CN105271176A - Mesoporous carbon material and manufacturing method thereof - Google Patents
Mesoporous carbon material and manufacturing method thereof Download PDFInfo
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- CN105271176A CN105271176A CN201510787918.XA CN201510787918A CN105271176A CN 105271176 A CN105271176 A CN 105271176A CN 201510787918 A CN201510787918 A CN 201510787918A CN 105271176 A CN105271176 A CN 105271176A
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Abstract
The invention discloses a mesoporous carbon material. The mesoporous carbon material is prepared from one or more types of nitrogenous macromolecular polymers or carbonized products of nitrogenous macromolecular polymers through a fused salt method without depending on mesoporous mold plates. The carbon material is of a classified porous three-dimensional structure and comprises micropores, mesopores and large holes. The mesoporous structure is a three-dimensional structure formed by stacking extremely-thin graphite-like carbon layers. The BET specific surface area of the carbon material is 2000-4000 m<2>/g, the pore volume of the large micropores and the mesopores (the aperture ranges from 1 nm to 50 nm) accounts for 80% or higher of the total pore volume, the pore size distribution is narrow and is concentrated to be 1-5 nm, and the average aperture is 2-4 nm. The preparation process of the material does not depend on any mold plate, raw materials are wide in source, the preparation method is simple, cost is low, engineered amplification can be achieved, and continuous production can be achieved.
Description
Technical field
The present invention relates to a kind of rich meso-porous carbon material and preparation method thereof, belong to Material Field.
Background technology
Meso-porous carbon material refers to the carbon material with mesopore orbit structure, and its aperture is at 2nm to 50nm, and it has relatively homogeneous pore passage structure, narrower pore size distribution and higher specific surface area and mesoporous pore volume.Therefore, meso-porous carbon material is relating to the adsorption/desorption of macromole and heavy ion group, has broad application prospects during high rate of diffusion problem.At biological technical field, meso-porous carbon material is used to absorption and is separated organic macromolecule, biomacromolecule and heavy metal ion.Meso-porous carbon material can also be used to environment purification, decomposing organic waste, carries out gas adsorption, vehicle maintenance service and purification of water quality.In Conversion of energy field, meso-porous carbon material can be used to the carrier making catalyzer, prepares efficient catalyzed reaction electrode.Particularly in energy storage field, meso-porous carbon material has innate advantage as the electrode material for electric double layer capacitor of adsorption/desorption heavy ion group.First meso-porous carbon material has bigger serface, adsorbable and hold more current carrier, more electrochemical reaction active sites is provided, mean higher specific storage, its relatively large pore passage structure, be conducive to the adsorption/desorption speed improving heavy ion group (about 1nm ionic diameter), realize the high power density of electrical condenser.Secondly, by force, in organic electrolyte and il electrolyte, electrochemical properties is stablized, and can bear higher voltage for the solidity to corrosion of meso-porous carbon material and resistant to elevated temperatures performance, is used for manufacturing high-voltage energy storage device, to meet high-energy service requirements.Again, meso-porous carbon material has high electronic conductivity usually, can carry larger current density, maintains higher electron transfer rate at electrode surface, while guarantee energy storage device high power density, can not sacrifice its capacity.Therefore meso-porous carbon material is used in the electrostatic double layer positive pole of lithium-ion capacitor, the electrode of organic system or ionic liquid double layer capacitor, all shows higher specific storage and excellent cycle performance.But meso-porous carbon material preparation process is complicated, and cost is high, is substantially all by first making mesoporous template, then the method adding carbon matrix precursor obtains.This mesoporous template comprises the Pluronic etc. of mesoporous silicon oxide (MCM-41, SBA-l, SBA-l5, FDU-5 etc.), polystyrene colloidal state particle, CeO2 nanoparticle, three blocks, these are sacrificed template and cannot reuse in preparation, further increase cost.Therefore, the technology still lacking a kind of mass-producing and through engineering approaches so far effectively controls the pore passage structure of nano-carbon material, to guarantee the consistence of nano-carbon material product in enormous quantities on chemical property.
Summary of the invention
The object of the invention is to invent and prepare a kind of rich meso-porous carbon material of low cost, first, its BET specific surface area is greater than 2000m2/g, and the pore volume being greater than the hole of 1nm accounts for more than 80% of total pore volume, and pore size distribution is narrow, concentrate on 1-5nm, its mean pore size is at 2-4nm.Secondly, the preparation process of this material does not rely on any template, and raw material sources are extensive, and preparation method is simple, with low cost, through engineering approaches can amplify, and can realize continuous prodution.
Object of the present invention is achieved through the following technical solutions: a kind of rich meso-porous carbon material, and this carbon material is a kind of carbon material of classifying porous three-dimensional structure, and wherein containing micropore, mesoporous and large micropore composition, its large micropore and mesoporous aperture are 1-50nm.
Of the present invention enter an improvement be: meso-hole structure be by very thin class Graphene carbon-coating pile up three-dimensional structure.
Of the present invention enter an improvement be: rich meso-porous carbon material BET specific surface area is at 3000-4000m
2/ g, its large micropore and mesoporous pore volume account for more than 80% of total pore volume, and pore size distribution is narrow, concentrates on 1-5nm, and its mean pore size is at 2-4nm.
Of the present invention enter an improvement be: meso-hole structure is the three-dimensional structure of being piled up by very thin class Graphene carbon-coating, and wherein, described carbon-coating is amorphous carbon thin layer or containing the class Graphene thin layer of a large amount of defect.
Of the present invention enter an improvement be: rich meso-porous carbon material is obtained through molte-salt synthesis by one or more nitrogenous high molecular polymers or its carbonized product.
Of the present invention enter an improvement be: molte-salt synthesis is mixed by the salt of carbonaceous material with molten state, reacts 10 minutes after-12 hours, obtain rich meso-porous carbon material under the high temperature of 500 DEG C-1100 DEG C.
Of the present invention enter an improvement be: by one or more nitrogenous high molecular polymers at 500-800 DEG C of carbonization 0-180 minute, the carbonized product of gained presses the mass ratio mixing of 1:0.5-6 with the salt of molten state, heating and melting, 10 minutes are reacted after-12 hours under the high temperature of 500 DEG C-1100 DEG C, cooling, adopt whizzer washing and filtering, after vacuum-drying, obtain rich meso-porous carbon material.
Of the present invention enter an improvement be: nitrogen containing polymer polymkeric substance is obtained by one or more nitrogenous monomer polymerizations.
Of the present invention enter an improvement be: carbonized product is the nitrogenous polymkeric substance product after high-temperature hot reason, and temperature is greater than 500 DEG C.
Of the present invention enter an improvement be: melting salt is the mixing of one or more salt in muriate, oxyhydroxide, carbonate, oxygen-carrying ion liquid.
The present invention compared with prior art has the following advantages: the present invention is rich, and meso-porous carbon material BET specific surface area is greater than 2000m
2/ g, and the pore volume being greater than the hole of 1nm accounts for more than 80% of total pore volume, and pore size distribution is narrow, concentrates on 1-5nm, its mean pore size is at 2-4nm; Secondly, the preparation process of this material does not rely on any template, and raw material sources are extensive, and preparation method is simple, with low cost, through engineering approaches can amplify, and can realize continuous prodution.
accompanying drawing illustrates:
Fig. 1 is the transmission electron microscope picture of the three-dimensional carbon Rotating fields of this rich meso-porous carbon material.
Fig. 2 is the high magnification scanning electron microscopy of the rich meso-porous carbon material in example 1.
Fig. 3 is the graph of pore diameter distribution of the rich meso-porous carbon material in example 1, calculates acquisition by the data of nitrogen desorption curve through non-local density functional theory (NL-DFT).
Fig. 4 is the scanning electron microscopy of the rich meso-porous carbon material in example 2.
Fig. 5 is the scanning electron microscopy of the rich meso-porous carbon material in example 3.
embodiment:
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.The element described in one embodiment of the invention and feature can combine with the element shown in one or more other embodiment and feature.It should be noted that for purposes of clarity, in explanation, eliminate expression and the description of unrelated to the invention, parts known to persons of ordinary skill in the art and process.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not paying creative work, all belongs to the scope of protection of the invention.
A kind of rich meso-porous carbon material and preparation method thereof, this rich meso-porous carbon material is obtained through molte-salt synthesis by one or more nitrogenous high molecular polymers or its carbonized product, does not rely on mesoporous template.This carbon material is a kind of carbon material of classifying porous three-dimensional structure, wherein containing a small amount of micropore, in a large number mesoporous and a small amount of macropore composition.Meso-hole structure is wherein the three-dimensional structure of being piled up by very thin class Graphene carbon-coating.This carbon material BET specific surface area is at 2000-4000m
2/ g, the pore volume of its large micropore and mesoporous (aperture is at 1-50nm) accounts for more than 80% of total pore volume, and pore size distribution is narrow, concentrates on 1-5nm, and its mean pore size is at 2-4nm.
Nitrogenous high molecular polymer is obtained by one or more nitrogenous monomer polymerizations, and carbonized product is the nitrogenous product of polymkeric substance after high temperature (being greater than 500 DEG C) heat reason.Molte-salt synthesis is by the mixing of carbonaceous material with one or more salt in the muriate of molten state, oxyhydroxide, carbonate, oxygen-carrying ion liquid, reacts 10 minutes after-12 hours, obtain rich meso-porous carbon material under the high temperature of 500-1100 DEG C.The carbon-coating forming the three-dimensional structure of rich mesoporous carbon is amorphous carbon thin layer or the class Graphene thin layer containing a large amount of defect.
Below in conjunction with specific embodiment, technical scheme of the present invention is described further:
Embodiment 1
By 100kg polystyrene 750 DEG C of carbonizations 10 minutes, the same sodium-chlor of carbonized product of gained, calcium hydroxide and Repone K press the mass ratio mixing of 1:1:1:1, heating and melting, react 30 minutes at 900 DEG C, cooling, adopts whizzer washing and filtering, after vacuum-drying, obtain the rich meso-porous carbon material of 18kg, as shown in Figure 2.Brunauer-Emmett-Teller (BET) specific surface area that this carbon material records through nitrogen adsorption detachment assays is 3312m2/g, its pore size distribution and corresponding pore volume calculate acquisition by the data of nitrogen desorption curve through non-local density functional theory (NL-DFT), as shown in Figure 3, the large micropore and the mesoporous pore volume that are wherein greater than 1nm account for 91.4% of total pore volume, and its mean pore size is 2.3nm.
Embodiment 2
Same for 200kg polypyrrole ammonium chloride, sodium hydroxide and magnesium chloride are pressed the mass ratio mixing of 1:1:2:1, heating and melting, reacts 3 hours at 1000 DEG C, and cooling adopts whizzer washing and filtering, after vacuum-drying, obtains the rich meso-porous carbon material of 60kg, as shown in Figure 4.Brunauer-Emmett-Teller (BET) specific surface area that this carbon material records through nitrogen adsorption detachment assays is 3503m2/g, its pore size distribution and corresponding pore volume calculate acquisition by the data of nitrogen desorption curve through non-local density functional theory (NL-DFT), the large micropore and the mesoporous pore volume that are wherein greater than 1nm account for 82% of total pore volume, and its mean pore size is 2.1nm.
Embodiment 3
150kg is gathered dially phthalate 1000 DEG C of carbonizations 2 hours, same lithium hydroxide, zinc hydroxide and calcium chloride press the mass ratio mixing of 1:1:2:3, heating and melting, react 1.5 hours at 700 DEG C, cooling, adopts whizzer washing and filtering, after vacuum-drying, obtain the rich meso-porous carbon material of 52kg, as shown in Figure 5.Brunauer-Emmett-Teller (BET) specific surface area that this carbon material records through nitrogen adsorption detachment assays is 2985m2/g, its pore size distribution and corresponding pore volume calculate acquisition by the data of nitrogen desorption curve through non-local density functional theory (NL-DFT), the large micropore and the mesoporous pore volume that are wherein greater than 1nm account for 87.3% of total pore volume, and its mean pore size is 2.6nm.
Although last it is noted that described the present invention and advantage thereof in detail above, be to be understood that and can carry out various change when not exceeding the spirit and scope of the present invention limited by appended claim, substituting and converting.And scope of the present invention is not limited only to the specific embodiment of process, equipment, means, method and step described by specification sheets.One of ordinary skilled in the art will readily appreciate that from disclosure of the present invention, can use perform the function substantially identical with corresponding embodiment described herein or obtain and its substantially identical result, existing and that will be developed in the future process, equipment, means, method or step according to the present invention.Therefore, appended claim is intended to comprise such process, equipment, means, method or step in their scope.
Claims (10)
1. a rich meso-porous carbon material, is characterized in that: this carbon material is a kind of carbon material of classifying porous three-dimensional structure, and wherein containing micropore, mesoporous and large micropore composition, its large micropore and mesoporous aperture are 1-50nm.
2. the rich meso-porous carbon material of one according to claim 1, is characterized in that: meso-hole structure is the three-dimensional structure of being piled up by very thin class Graphene carbon-coating.
3. the rich meso-porous carbon material of one according to claim 1 and 2, is characterized in that: described rich meso-porous carbon material BET specific surface area is at 3000-4000m
2/ g, its large micropore and mesoporous pore volume account for more than 80% of total pore volume, and pore size distribution is narrow, concentrates on 1-5nm, and its mean pore size is at 2-4nm.
4. the rich meso-porous carbon material of one according to claim 1, it is characterized in that: described meso-hole structure is the three-dimensional structure of being piled up by very thin class Graphene carbon-coating, wherein, described carbon-coating is amorphous carbon thin layer or the class Graphene thin layer containing a large amount of defect.
5. a manufacture method for rich meso-porous carbon material, is characterized in that: rich meso-porous carbon material is obtained through molte-salt synthesis by one or more nitrogenous high molecular polymers or its carbonized product.
6. the manufacture method of a kind of rich meso-porous carbon material according to claim 5, is characterized in that: molte-salt synthesis is mixed by the salt of carbonaceous material with molten state, reacts 10 minutes after-12 hours, obtain rich meso-porous carbon material under the high temperature of 500 DEG C-1100 DEG C.
7. the manufacture method of a kind of rich meso-porous carbon material according to claim 5 or 6, it is characterized in that: by one or more nitrogenous high molecular polymers at 500-800 DEG C of carbonization 0-180 minute, the carbonized product of gained presses the mass ratio mixing of 1:0.5-6 with the salt of molten state, 10 minutes are reacted after-12 hours under the high temperature of 500 DEG C-1100 DEG C, cooling, adopt whizzer washing and filtering, after vacuum-drying, obtain rich meso-porous carbon material.
8. the manufacture method of a kind of rich meso-porous carbon material according to claim 5, is characterized in that: described nitrogen containing polymer polymkeric substance is obtained by one or more nitrogenous monomer polymerizations.
9. the manufacture method of a kind of rich meso-porous carbon material according to claim 5, is characterized in that: described carbonized product is the nitrogenous product of polymkeric substance after high-temperature hot reason, and temperature is greater than 500 DEG C.
10. the manufacture method of a kind of rich meso-porous carbon material according to claim 5, is characterized in that: melting salt is the mixing of one or more salt in muriate, oxyhydroxide, carbonate, oxygen-carrying ion liquid.
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| PCT/CN2016/081799 WO2017084251A1 (en) | 2015-11-17 | 2016-05-12 | Mesoporous carbon material and manufacturing method therefor |
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| CN105618015A (en) * | 2016-03-18 | 2016-06-01 | 西北师范大学 | Preparation of three-dimensional mesoporous carbon composite material and application of composite material as solid-phase micro-extraction fiber coating material |
| WO2017084251A1 (en) * | 2015-11-17 | 2017-05-26 | 南通绿业中试技术研究院有限公司 | Mesoporous carbon material and manufacturing method therefor |
| CN106744803A (en) * | 2017-01-23 | 2017-05-31 | 深圳大学 | A kind of method and porous carbon for preparing porous carbon |
| CN106865546A (en) * | 2017-01-23 | 2017-06-20 | 北京大学深圳研究生院 | A kind of mesoporous micro-pore carbon material and its preparation method and application |
| WO2019078073A1 (en) * | 2017-10-16 | 2019-04-25 | 積水化学工業株式会社 | Composite body, electrode material for electricity storage devices, and electricity storage device |
| WO2021060243A1 (en) * | 2019-09-24 | 2021-04-01 | 積水化学工業株式会社 | Carbon material and electrode material for power storage device |
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| WO2017084251A1 (en) * | 2015-11-17 | 2017-05-26 | 南通绿业中试技术研究院有限公司 | Mesoporous carbon material and manufacturing method therefor |
| CN105618015A (en) * | 2016-03-18 | 2016-06-01 | 西北师范大学 | Preparation of three-dimensional mesoporous carbon composite material and application of composite material as solid-phase micro-extraction fiber coating material |
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| WO2019078073A1 (en) * | 2017-10-16 | 2019-04-25 | 積水化学工業株式会社 | Composite body, electrode material for electricity storage devices, and electricity storage device |
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| WO2021060243A1 (en) * | 2019-09-24 | 2021-04-01 | 積水化学工業株式会社 | Carbon material and electrode material for power storage device |
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Application publication date: 20160127 |