CN102502588A - Method for preparing mesoporous carbon with controllable aperture distribution - Google Patents
Method for preparing mesoporous carbon with controllable aperture distribution Download PDFInfo
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Abstract
The invention discloses a method for preparing mesoporous carbon with controllable aperture distribution. The method comprises the following steps of: dispersing nano particles into a carbon precursor solution, and performing ball milling and mixing, wherein the mass ratio of the nano particles to the carbon precursor is (0.1-10): 1; controlling the consumption of the solution to keep the mixture pasty; removing the solvent, and then performing carbonization for 0.1 to 3 hours at the temperature of between 500 and 1,200 DEG C in an inert atmosphere; cleaning with acid or alkali liquor to remove a template agent; and drying the sample, and thus obtaining the mesoporous carbon with controllable aperture distribution. The carbon precursor solution comprises an ethanol solution of thermosetting phenol resin, a methylbenzene solution of asphalt, a dimethyl sulfoxide solution of polyacrylonitrile and an aqueous solution of sucrose; the mass ratio of the solution to the carbon precursor is 1:1-10:1; and the ball milling speed is 200 to 500 revolutions per minute, and the ball milling time is 0.5 to 5 hours. The preparation method is simple; the cost of the product is low; and the mesoporous carbon of which the aperture distribution is centralized in nano particle diameter, can be prepared by using a small amount of solvent.
Description
Technical field
The present invention relates to the preparation method of the controlled mesopore charcoal of a kind of pore size distribution.
Background technology
Porous charcoal has obtained using widely at aspects such as gas-liquid absorption mutually, support of the catalyst and super capacitor electrodes owing to have high-specific surface area, flourishing hole and resistance to acids and bases.The controlled mesopore charcoal of pore size distribution is vital to the utilising efficiency that improves the mesopore charcoal.The preparation method of porous charcoal mainly contains physical activation method, chemical activation method, catalytic activation method and template.Physical activation method, chemical activation method and catalytic activation method can be prepared the porous charcoal of high-specific surface area through suitable process conditions, but the pore size distribution broad.Though the organic formwork method in the template can have the mesopore charcoal that certain pore size distributes through selecting suitable organic formwork agent only can prepare through simple charing step, the porous charcoal pore size distribution of preparation is still not really concentrated; And typical inorganic template can be introduced carbon precursor in the template through the wall thickness of regulatory molecule sieve, prepares the controlled porous charcoal of pore size distribution through operations such as charing, template remove.Though this method can be controlled the pore structure of mesopore charcoal, need synthetic molecular sieve template, complicated process of preparation.Recently; People such as Song Yan utilize nanoparticle to be template; The controlled mesopore charcoal of preparation pore size distribution; But this preparation method needs a large amount of solvents, and (Pore development of thermosetting phenol resin derived mesoporous carbon through a commercially nanosized template Materials Science and Engineering A 473 (2008) 153-157) are difficult to scale operation.
Summary of the invention
The invention discloses the preparation method of the controlled mesopore charcoal of a kind of pore size distribution, the employing nanoparticle is a template, with ball milled nanoparticle and carbon precursor is mixed, and controls the aperture of porous charcoal through the particle diameter of control nanoparticle.The present invention not only preparation technology is simple, and pore size distribution is controlled, and only needs a spot of solvent can nanoparticle and carbon precursor be mixed; Through removing solvent; Charing, removing etc. of template can be prepared the porous charcoal that the aperture concentrates on the template particle diameter; Effectively overcome the mesopore charcoal that adopts prior art for preparing, pore size distribution is wide, complicated process of preparation and be difficult to drawback such as large-scale industrial production.
The preparation method of the mesopore charcoal that a kind of pore size distribution is controlled is characterized in that concrete steps are following:
A) nanoparticle is dispersed in the solution that is dissolved with carbon precursor, ball mill mixing, wherein the mass ratio of nanoparticle and carbon precursor is 0.1-10: 1, it is pasty state that the consumption of control solvent makes mixture;
B) remove behind the solvent 500-1200 ℃ of charing 0.1-3h under the inert atmosphere;
C) with acid or alkali lye cleaning and removing template agent removing, till detecting less than the nanoparticle thing with ordinary method;
D) with step C) after the sample oven dry of preparation both the controlled mesopore charcoal of pore size distribution.
The described carbon matrix precursor solution that is dissolved with comprises: be dissolved with the ethanolic soln of heat-reactive phenolic resin, be dissolved with the bituminous toluene solution, be dissolved with the dimethyl sulphoxide solution of polyacrylonitrile, be dissolved with the aqueous solution of sucrose; Wherein the mass ratio of solution and carbon precursor is 1: 1-10: 1.
Described ball mill mixing, ball milling speed are 200-500 rev/min, and the ball milling time is 0.5-5 hour.
Described nanoparticle is a silicon oxide, Natural manganese dioxide, zinc oxide.
The present invention compared with prior art has following advantage:
(1) preparation method is simple;
(2) select a spot of solvent for use, can prepare the porous charcoal that pore size distribution concentrates on nano particle diameter;
(3) the porous charcoal pore size distribution of preparation is controlled, can select suitable nanoparticle by pore size distribution as required;
(4) product cost is low.
Embodiment
Below in conjunction with embodiment the present invention is specified.
Embodiment 1
With particle diameter is that the nano silicon oxide of 8nm adds in the ethanolic soln of heat-reactive phenolic resin resin, and the two mass ratio is 0.1: 1, removes solvent; Ethanol and resol mass ratio are 5: 1; 300 rev/mins of ball milling 2h, 80 ℃ of curing, 500 ℃ of following charing 0.1h; The NaOH solution washing obtains product after the oven dry till detecting less than nanoparticle with ordinary method.Product performance index is seen table 1.
Embodiment 2
With particle diameter is that the two mass ratio is 2: 1, removes solvent in the nano zine oxide adding bituminous toluene solution of 12nm; Toluene is 1: 1 with the asphalt quality ratio; 200 rev/mins of ball milling 5h, 200 ℃ of curing, 700 ℃ of following charing 2h; The HCl washing obtains product after the oven dry till detecting less than nanoparticle with ordinary method.Product performance index is seen table 1.
Embodiment 3
With particle diameter is that the nano magnesia of 15nm adds in the dimethyl sulphoxide solution of polyacrylonitrile, and the two mass ratio is 10: 1, removes solvent; DMSO 99.8MIN. and polyacrylonitrile mass ratio are 10: 1; 500 rev/mins of ball milling 0.5h, 400 ℃ of curing, 1200 ℃ of following charing 3h; The HCl washing obtains product after the oven dry till detecting less than nanoparticle with ordinary method.Product performance index is seen table 1.
Embodiment 4
With particle diameter is that the nano silicon oxide of 8nm adds in the aqueous solution of sucrose, and the two mass ratio is 7: 1, removes solvent; Ethanol and resol mass ratio are 6: 1; 400 rev/mins of ball milling 3h, 100 ℃ of curing, 900 ℃ of following charing 1h; The NaOH solution washing obtains product after the oven dry till detecting less than nanoparticle with ordinary method.Product performance index is seen table 1.
The performance index of table 1 porous charcoal
| Embodiment | BET specific surface area (m 2/g) | Pore volume (cm 3/g) | Mean pore size (nm) |
| 1 | 221 | 0.37 | 8.62 |
| 2 | 754 | 1.91 | 15.96 |
| 3 | 460 | 1.83 | 17.72 |
| 4 | 634 | 1.18 | 8.67 |
Claims (4)
1. the preparation method of the controlled mesopore charcoal of a pore size distribution is characterized in that concrete steps are following:
A) nanoparticle is dispersed in the solution that is dissolved with carbon precursor, ball mill mixing, wherein the mass ratio of nanoparticle and carbon precursor is 0.1-10: 1, it is pasty state that the consumption of control solvent makes mixture;
B) remove behind the solvent 500-1200 ℃ of charing 0.1-3h under the inert atmosphere;
C) with acid or alkali lye cleaning and removing template agent removing, till detecting less than the nanoparticle thing with ordinary method;
D) with step C) after the sample oven dry of preparation both the controlled mesopore charcoal of pore size distribution.
2. the preparation method of the mesopore charcoal that a kind of pore size distribution according to claim 1 is controlled; It is characterized in that: the described carbon matrix precursor solution that is dissolved with comprises: the ethanolic soln that is dissolved with heat-reactive phenolic resin; Be dissolved with the bituminous toluene solution; Be dissolved with the dimethyl sulphoxide solution of polyacrylonitrile, be dissolved with the aqueous solution of sucrose; Wherein the mass ratio of solution and carbon precursor is 1: 1-10: 1.
3. the preparation method of the mesopore charcoal that a kind of pore size distribution according to claim 1 is controlled is characterized in that: described ball mill mixing, ball milling speed are 200-500 rev/min, and the ball milling time is 0.5-5 hour.
4. the preparation method of the mesopore charcoal that a kind of pore size distribution according to claim 1 is controlled is characterized in that: described nanoparticle is a silicon oxide, Natural manganese dioxide, zinc oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102962035A (en) * | 2012-09-19 | 2013-03-13 | 上海理工大学 | Method for increasing amine compound loading amount in nanoporous carbon and keeping nanopores |
| CN104821398A (en) * | 2015-01-26 | 2015-08-05 | 中国石油大学(华东) | Lithium-ion battery negative electrode material bitumen-based porous carbon/ZnMn2O4 preparation method |
| CN105129771A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of mesoporous carbon with adjustable aperture |
| CN109110742A (en) * | 2017-06-23 | 2019-01-01 | 四川大学 | Utilize the mesoporous carbon and preparation method of manganese compound preparation |
| CN109621998A (en) * | 2018-12-06 | 2019-04-16 | 华南农业大学 | A kind of three-dimensional meso-hole carbon load molybdenum carbide and its preparation method and application |
| CN111498844A (en) * | 2019-01-31 | 2020-08-07 | 山东欧铂新材料有限公司 | Mesoporous activated carbon material and preparation method and application thereof |
| CN114408950A (en) * | 2022-02-22 | 2022-04-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
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| CN101696005A (en) * | 2009-10-15 | 2010-04-21 | 浙江大学 | Method for preparing acrylonitrile polymer based mesoporous carbon |
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| CN101696005A (en) * | 2009-10-15 | 2010-04-21 | 浙江大学 | Method for preparing acrylonitrile polymer based mesoporous carbon |
Non-Patent Citations (2)
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| 唐志红等: "Properties of mesoporous carbons prepared from different carbon precursors using nanosize silica as a template", 《新型炭材料》 * |
| 唐志红等: "炭前驱体对纳米粒子模板法制备的中孔炭结构影响", 《第22届炭-石墨材料学术会议论文集》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102962035A (en) * | 2012-09-19 | 2013-03-13 | 上海理工大学 | Method for increasing amine compound loading amount in nanoporous carbon and keeping nanopores |
| CN104821398A (en) * | 2015-01-26 | 2015-08-05 | 中国石油大学(华东) | Lithium-ion battery negative electrode material bitumen-based porous carbon/ZnMn2O4 preparation method |
| CN105129771A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of mesoporous carbon with adjustable aperture |
| CN105129771B (en) * | 2015-09-09 | 2017-03-15 | 上海大学 | A kind of preparation method of the mesoporous carbon of aperture controllable |
| CN109110742A (en) * | 2017-06-23 | 2019-01-01 | 四川大学 | Utilize the mesoporous carbon and preparation method of manganese compound preparation |
| CN109110742B (en) * | 2017-06-23 | 2021-12-24 | 四川大学 | Mesoporous carbon prepared by manganese compound and preparation method thereof |
| CN109621998A (en) * | 2018-12-06 | 2019-04-16 | 华南农业大学 | A kind of three-dimensional meso-hole carbon load molybdenum carbide and its preparation method and application |
| CN109621998B (en) * | 2018-12-06 | 2021-04-02 | 华南农业大学 | Three-dimensional mesoporous carbon loaded molybdenum carbide and preparation method and application thereof |
| CN111498844A (en) * | 2019-01-31 | 2020-08-07 | 山东欧铂新材料有限公司 | Mesoporous activated carbon material and preparation method and application thereof |
| CN114408950A (en) * | 2022-02-22 | 2022-04-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
| CN114408950B (en) * | 2022-02-22 | 2023-08-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
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Application publication date: 20120620 |