CN105692591A - Preparation method of blocky porous carbon with large specific surface area - Google Patents
Preparation method of blocky porous carbon with large specific surface area Download PDFInfo
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- CN105692591A CN105692591A CN201610164445.2A CN201610164445A CN105692591A CN 105692591 A CN105692591 A CN 105692591A CN 201610164445 A CN201610164445 A CN 201610164445A CN 105692591 A CN105692591 A CN 105692591A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a preparation method of blocky porous carbon with a large specific surface area. Phenols, polysaccharides, water and ionic liquid are mixed in a mass ratio of 1:(1-4):(10-40):(0.01-1). The preparation method comprises the following steps: firstly, mixing the phenols and the polysaccharides; adding deionized water; stirring the mixture at a temperature of 50 DEG C in order that the phenols and the polysaccharides are fully dissolved; adding the ionic liquid; uniformly mixing at a temperature of 50 DEG C while stirring; putting the mixture into a microwave oven of which the power is 400-1000w; heating for 10-600s; flushing the obtained material with water and ethanol, and drying to obtain a blocky porous carbon material with a large specific surface area. In the method, the polysaccharides and the phenols are used as reaction monomers, the ionic liquid is added to serve as a solvent and a templating agent, and heating is performed through a one-step microwave method to form the blocky porous carbon with the large specific surface area. The specific surface area of the prepared blocky porous carbon is up to 1500m<2>/g. The method has the advantages of simple process, convenience in operation, less equipment, further reduction of the cost, convenience in popularization and application, and suitability for mass production.
Description
Technical field
The present invention relates to porous charcoal art, the preparation method that a kind of specific area block body stephanoporate carbon is particularly provided。
Background technology
Block body stephanoporate Carbon Materials has good anticorrosive stability (ph stability etc.), good electric conductivity, the features such as superpower absorbability, simultaneously because the profile of its block, commercial Application can be made directly, so its synthesis is no matter in basic research, or all significant in practical application。Tradition prepares block material with carbon element mainly by bonding casting pressure, template duplicating, aerosol etc.。The shortcoming of bonding casting pressure is that the mechanical strength of block charcoal, pore volume etc. are had a significant impact by the kind of binding agent, consumption。And the method for stencil duplicating needs first synthesizing block silica material, so cost is high, of long duration, not easily industrialization；Aerocolloidal method needs strictly to regulate and control experiment condition, through aging for a long time, then carries out CO2Supercritical drying, block Carbon Materials is made in finally at high temperature carbonization, and the method is owing to process is complicated and supercritical drying cost intensive is difficult to scale on producing。
Patent CN101948106B uses saccharide and phenols to be reaction monomers, and adding mineral acid/organic acid/sulfate is catalyst, utilizes hydrothermal carbonization method to form it into block charcoal, immediately carbonization under an inert atmosphere, obtains the porous carbon material of high-specific surface area。Although the method uses the hydrothermal carbonization method of mild condition, the pressure and temperature difficulty in water heating kettle controls, and the concordance of product is difficult to ensure that。And mild condition, the block body stephanoporate material with carbon element of preparation only has 700m than table2/ g, far below the product specific surface area of activated carbon bonding casting pressure, it is necessary to after steam activation, ability specific surface area is up to 2600m2/ g, activation power consumption is big especially, is unfavorable for industrialized production。
Microwave is as a kind of new mode of heating; have heating rapidly, uniformly, be absent from the advantages such as thermograde; many reaction systems are had the effect accelerating chemical reaction, and in the industrial scale productions such as microwave chemical successful Application wastewater treatment, organic chemical synthesis。This is easy to utilize microwave method, the method of energy-conserving and environment-protective, using economical and practical saccharide and phenols is the block Carbon Materials that reaction monomers polyreaction generates, and its material surface is rich in various functional groups, specific surface area is high, is expected to for adsorbing metal ions, organic compound。
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, the preparation method that it is an object of the invention to provide a kind of specific area block body stephanoporate carbon, the method uses saccharide and phenols to be reaction monomers, add ionic liquid as solvent and template, utilize a step microwave method to be heated forming high-specific surface area block body stephanoporate carbon。
For achieving the above object, the present invention adopts such as purgation technical scheme: the preparation method of a kind of specific area block body stephanoporate carbon, by phenols: saccharide: water: ionic liquid=1: the mass ratio of 1-4: 10-40: 0.01-1 mixes, first phenols and saccharide are mixed, add deionized water, and stirring makes phenols and saccharide fully dissolve at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 400-1000w, heating 10～600s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
As a kind of preferred version, described phenols is at least one in phenol, resorcinol, phloroglucinol。
As a kind of preferred version, described saccharide is glucose, fructose, lactose, sucrose, cellulose, at least one in starch。
As a kind of preferred version, described ionic liquid is at least one in N-methyl butyl pyrrolidine bis-trifluoromethylsulfoandimide salt, N-methyl butyl piperidines bis-trifluoromethylsulfoandimide salt, 1-ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt, 1-ethyl-3-methylimidazole tetrafluoroborate, trimethyl the third ammonium bis-trifluoromethylsulfoandimide salt and 1-hexyl-3-Methylimidazole. bis-trifluoromethylsulfoandimide salt。
The present invention compared with prior art has clear advantage and beneficial effect, particularly as follows:
1) the inventive method is with ionic liquid for microwave absorbing material, and with microwave for heating source, within whole course of reaction only needs 10 minutes, can realize the efficiently quickly preparation of high-specific surface area block body stephanoporate carbon material。
2) use ionic liquid as precursors and the regulator of material hole structure, Carbon Materials can change the hierarchical porous structure of material。Ionic liquid refers to and presents liquid, the complete salt being made up of zwitterion in room temperature or under room temperature, also referred to as low temperature molten salt。Ionic liquid is as ionic compound, and the relatively low main cause of its fusing point is the unsymmetry of some substituent group in its structure, makes ion not to be piled into caused by crystal regularly。It is little that functional type ionic liquid has vapour pressure, and volatility is low, and hetero atom enriches, the features such as solvability is strong。Wherein, most important feature is that ionic liquid is as supermolecule solvent, it is possible to as the place of molecular recognition Yu assembling。Meanwhile, ionic liquid itself also shows the character of surfactant, it is possible to organize nanostructured good, long-range order by assembling to be formed。Ionic liquid as the template of synthetic material, can make the material of preparation have abundant functional group and pore passage structure。The block body stephanoporate carbon material specific surface area prepared is up to 1500m2/ more than g。
3) present invention process is simple, easy to operate, producing equipment few, thus reducing cost further, it is simple to popularization and application, being suitable to large-scale production。
Detailed description of the invention
Embodiment 1
A kind of preparation method of specific area block body stephanoporate carbon, by phenols: saccharide: water: ionic liquid=1: the mass ratio of 1: 10: 0.01 mixes, first, phenols and saccharide are mixed, adding deionized water makes phenols and glucide in this mixture stir fully dissolving at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 1000w, heating 10s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
This phenols is phenol；This saccharide is glucose；This ionic liquid is N-methyl butyl pyrrolidine bis-trifluoromethylsulfoandimide salt
Embodiment 2
A kind of preparation method of specific area block body stephanoporate carbon, by phenols: saccharide: water: ionic liquid=1: the mass ratio of 4: 40: 1 mixes, first phenols and saccharide are mixed, add deionized water, and stirring makes phenols and saccharide fully dissolve at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 400w, heating 600s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
This phenols is that phenol, resorcinol, phloroglucinol 1:1:1 in mass ratio mixes；This saccharide is fructose and cellulose 1:2 in mass ratio mixes；This ionic liquid is that 1-ethyl-3-methylimidazole tetrafluoroborate, trimethyl the third ammonium bis-trifluoromethylsulfoandimide salt and 1-hexyl-3-Methylimidazole. bis-trifluoromethylsulfoandimide salt 1:2:3 in mass ratio mix。
Embodiment 3
A kind of preparation method of specific area block body stephanoporate carbon, by phenols: saccharide: water: ionic liquid=1: the mass ratio of 2: 20: 0.3 mixes, first phenols and saccharide are mixed, add deionized water, and stirring makes phenols and saccharide fully dissolve at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 700w, heating 450s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
This phenols is resorcinol；This saccharide is lactose；This ionic liquid is N-methyl butyl piperidines bis-trifluoromethylsulfoandimide salt。
Embodiment 4
A kind of preparation method of specific area block body stephanoporate carbon, by phenols: saccharide: water: ionic liquid=1: the mass ratio of 3: 30: 0.7 mixes, first phenols and saccharide are mixed, add deionized water, and stirring makes phenols and saccharide fully dissolve at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 800w, heating 380s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
This phenols is phloroglucinol；This saccharide is starch；This ionic liquid is 1-ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt。
Comparative example: the block body stephanoporate Carbon Materials of activated carbon bonding casting pressure on market。
Product and comparative example product obtained by embodiment 1～4 carry out performance test:
Respectively the block body stephanoporate Carbon Materials of preparation in above-described embodiment and comparative example is adopted the specific surface area of the full-automatic specific surface area analysis instrument test material of ASAP2020 of Micromeritics Instrument Corp. U.S.A。Meanwhile, take in 30mg embodiment and comparative example the block Carbon Materials of preparation respectively in the methyl orange of 200mg/L, basic fuchsin and in rhodamine B solution, survey its adsorbance。
Table 1 lists the block Carbon Materials Performance comparision of different embodiment and comparative example。
As it can be seen from table 1 high-specific surface area block body Carbon Materials specific surface prepared by embodiments of the invention is big, high adsorption capacity。
The above, it it is only presently preferred embodiments of the present invention, not the technical scope of the present invention is imposed any restrictions, therefore every technical spirit according to the present invention is to any trickle amendment made for any of the above embodiments, equivalent variations and modification, all still falls within the scope of technical solution of the present invention。
Claims (4)
1. the preparation method of a specific area block body stephanoporate carbon, it is characterized in that: by phenols: saccharide: water: ionic liquid=1: the mass ratio of 1-4: 10-40: 0.01-1 mixes, first phenols and saccharide are mixed, add deionized water, and stirring makes phenols and saccharide fully dissolve at 50 DEG C of temperature, it is subsequently adding ionic liquid, it is uniformly mixed at 50 DEG C of temperature, it is placed in the microwave oven that power is 400-1000w, heating 10～600s, dry after the material with water obtained and alcohol flushing, obtain high-specific surface area block body stephanoporate carbon material。
2. the preparation method according to a claim 1 specific area block body stephanoporate carbon, it is characterised in that: described phenols is at least one in phenol, resorcinol, phloroglucinol。
3. the preparation method according to a claim 1 specific area block body stephanoporate carbon, it is characterised in that: described saccharide is glucose, fructose, lactose, sucrose, cellulose, at least one in starch。
4. the preparation method according to a claim 1 specific area block body stephanoporate carbon, it is characterised in that: described ionic liquid is at least one in N-methyl butyl pyrrolidine bis-trifluoromethylsulfoandimide salt, N-methyl butyl piperidines bis-trifluoromethylsulfoandimide salt, 1-ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt, 1-ethyl-3-methylimidazole tetrafluoroborate, trimethyl the third ammonium bis-trifluoromethylsulfoandimide salt and 1-hexyl-3-Methylimidazole. bis-trifluoromethylsulfoandimide salt。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324333A (en) * | 2017-06-14 | 2017-11-07 | 万华化学集团股份有限公司 | A kind of monoblock type sorbing material, preparation method and the method using its reduction diisocyanate chromatic number |
| CN108439370A (en) * | 2018-04-25 | 2018-08-24 | 江苏大学 | A kind of preparation method and its usage of two dimension porous boron nitrogen codope carbon nanomaterial |
| CN112058231A (en) * | 2020-09-10 | 2020-12-11 | 上海理工大学 | Method for preparing porous biochar by low-temperature pyrolysis of ionic liquid modified waste biomass, porous biochar and application of porous biochar |
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| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| CN103395769A (en) * | 2013-07-31 | 2013-11-20 | 浙江大学 | Preparation method of porous carbon material based on ionic heat process |
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2016
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| CN103395769A (en) * | 2013-07-31 | 2013-11-20 | 浙江大学 | Preparation method of porous carbon material based on ionic heat process |
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| WEILI ZHANG ET AL.: "One-pot synthesis of carbonaceous monolith with surface sulfonic groups and its carbonization/activation", 《CARBON》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324333A (en) * | 2017-06-14 | 2017-11-07 | 万华化学集团股份有限公司 | A kind of monoblock type sorbing material, preparation method and the method using its reduction diisocyanate chromatic number |
| CN107324333B (en) * | 2017-06-14 | 2019-09-03 | 万华化学集团股份有限公司 | A kind of monoblock type adsorbent material, preparation method and the method for reducing diisocyanate chromatic number using it |
| CN108439370A (en) * | 2018-04-25 | 2018-08-24 | 江苏大学 | A kind of preparation method and its usage of two dimension porous boron nitrogen codope carbon nanomaterial |
| CN112058231A (en) * | 2020-09-10 | 2020-12-11 | 上海理工大学 | Method for preparing porous biochar by low-temperature pyrolysis of ionic liquid modified waste biomass, porous biochar and application of porous biochar |
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