CN104211039A - Preparation method for ellipsoidal mesoporous carbon applicable to supercapacitor materials - Google Patents
Preparation method for ellipsoidal mesoporous carbon applicable to supercapacitor materials Download PDFInfo
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- CN104211039A CN104211039A CN201310221922.0A CN201310221922A CN104211039A CN 104211039 A CN104211039 A CN 104211039A CN 201310221922 A CN201310221922 A CN 201310221922A CN 104211039 A CN104211039 A CN 104211039A
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Abstract
The invention discloses a preparation method for ellipsoidal mesoporous carbon applicable to supercapacitor materials. The method includes: taking ellipsoidal mesoporous silica as a hard template agent, filling mesoporous channels with liquid grease, conducting drying, then performing carbonization in an inert atmosphere, and removing silica, thus obtaining the ellipsoidal mesoporous carbon. The preparation method provided by the invention is easy to operate, and the obtained ellipsoidal mesoporous carbon has high ion transport properties and is suitable for supercapacitor materials.
Description
Technical field
The present invention relates to a kind of preparation method of ellipsoid shape mesoporous carbon, more particularly relating to a kind of ellipsoid shape mesoporous silicon oxide is hard mould agent, in its duct, insert grease, and carbonization is the method for corresponding pattern porous carbon under an inert atmosphere.
Background technology
The mesoporous carbon of 2-dimensional mesoscopic structure not only has large specific surface area, large pore volume and aperture, and its duct has regular two-dimensional hexagonal, and the duct of this flat shape is conducive to the transmission of electric charge.Thus mesoporous carbon is usually used for super capacitor material by people.Bibliographical information, long duct is unfavorable for mass transfer, only has short duct to be just conducive to mass transfer.And the mesoporous carbon that at present laboratory or market can provide is mainly the mesoporous carbon of CMK series, their duct is all long and be unfavorable for transferring charge.The invention provides a kind of preparation method with mesoporous ellipse Spherical Carbon compared with short-bore road, it has ellipsoid shape macro morphology, has short and orderly internal gutter simultaneously.
The method that document and patent report prepare porous carbon is a lot, but does not also have about special appearance as the preparation of ellipsoid shape mesoporous carbon is reported.Simultaneously, in document or patent, multiplex sucrose or resol etc. do carbon matrix precursor preparation, due to make of sucrose carbon matrix precursor prepare mesoporous carbon time, need to use sulfuric acid for catalyzer is by sucrose carbonization, and when doing carbon matrix precursor with resol, often need to prepare low-molecular-weight resol in advance, therefore the preparation method of above two kinds of mesoporous carbon is relatively loaded down with trivial details.And adopt grease to be the presoma of carbon, owing to there being raw material directly to buy, thus preparation method seems simple.
The ellipsoid shape mesoporous silicon oxide that the present invention synthesizes in laboratory is voluntarily hard mould agent, and when inserting grease in ellipsoid shape mesoporous silicon oxide, high temperature cabonization in inert atmosphere, finally obtains ellipsoid shape mesoporous carbon.Gained mesoporous carbon has good chemical property, goes for the material of ultracapacitor.
Summary of the invention
Be hard mould agent with axiolitic mesoporous silicon oxide, in mesopore orbit, insert liquid fat, carbonization in an inert atmosphere after oven dry, after removing silicon-dioxide, obtain axiolitic mesoporous carbon.
The object of the invention is to solve the carbon material adopted in ultracapacitor production process, the duct of its mesoporous carbon used is long and affect ion transport, and result causes electrical property to reduce.And adopt ellipsoid shape mesoporous carbon to do ultracapacitor, can address this problem well.It is low that the method has production cost, and technique is simple, and gained ellipsoid shape mesoporous carbon has the advantages such as good chemical property.
Know-why of the present invention:
The preparation method of a kind of ellipsoid shape mesoporous carbon of the present invention.Namely be hard mould agent with axiolitic mesoporous silicon oxide, filling liquid grease in its mesopore orbit, carbonization in an inert atmosphere after oven dry, obtains mesoporous carbon/silica composite, then with the removing such as sodium hydroxide or hydrofluoric acid silicon-dioxide, axiolitic mesoporous carbon is obtained.
Technical scheme of the present invention:
A preparation method for ellipsoid shape mesoporous carbon, comprises the steps:
(1), liquid fat is dissolved in ethanol, add axiolitic mesoporous silicon oxide micro-and nano-particles, wherein the mass ratio of liquid fat and silicon-dioxide micro-and nano-particles is 0.5-1.5:1, be preferably 0.8-1.2:1, leave standstill until ethanol volatilization is dry after stirring, then constant temperature 12-48h under 18-50 degree, namely obtains grease/silica composite.
Described ellipsoid shape mesoporous silicon oxide, its major axis is 0.45 ~ 4.0 micron, and minor axis is 0.3 ~ 0.8 micron, and ratio and the axial ratio of major axis and minor axis are 1.5 ~ 5.0.Preferred major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36.
Described liquid fat is one or more mixed solution of soybean oil, peanut oil, sunflower seed oil, honey, rapeseed oil, cotton seed oil.
(2), grease/silica composite at high temperature roasting of will obtaining in step (1), control between maturing temperature 400-1000 DEG C, preferentially between 600-1000 DEG C, carry out roasting, roasting time is 2-12h, naturally cools to room temperature; Axiolitic carbon/silicon-dioxide micro-and nano-particles can be obtained;
(3) the axiolitic carbon/silicon-dioxide micro-and nano-particles of step (2) is put into (ratio being 1:10 according to mass/volume ratio (mixture: solution)) in the sodium hydroxide of 2 mol.L-1 or the hydrofluoric acid solution of 1 mol.L-1, stir 24 hours.
(4) filtered by the mixture of step (3), and constantly spend deionized water washings to pH in neutral, then air drying, namely obtains ellipsoid shape mesoporous carbon.
Had wide practical use in ultracapacitor field by the ellipsoid shape mesoporous carbon of gained of the present invention.
Beneficial effect of the present invention:
The preparation method of a kind of ellipsoid shape mesoporous carbon of the present invention, owing to being utilize ellipsoid shape mesoporous silicon oxide to do hard mould agent, be carbon matrix precursor with common liquid fat, but high temperature cabonization forms under inert atmosphere, owing to remaining duct shorter in mesoporous carbon, thus there is good chemical property.Working method is simple, with low cost, can repeat.
Accompanying drawing illustrates:
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
Fig. 1 is the scanning electron microscope image of mesoporous class ball carbon.
Fig. 2 is the little angle X-ray diffracting spectrum of ellipsoid shape mesoporous carbon.
Fig. 3 is the graph of pore diameter distribution of ellipsoid shape mesoporous carbon.
Fig. 4 is the cyclic voltammetry curve figure of ellipsoid shape mesoporous carbon.Test condition: sample is arrived 0.2V scope internal recycle relative to saturated calomel electrode electrode-0.5 at potential windows with certain scanning speed in 3M KOH electrolyte solution.
Embodiment
Below by way of specific embodiment, also the invention will be further described by reference to the accompanying drawings, but the present invention is not limited to following examples.
Described method if no special instructions, is ordinary method.Described material if no special instructions, all can be bought from open commercial sources and obtain.
Pattern anisotropic ellipsoid shape mesoporous silicon oxide micro-and nano-particles synthesizes according to following patent: the .CN101850984A such as Shen Shaodian: a kind of ellipsoid shape mesoporous silica molecular sieve and preparation method thereof synthesis [P] .2010-10-06.
Embodiment 1
A preparation method for ellipsoid shape mesoporous carbon, comprises the steps:
(1) soybean oil 0.5 gram, is taken, join in 1 gram of ellipsoid shape mesoporous silicon oxide (major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36), be placed on after stirring in 18 degree of air and dry, namely obtain soybean oil/silica composite;
(2), in nitrogen atmosphere, soybean oil/the silica composite of step (1) gained is placed in retort furnace (DC-B8/11 type, Beijing original creation Science and Technology Ltd.) in be slowly warming up to 600 DEG C from room temperature, and at such a temperature after roasting 2h, naturally cool to room temperature; Axiolitic carbon/SiO2 micro-and nano-particles;
(3), the mixture that obtains after step (2) roasting puts into the sodium hydroxide solution (ratio being 1:10 according to mass/volume ratio (mixture: solution)) of 2 mol.L-1, stirs 24 hours;
(4) filtered by the mixture of step (3), and constantly spend deionized water washings to pH in neutral, then air drying, namely obtains ellipsoid shape mesoporous carbon.
By above-mentioned ellipsoid shape mesoporous carbon scanning electron microscopic observation, obtain the electromicroscopic photograph of accompanying drawing 1, visible sample still keeps ellipsoid shape.
Ellipsoid shape mesoporous carbon is little angle XRD test, sees Fig. 2, mesoporous carbon sample has obvious diffraction peak, through confirming as two-dimensional hexagonal structure angle of diffraction about 1.1,1.8 and 2.2 degree.
Carry out nitrogen adsorption-desorption test to ellipsoid shape mesoporous carbon, see Fig. 3, the uniform pore diameter of sample is distributed in about 7.7 nm.
The electrical property of ellipsoid shape mesoporous carbon is tested, sees Fig. 4, the cyclic voltammetry curve figure of the electrode prepared with ellipsoid shape meso-porous carbon material in the KOH of 6.0 mol.L-1.As can be seen from the figure, the redox processes substantially symmetrically state of this electrode, forms accurate rectangular configuration, illustrates that this electrode embodies good capacitive characteristics.The large current density electrical feature that this electrode has had is described.This material is expected to material as ultracapacitor for the preparation of ultracapacitor.
Embodiment 2
A preparation method for ellipsoid shape mesoporous carbon, comprises the steps:
(1) peanut grease 1.0 grams, is taken, join in 1.0 grams of ellipsoid shape mesoporous silicon oxides (major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36), be placed on after stirring in 25 degree of air and dry, namely obtain peanut grease/silica composite;
(2), in argon gas atmosphere, peanut grease/the silica composite of step (1) gained is placed in retort furnace (DC-B8/11 type, Beijing original creation Science and Technology Ltd.) in be slowly warming up to 800 DEG C from room temperature, and at such a temperature after roasting 4h, naturally cool to room temperature; Axiolitic carbon/SiO2 micro-and nano-particles;
(3), the mixture that obtains after step (2) roasting puts into the hydrofluoric acid solution (ratio being 1:10 according to mass/volume ratio (mixture: solution)) of 1 mol.L-1, stirs 24 hours;
(4) filtered by the mixture of step (3), and constantly spend deionized water washings to pH in neutral, then air drying, namely obtains ellipsoid shape mesoporous carbon.
Embodiment 3
A preparation method for ellipsoid shape mesoporous carbon, comprises the steps:
(1) honey 15 grams, is taken, join in 10 grams of ellipsoid shape mesoporous silicon oxides (major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36), be placed on after stirring in 50 degree of air and dry, namely obtain honey/silica composite;
(2), in nitrogen atmosphere, honey/the silica composite of step (1) gained is placed in retort furnace (DC-B8/11 type, Beijing original creation Science and Technology Ltd.) in be slowly warming up to 1000 DEG C from room temperature, and at such a temperature after roasting 12h, naturally cool to room temperature; Axiolitic carbon/SiO2 micro-and nano-particles;
(3), the mixture that obtains after step (2) roasting puts into the sodium hydroxide solution (ratio being 1:10 according to mass/volume ratio (mixture: solution)) of 2 mol.L-1, stirs 24 hours;
(4) filtered by the mixture of step (3), and constantly spend deionized water washings to pH in neutral, then air drying, namely obtains ellipsoid shape mesoporous carbon.
Claims (8)
1. one kind has higher chemical property, can be used for the preparation method of the ellipsoid shape mesoporous carbon of super capacitor material, it is characterized in that: adopt ellipsoid shape mesoporous silicon oxide to be hard mould agent, liquid fat is inserted in wherein duct, after oven dry, carbonization under an inert atmosphere, then removes silicon-dioxide, finally obtains axiolitic mesoporous carbon.
2. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, it is characterized in that: described ellipsoid shape mesoporous silicon oxide, its major axis is 0.45 ~ 4.0 micron, and minor axis is 0.3 ~ 0.8 micron, and ratio and the axial ratio of major axis and minor axis are 1.5 ~ 5.0.
3. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, is characterized in that: described liquid fat is one or more mixed solution of soybean oil, peanut oil, sunflower seed oil, honey, rapeseed oil, cotton seed oil.
4. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, is characterized in that: described hard mould agent--axiolitic mesoporous silica particles, its major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36.
5. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, is characterized in that: the mass ratio between liquid fat used in described preparation process and ellipsoid shape mesoporous silicon oxide is 0.5-1.5.
6. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, it is characterized in that: described bake out temperature, its bake out temperature controls between 18-50 degree.
7. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, is characterized in that: the atmosphere in described carbonization process, adopts inert atmosphere and nitrogen or argon shield in carbonization process.
8. the preparation method of ellipsoid shape mesoporous carbon as claimed in claim 1, it is characterized in that: the carbonization temperature in described carbonization process, its carbonization temperature is at 400-1000 degree.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111924825A (en) * | 2020-09-08 | 2020-11-13 | 中国石油化工股份有限公司 | Porous carbon material and method for preparing porous carbon material by using catalytic cracking diesel oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1948148A (en) * | 2006-11-11 | 2007-04-18 | 大连理工大学 | Method of preparing ordered structure mesopore carbon using asphalt vinyl matter as raw material |
| CN102295281A (en) * | 2011-06-21 | 2011-12-28 | 华东理工大学 | Method for preparing graded porous carbon with hollow mesoporous silicon spheres as templates |
| CN103072970A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Spherical hollow mesoporous carbon shell and preparing method thereof |
| CN103086346A (en) * | 2011-10-28 | 2013-05-08 | 沈阳药科大学 | Preparation method and applications of mesoporous carbon |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948148A (en) * | 2006-11-11 | 2007-04-18 | 大连理工大学 | Method of preparing ordered structure mesopore carbon using asphalt vinyl matter as raw material |
| CN102295281A (en) * | 2011-06-21 | 2011-12-28 | 华东理工大学 | Method for preparing graded porous carbon with hollow mesoporous silicon spheres as templates |
| CN103086346A (en) * | 2011-10-28 | 2013-05-08 | 沈阳药科大学 | Preparation method and applications of mesoporous carbon |
| CN103072970A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Spherical hollow mesoporous carbon shell and preparing method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111924825A (en) * | 2020-09-08 | 2020-11-13 | 中国石油化工股份有限公司 | Porous carbon material and method for preparing porous carbon material by using catalytic cracking diesel oil |
| CN111924825B (en) * | 2020-09-08 | 2021-12-17 | 中国石油化工股份有限公司 | Porous carbon material and method for preparing porous carbon material by using catalytic cracking diesel oil |
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Application publication date: 20141217 |