CN105692591B - A kind of preparation method of high specific area block body stephanoporate carbon - Google Patents
A kind of preparation method of high specific area block body stephanoporate carbon Download PDFInfo
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- CN105692591B CN105692591B CN201610164445.2A CN201610164445A CN105692591B CN 105692591 B CN105692591 B CN 105692591B CN 201610164445 A CN201610164445 A CN 201610164445A CN 105692591 B CN105692591 B CN 105692591B
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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
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The present invention discloses a kind of preparation method of high specific area block body stephanoporate carbon, by phenols: carbohydrate: water: ionic liquid=1: 1-4: 10-40: 0.01-1 mass ratio is mixed, phenols and carbohydrate are mixed first, add deionized water, and stirring dissolves phenols and carbohydrate sufficiently at 50 °C, then ionic liquid is added, it is uniformly mixed at 50 °C, it is placed in the micro-wave oven that power is 400-1000w, heat 10~600s, obtained material with water and ethyl alcohol is dry after rinsing, and obtains high-specific surface area block body stephanoporate carbon material.This method is reaction monomers using carbohydrate and phenols, and ionic liquid is added as solvent and template, carries out being thermally formed high-specific surface area block body stephanoporate carbon using a step microwave method, the block body stephanoporate carbon material specific surface area prepared is up to 1500m2/ g or more.Present invention process is simple, easy to operate, and production equipment is few, thus further reduce the cost, it is easy to promote and utilize, it is suitable for large-scale production.
Description
Technical field
The present invention relates to porous charcoal field technologies, are especially to provide a kind of preparation method of high specific area block body stephanoporate carbon.
Background technique
Block body stephanoporate Carbon Materials have good anticorrosive stability (ph stability etc.), good electric conductivity, superpower
Adsorption capacity the features such as, simultaneously because the shape of its block, can directly carry out industrial application, so no matter its synthesis is in base
Plinth research aspect, or be all of great significance in practical application.Tradition prepares block carbon material and mainly passes through bonding casting
Pressure, template duplicating, aerosol etc..The shortcomings that bonding casting pressure is mechanical strength to block charcoal of the type, dosage of binder, Kong Rong
Etc. having a significant impact.And the method for stencil duplicating needs synthesizing block silica material first, thus it is at high cost, of long duration, no
Easily industrialization；The method of aerosol needs stringent regulation experiment condition then to carry out CO by prolonged aging2It is overcritical
Dry, finally carbonization is made block Carbon Materials at high temperature, this method due to process complexity and supercritical drying it is expensive
It is difficult scale in production.
Patent CN 101948106B is reaction monomers using carbohydrate and phenols, and inorganic acid/organic acid/sulfate is added and is
Catalyst forms it into block charcoal using hydrothermal carbonization method, is carbonized under an inert atmosphere immediately, obtains the porous of high-specific surface area
Carbon Materials.Although the mild hydrothermal carbonization method of this method use condition, the pressure and temperature in water heating kettle is difficult to control, the one of product
Cause property is difficult to ensure.And mild condition, the block body stephanoporate carbon material of preparation only have 700m than table2/ g, it is viscous far below active carbon
The product specific surface area of knot casting pressure needs ability specific surface area after steam activation to be up to 2600m2/ g, activation energy consumption is especially big,
It is unfavorable for industrialized production.
The microwave heating method new as one kind has many advantages, such as that heating is rapid, uniform, there is no temperature gradients, to perhaps
More reaction systems have the effect of accelerating chemical reaction, and wastewater treatment has been applied successfully in microwave chemical, organic chemistry closes
At in equal industrial scales production.Using microwave method, this is easy, and energy-saving and environment-friendly method uses economical and practical carbohydrate and phenol
Class is the block Carbon Materials that reaction monomers polymerization reaction generates, and material surface is rich in various functional groups, and 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 in view of the existing deficiencies of the prior art, the purpose of the present invention is to provide a kind of high specific surfaces
The preparation method of product block body stephanoporate carbon, this method are reaction monomers using carbohydrate and phenols, be added ionic liquid as solvent with
Template carries out being thermally formed high-specific surface area block body stephanoporate carbon using a step microwave method.
To achieve the above object, the present invention is using following technical solution: a kind of preparation of high specific area block body stephanoporate carbon
Method, by phenols: carbohydrate: water: ionic liquid=1: 1-4: 10-40: 0.01-1 mass ratio is mixed, first by phenols and
Carbohydrate is mixed, and deionized water is added, and at 50 °C stirring dissolve phenols and carbohydrate sufficiently, be then added from
Sub- liquid, is uniformly mixed at 50 °C, is placed in the micro-wave oven that power is 400-1000w, heats 10~600s, obtain
The material with water and ethyl alcohol arrived is dry after rinsing, and obtains high-specific surface area block body stephanoporate carbon material.
As a preferred embodiment, the phenols is at least one of phenol, resorcinol, phloroglucin.
As a preferred embodiment, the carbohydrate is glucose, fructose, lactose, sucrose, cellulose, in starch at least
It is a kind of.
As a preferred embodiment, the ionic liquid is N- methyl butyl pyrrolidines bis-trifluoromethylsulfoandimide salt, N-
Methyl butyl piperidines bis-trifluoromethylsulfoandimide salt, 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt, 1- ethyl -3-
Methyl imidazolium tetrafluoroborate, trimethyl the third ammonium bis-trifluoromethylsulfoandimide salt and the double trifluoro methylsulphurs of 1- hexyl -3- methylimidazole
At least one of imide salts.
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically:
1) the method for the present invention is using ionic liquid as microwave absorbing material, and using microwave as heating source, and entire reaction process is only
Within needing 10 minutes, the efficient quick preparation of high-specific surface area block body stephanoporate carbon material can be realized.
2) regulator for using ionic liquid as precursors and material pore structure, can change in Carbon Materials
The hierarchical porous structure of material.Ionic liquid refer to room temperature or close at room temperature present liquid, completely by zwitterion institute group
At salt, also referred to as low temperature molten salt.For ionic liquid as ionic compound, lower melting-point main cause is its structure
In certain substituent groups asymmetry, prevent ion from being regularly piled into caused by crystal.Functional form ionic liquid has steam
Press small, the features such as volatility is low, and hetero atom is abundant, and solvability is strong.Wherein, most important feature is ionic liquid as oversubscription
Sub- solvent can be used as the place of molecular recognition and assembling.Meanwhile ionic liquid itself also shows the property of surfactant
Matter can form that tissue is good, nanostructure of long-range order by assembling.Ionic liquid can be used as the structure of synthetic material
Template makes the material of preparation have functional group abundant and cellular structure.The block body stephanoporate carbon material specific surface area prepared
Up to 1500m2/ g or more.
3) present invention process is simple, easy to operate, and production equipment is few, thus further reduce the cost, it is easy to promote and utilize,
Suitable for large-scale production.
Specific embodiment
Embodiment 1
A kind of preparation method of high specific area block body stephanoporate carbon, by phenols: carbohydrate: water: ionic liquid=1: 1: 10: 0.01
Mass ratio mixed, firstly, phenols and carbohydrate are mixed, adding deionized water makes phenols and carbohydrate object in the mixture
Matter stirs abundant dissolution at 50 °C, and ionic liquid is then added, is uniformly mixed at 50 °C, is placed in power
In the micro-wave oven of 1000w, to heat 10s, obtained material with water and ethyl alcohol are dry after rinsing, and it is more to obtain high-specific surface area block body
Hole Carbon Materials.
The phenols is phenol；The carbohydrate is glucose；The ionic liquid is the double trifluoro methylsulfonyls of N- methyl butyl pyrrolidines
Inferior amine salt
Embodiment 2
A kind of preparation method of high specific area block body stephanoporate carbon, by phenols: carbohydrate: water: ionic liquid=1: 4: 40: 1
Mass ratio is mixed, and first mixes phenols and carbohydrate, adds deionized water, and stirring makes phenol at 50 °C
Class and carbohydrate sufficiently dissolve, and ionic liquid is then added, is uniformly mixed at 50 °C, and being placed in power is the micro- of 400w
In wave furnace, 600s is heated, obtained material with water and ethyl alcohol are dry after rinsing, and obtain high-specific surface area block body stephanoporate carbon material.
The phenols is phenol, resorcinol, phloroglucin 1:1:1 in mass ratio are mixed；The carbohydrate is fructose and fibre
Dimension element 1:2 in mass ratio is mixed；The ionic liquid is 1- ethyl-3-methylimidazole tetrafluoroborate, trimethyl the third ammonium pair
Trifluoro sulfonamide and 1- hexyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt 1:2:3 in mass ratio are mixed.
Embodiment 3
A kind of preparation method of high specific area block body stephanoporate carbon, by phenols: carbohydrate: water: ionic liquid=1: 2: 20: 0.3
Mass ratio mixed, phenols and carbohydrate are mixed first, add deionized water, and at 50 °C stirring make
Phenols and carbohydrate sufficiently dissolve, and ionic liquid is then added, is uniformly mixed at 50 °C, and being placed in power is 700w's
In micro-wave oven, 450s is heated, obtained material with water and ethyl alcohol are dry after rinsing, and obtain high-specific surface area block body stephanoporate carbon material
Material.
The phenols is resorcinol；The carbohydrate is lactose；The ionic liquid is the double trifluoro methylsulfonyls of N- methyl butyl piperidines
Inferior amine salt.
Embodiment 4
A kind of preparation method of high specific area block body stephanoporate carbon, by phenols: carbohydrate: water: ionic liquid=1: 3: 30: 0.7
Mass ratio mixed, phenols and carbohydrate are mixed first, add deionized water, and at 50 °C stirring make
Phenols and carbohydrate sufficiently dissolve, and ionic liquid is then added, is uniformly mixed at 50 °C, and being placed in power is 800w's
In micro-wave oven, 380s is heated, obtained material with water and ethyl alcohol are dry after rinsing, and obtain high-specific surface area block body stephanoporate carbon material
Material.
The phenols is phloroglucin；The carbohydrate is starch；The ionic liquid is the double trifluoro methylsulphurs of 1- ethyl-3-methylimidazole
Imide salts.
Comparative example: the block body stephanoporate Carbon Materials of active carbon bonding casting pressure in the market.
Product obtained by Examples 1 to 4 and comparative example product are tested for the property:
Respectively by the block body stephanoporate Carbon Materials prepared in above-described embodiment and comparative example using Micromeritics Instrument Corp. U.S.A
The specific surface area of the full-automatic specific surface area analysis instrument test material of ASAP2020.Meanwhile 30mg embodiment and comparative example is taken respectively
The block Carbon Materials of middle preparation survey its adsorbance in the methyl orange of 200mg/L, basic fuchsin and rhodamine B solution.
The block Carbon Materials performance that table 1 lists different embodiment and comparative examples compares.
As it can be seen from table 1 the high-specific surface area block body Carbon Materials specific surface of the embodiment of the present invention preparation is big, adsorption energy
Power is strong.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore any trickle amendment, equivalent variations and modification made to the above embodiment according to the technical essence of the invention, still
Belong in the range of technical solution of the present invention.
Claims (1)
1. a kind of preparation method of high specific area block body stephanoporate carbon, it is characterised in that: press phenols: carbohydrate: water: ionic liquid=1:
The mass ratio of 1-4: 10-40: 0 .01-1 is mixed, and first mixes phenols and carbohydrate, adds deionized water, and
Stirring dissolves phenols and carbohydrate sufficiently at 50 °C, and ionic liquid is then added, and is stirred at 50 °C
It is even, it is placed in the micro-wave oven that power is 400-1000w, heats 10~600s, obtained material with water and ethyl alcohol are dry after rinsing,
Obtain high-specific surface area block body stephanoporate carbon material；The phenols is at least one of phenol, resorcinol, phloroglucin, institute
Stating carbohydrate is glucose, fructose, lactose, sucrose, cellulose, at least one of starch；The ionic liquid is N- methyl fourth
Base pyrrolidines 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
At least one of 1- hexyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt.
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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| One-pot synthesis of carbonaceous monolith with surface sulfonic groups and its carbonization/activation;Weili Zhang et al.;《CARBON》;20101224;第1811-1820页 |
| 微波加热技术在多孔炭处理中的应用;檀素霞等;《炭素技术》;20061231;第25卷(第4期);第35-39页 |
| 离子液体为新型前驱体制备含氮碳纳米材料及其应用;来庆学等;《化学进展》;20131031;第25卷(第10期);第1703-1702页 |
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