diameter is less than 1.0mm.
4. in the pressed active carbon method of water float, can it is characterized in that: described dry method, refer to and mixed with biomass by salt of wormwood powder a kind of preparation according to claim 1, is not adopt the salt of wormwood being dissolved in water or alcohol.
5. in the pressed active carbon method of water float, can it is characterized in that: described is even a kind of preparation according to claim 1, refer to the mixture constantly stirring salt of wormwood powder and biomass, until visually even.
6. in the pressed active carbon method of water float, can it is characterized in that a kind of preparation according to claim 1: described activation temperature is 570-750 DEG C.
7. in the pressed active carbon method of water float, can it is characterized in that: described washing a kind of preparation according to claim 1, refer to that washing is 7.0-8.0 to the pH value of washing lotion.
8. in the pressed active carbon method of water float, can it is characterized in that a kind of preparation according to claim 1: described cooling refers to and naturally cools under nitrogen protection under 100 DEG C.
9. the convenient preparation method of a kind of biomass-based nitrating gac according to claim 1, is characterized in that: described drying refers on 110 DEG C of forced air drying 10h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106115698A (en) * | 2016-06-24 | 2016-11-16 | 浙江大学 | A kind of utilization reclaims useless charcoal method preparing nitrogenous porous charcoal and products thereof and application |
| CN106179440A (en) * | 2016-06-24 | 2016-12-07 | 浙江大学 | N doping multi-stage porous charcoal and its preparation method 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 |
| CN108940191A (en) * | 2018-06-05 | 2018-12-07 | 西北农林科技大学 | A kind of sulphur N doping multiporous biological charcoal, preparation method and application |
| 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 |
| CN115945182A (en) * | 2022-12-20 | 2023-04-11 | 安徽工业大学 | Adsorbent for treating VOCs and dioxin in organic coating pyrolysis flue gas and preparation method thereof |
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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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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 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106115698A (en) * | 2016-06-24 | 2016-11-16 | 浙江大学 | A kind of utilization reclaims useless charcoal method preparing nitrogenous porous charcoal and products thereof and application |
| CN106179440A (en) * | 2016-06-24 | 2016-12-07 | 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 |
| CN108940191A (en) * | 2018-06-05 | 2018-12-07 | 西北农林科技大学 | A kind of sulphur N doping multiporous biological charcoal, preparation method and application |
| 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 |
| CN115945182A (en) * | 2022-12-20 | 2023-04-11 | 安徽工业大学 | Adsorbent for treating VOCs and dioxin in organic coating pyrolysis flue gas and preparation method thereof |
| CN115945182B (en) * | 2022-12-20 | 2024-04-16 | 安徽工业大学 | Adsorbent for treating VOCs and dioxins in organic coating pyrolysis flue gas and preparation method thereof |
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