CN105523539A - Preparation method of porous carbon material - Google Patents
Preparation method of porous carbon material Download PDFInfo
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- CN105523539A CN105523539A CN201610052368.1A CN201610052368A CN105523539A CN 105523539 A CN105523539 A CN 105523539A CN 201610052368 A CN201610052368 A CN 201610052368A CN 105523539 A CN105523539 A CN 105523539A
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- C01—INORGANIC CHEMISTRY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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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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- C—CHEMISTRY; METALLURGY
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- 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 invention provides a preparation method of a porous carbon material. Phenol and formaldehyde are taken as starting materials, an alkaline compound is taken as a catalyst, a condensation polymerization reaction of phenol and formaldehyde is adjusted, ethylene glycol with a low boiling point is taken as a hole forming agent, and the porous carbon material is synthesized through five procedures of mixing, preparation, blending, curing and pyrolysis; meanwhile, a high-viscosity phase is endowed with different characteristics during phase separation by adjusting ingredients during mixing and a process during preparation, finally, pore features of porous carbon are accurately cut, and the porous carbon material meeting demands of multiple application fields can be prepared. Compared with an existing technology, the method can effectively avoid the uncontrollability of cutting of the pore features of the porous carbon due to difference of the ingredients and structures of industrial-grade resin carbonaceous precursor to a great extent, the repeatability of a porous carbon synthesis process is improved, and accurate cutting of the pore features of the porous carbon is realized.
Description
Technical field
The present invention relates to a kind of technology of preparing of carbon element functional materials, particularly a kind of preparation method of porous carbon materials.
Background technology
Porous carbon is a kind of carbon element functional materials of pore texture prosperity, have that chemical stability is high, catalytic activity be strong, good conductivity, the advantage such as cheap, be widely used in the various fields such as gas delivery, Water warfare, Chu Qing, ultracapacitor, fuel cell, lithium-ion secondary cell, dye-sensitized solar cells and carbide ceramics be shaping.The pore character of these purposes and porous carbon is closely bound up.Such as, when porous carbon is as adsorbent macromole (polymkeric substance, dyestuff, vitamin b6 usp etc.), require that its aperture is mesoporous yardstick (i.e. 2nm< aperture <50nm); When porous carbon prepares complicated shape, difficult process engineering pottery as precast body by reaction formation, the pore character of porous carbon dominates the performance of final ceramic part.
Therefore, the pore character how effectively controlling porous carbon is the prerequisite determining its application, has very important meaning.
The pore character of porous carbon relies on its preparation technology to a great extent.Typical preparation technology comprises activation method, template, biomass carbonization method, organic gel carbonization method and organic polymer and to be separated carborization etc.Wherein, the organic polymer carborization that is separated can control the pore character of porous carbon effectively.United States Patent (USP) (3859421,1975) by this method with finished product furfuryl alcohol resin for carbonaceous precursor has prepared porous carbon.YanXiangWang (Carbon, 2003, the 41:2065 – 2072) impact of processing parameter on finished product furfuryl alcohol resin porous carbon compared with systematic research, achieves the cutting of porous carbon pore character.Chinese patent " preparation method (CN200710018125.7) of porous carbon materials " has synthesized porous carbon with finished product heat-reactive phenolic resin (technical grade 2130#) for carbonaceous precursor, is achieved the cutting of porous carbon pore character by adjusting process parameter.As can be seen here, there is not yet the report of resin carbonaceous precursor self character (comprising molecular structure, viscosity, water-content, gelation time etc.) as the approach of regulation and control porous carbon pore character in existing disclosed document.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of porous carbon materials, the method for starting raw material, by adjustment resin carbonaceous precursor characteristic, realizes the cutting of porous carbon pore character with phenol and formaldehyde.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for porous carbon materials, comprises the following steps:
1) batch mixing: first phenol and basic cpd are mixed by the weight ratio of 1:0.02 ~ 1:0.12, add formaldehyde subsequently, stir, obtains mixing solutions; Wherein, phenol, formaldehyde mole ratio are 1:1 ~ 1:1.8;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 1 ~ 3h carries out polycondensation, and after subsequent dewatering, room temperature is placed, and obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1 ~ 1:1.5, the colloidal resin and ethylene glycol with mobility are mixed, add benzene sulfonyl chloride subsequently, stir, be made into colloidal resin mixture; Wherein, the add-on of benzene sulfonyl chloride is 4 ~ 15% of colloidal resin and ethylene glycol gross weight;
4) solidify: first colloidal resin mixture is cured, obtains cured body;
5) pyrolysis: at N
2under protection, cured body is carried out pyrolysis, rise to 800 DEG C by room temperature, insulation 1h, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
Described basic cpd is the one in sodium carbonate, sodium hydroxide, potassium hydroxide, ammoniacal liquor.
Described dehydration is vacuum hydro-extraction 0.5 ~ 3h at 60 DEG C.
The time that described room temperature is placed is 0.5 ~ 15h.
Described solidification detailed process is as follows: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rises to 180 DEG C of insulation 16h by 60 DEG C, obtains cured body.
Rise to 180 DEG C of warming machines adopted by 60 DEG C to be made as and to raise 20 DEG C every 12h.
The temperature rise rate that described room temperature rises to 800 DEG C is 2 DEG C/min.
Compared with prior art, the beneficial effect that has of the present invention:
The present invention for starting raw material, take basic cpd as the polycondensation of catalyzer adjustment phenol and formaldehyde with phenol and formaldehyde, obtained colloidal resin, and repeatability better; With lower boiling ethylene glycol for pore-forming agent, by batch mixing, system material, batching, solidification, the large synthesizing porous carbon material of operation of pyrolysis five.The method is under the prerequisite of pore channel of giving carbon material prosperity, by technique when composition during adjustment batch mixing and system material, give the characteristic that resin carbonaceous precursor is different, finally realize the accurate cutting of porous carbon pore character (relevant parameter comprises aperture size, void content, density etc.), average pore rate is 27.5 ~ 40.5%, and mean density is 0.61 ~ 1.21g/cm
3, therefore can prepare the porous carbon meeting numerous Application Areas demands.The method compared with prior art, on the basis of not obvious increase cost, the uncontrollability of the porous carbon pore character cutting that the difference because of the composition and structure of technical grade resin carbonaceous precursor can be avoided to a great extent to cause, promote the repeatability of porous carbon synthesis technique, realize the accurate cutting of porous carbon pore character, overcome the problem of application performance by the domination of its pore character of porous carbon in prior art.
Accompanying drawing explanation
Fig. 1 is the photomacrograph of porous carbon materials in the embodiment of the present invention 1;
Fig. 2 is the SEM pattern of porous carbon materials in the embodiment of the present invention 1;
Fig. 3 is the XRD curve of porous carbon materials in the embodiment of the present invention 1;
Fig. 4 is the relative value of the significant parameter of three revision test acquisitions in the embodiment of the present invention 1.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
Embodiment 1:
1) batch mixing: first by the weight ratio of 1:0.03 by phenol and sodium carbonate by being uniformly mixed, add formaldehyde subsequently, stir further and obtain mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1.5;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 3h carries out polycondensation, vacuum hydro-extraction 2h at 60 DEG C subsequently, and after stopping stirring, room temperature places 15h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1.5 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 6% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
The intermediate product that the present embodiment obtains---colloidal resin is gluey and is garnet.Respectively as depicted in figs. 1 and 2, the macrostructure of visible porous carbon is complete, do not occur crackle, and its inside has formed the crosslinked pore texture of nano-scale for the final product that the present embodiment obtains---the photomacrograph of porous carbon and SEM pattern.The XRD curve of porous carbon as shown in Figure 3.As shown in Figure 3, the XRD curve of porous carbon only there are two wider diffraction peaks, respectively (002) and (100) diffraction peak of corresponding graphite, mean that porous carbon has the vitreous carbon material of class graphite microcrystal accumulation.Fig. 4 is the relative value (namely same type parameter is all divided by maximum value wherein) of the significant parameter of colloidal resin and the porous carbon obtained in triplicate according to the present embodiment.As shown in Figure 4, the process repeatability that the present invention relates to is better, and three significant parameters of colloidal resin and the deviation of two significant parameters of porous carbon in three tests are all less than 5%.In addition, the average residual water content of colloidal resin is 16.3%, and average gelation time is 15min, and average viscosity is 88.75Pas; The average pore rate of porous carbon is 40.5%, and mean density is 0.61g/cm
3.
Embodiment 2:
1) batch mixing: first by the weight ratio of 1:0.03 by phenol and sodium hydroxide by being uniformly mixed, add formaldehyde subsequently, stir further and obtain mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1.3;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 3h carries out polycondensation, vacuum hydro-extraction 1h at 60 DEG C subsequently, and after stopping stirring, room temperature places 0.66h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1.5 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 6% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
The present embodiment obtain intermediate product---the residual moisture content of colloidal resin is 24.04%, and gelation time is 8.5min, and viscosity is 27.9Pas; The void content of final product---porous carbon is 31.66%, and density is 0.69g/cm
3.
Embodiment 3:
1) batch mixing: first by the weight ratio of 1:0.03 by phenol and sodium carbonate by being uniformly mixed, add formaldehyde subsequently, stir further and obtain mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1.17;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 2h carries out polycondensation, vacuum hydro-extraction 2h at 60 DEG C subsequently, and after stopping stirring, room temperature places 15h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1.5 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 6% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
The present embodiment obtain intermediate product---the residual moisture content of colloidal resin is 13.15%, and gelation time is 16min, and viscosity is 4.4Pas; The void content of final product---porous carbon is 27.5%, and density is 1.21g/cm
3.
Embodiment 4:
1) batch mixing: first by the weight ratio of 1:0.02 by phenol and sodium hydroxide by being uniformly mixed, add formaldehyde subsequently, stir further and obtain mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1.8;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 1h carries out polycondensation, vacuum hydro-extraction 0.5h at 60 DEG C subsequently, and after stopping stirring, room temperature places 0.5h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 4% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
Embodiment 5:
1) batch mixing: first by the weight ratio of 1:0.12 by phenol and potassium hydroxide by being uniformly mixed, add formaldehyde subsequently, stir further and obtain mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 1.5h carries out polycondensation, vacuum hydro-extraction 3h at 60 DEG C subsequently, and after stopping stirring, room temperature places 5h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1.2 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 15% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
Embodiment 6:
1) batch mixing: first by the weight ratio of 1:0.08, phenol and ammoniacal liquor (ammoniacal liquor massfraction is 25%), by being uniformly mixed, are added formaldehyde subsequently, stirs further and obtains mixing solutions; Wherein, the mol ratio of phenol, formaldehyde is 1:1;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 3h carries out polycondensation, vacuum hydro-extraction 1.5h at 60 DEG C subsequently, and after stopping stirring, room temperature places 10h, obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1.3 by colloidal resin and ethylene glycol by being uniformly mixed, add the benzene sulfonyl chloride of colloidal resin and ethylene glycol gross weight 10% subsequently, stir further and be made into colloidal resin mixture;
4) solidify: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, is warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, the warming machine rising to 180 DEG C of insulation 16h by 60 DEG C is made as and raises 20 DEG C every 12h;
5) pyrolysis: at N
2carry out pyrolysis under protection, rise to 800 DEG C by room temperature, insulation 1h, temperature rise rate is 2 DEG C/min, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
The present invention for starting raw material, take basic cpd as the polycondensation of catalyzer adjustment phenol and formaldehyde with phenol and formaldehyde, with lower boiling ethylene glycol for pore-forming agent, by batch mixing, system material, batching, solidification, the large synthesizing porous carbon material of operation of pyrolysis five.Simultaneously by technique when composition during adjustment batch mixing and system material, the characteristic that when imparting is separated, high viscosity phase (resin carbonaceous precursor) is different, finally realize the accurate cutting of porous carbon pore character, therefore can prepare the porous carbon materials meeting numerous Application Areas demands.The method compared with prior art, on the basis of not obvious increase cost, the uncontrollability of the porous carbon pore character cutting that the difference because of the composition and structure of technical grade resin carbonaceous precursor can be avoided to a great extent to cause, promote the repeatability of porous carbon synthesis technique, realize the accurate cutting of porous carbon pore character.
Claims (7)
1. a preparation method for porous carbon materials, is characterized in that: comprise the following steps:
1) batch mixing: first phenol and basic cpd are mixed by the weight ratio of 1:0.02 ~ 1:0.12, add formaldehyde subsequently, stir, obtains mixing solutions; Wherein, phenol, formaldehyde mole ratio are 1:1 ~ 1:1.8;
2) system material: first mixing solutions is heated to 85 DEG C under whipped state, insulation 1 ~ 3h carries out polycondensation, and after subsequent dewatering, room temperature is placed, and obtains the colloidal resin with mobility;
3) prepare burden; First by the weight ratio of 1:1 ~ 1:1.5, the colloidal resin and ethylene glycol with mobility are mixed, add benzene sulfonyl chloride subsequently, stir, be made into colloidal resin mixture; Wherein, the add-on of benzene sulfonyl chloride is 4 ~ 15% of colloidal resin and ethylene glycol gross weight;
4) solidify: first colloidal resin mixture is cured, obtains cured body;
5) pyrolysis: at N
2under protection, cured body is carried out pyrolysis, rise to 800 DEG C by room temperature, insulation 1h, cools to room temperature with the furnace after completing pyrolysis, obtains porous carbon materials.
2. the preparation method of porous carbon materials according to claim 1, is characterized in that: described basic cpd is the one in sodium carbonate, sodium hydroxide, potassium hydroxide, ammoniacal liquor.
3. the preparation method of porous carbon materials according to claim 1, is characterized in that: described dehydration is vacuum hydro-extraction 0.5 ~ 3h at 60 DEG C.
4. the preparation method of porous carbon materials according to claim 1, is characterized in that: the time that described room temperature is placed is 0.5 ~ 15h.
5. the preparation method of porous carbon materials according to claim 1, it is characterized in that: described solidification detailed process is as follows: first colloidal resin mixture is heated to 50 DEG C of insulation 6h, be warmed up to 60 DEG C subsequently, then rise to 180 DEG C of insulation 16h by 60 DEG C, obtain cured body.
6. the preparation method of porous carbon materials according to claim 5, is characterized in that: rise to 180 DEG C of warming machines adopted by 60 DEG C and be made as and raise 20 DEG C every 12h.
7. the preparation method of porous carbon materials according to claim 1, is characterized in that: the temperature rise rate that described room temperature rises to 800 DEG C is 2 DEG C/min.
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Cited By (1)
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| CN106311142A (en) * | 2016-09-09 | 2017-01-11 | 上海电力学院 | Preparation method of carbon aerogel desulfurizer for high-temperature desulfuration |
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