CN106976865A - A kind of meso-porous carbon material and preparation method thereof - Google Patents
A kind of meso-porous carbon material and preparation method thereof Download PDFInfo
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- CN106976865A CN106976865A CN201710378313.4A CN201710378313A CN106976865A CN 106976865 A CN106976865 A CN 106976865A CN 201710378313 A CN201710378313 A CN 201710378313A CN 106976865 A CN106976865 A CN 106976865A
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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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention discloses a kind of meso-porous carbon material and preparation method thereof.The preparation method of the present invention is comprised the following steps that：Mesoporous nano silicon dioxide is scattered in polar non-solute first, ultrasonically treated 2 5h obtains dispersion liquid；Then Kynoar is dissolved in dispersion liquid at 20~80 DEG C, stirs 4~24h, 1~5h of baking oven standing is put into afterwards and obtains uniform casting solution；Primary membrane is immersed in 5min in coagulating bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film by casting solution by blade applicator blade coating generation primary membrane.Polyvinylidene fluoride film obtains carbon material by high temperature cabonization, eventually passes hydrofluoric acid wash, obtains meso-porous carbon material.Meso-porous carbon material prepared by the present invention has big specific surface area, and homogeneous pore passage structure has a good application prospect in fields such as lithium ion battery, ultracapacitors.
Description
Technical field
The present invention relates to a kind of mesoporous carbon and preparation method thereof, belong to technical field of nano material.
Background technology
With the surge and industrialized development of population, substantial amounts of fossil fuels (such as coal, oil, natural gas) burning and
The influence of the mankind's activities such as green vegetation reduction so that environmental pollution and energy crisis turn into what human kind sustainable development was faced
Two big challenges.Fossil fuels are non-renewable resources, the need for can not meeting economic long-run development, and these traditional fossils
The burning of the energy can bring serious environmental problem.Therefore, reproducible cleaning new energy is developed, the sustainable development of industry is realized
Exhibition is reached common understanding in the world.
Porous carbon materials because with high specific surface area and excellent physicochemical properties be widely used in catalyst carrier,
In terms of separation material and advanced electronic material.The common method of synthesizing porous carbon material includes organogel carbonizatin method, catalysis
Activation method and polymer carbonization method etc..The most specific surface areas of porous carbon materials prepared by these methods are low, and aperture is non-adjustable and not
It is homogeneous.In recent years, porous carbon preparation method achieves some new breakthroughs, with silica gel, zeolite molecular sieve, metal organic framework material
It is precursor template to expect (MOFs), has prepared high-specific surface area and orderly meso-porous nano carbon material, in gas selection absorption, storage
Preferable performance is shown in terms of hydrogen, electrochemistry and catalysis, one of this area study hotspot is had become.
The content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of preparation method is simple, Large ratio surface
Long-pending meso-porous carbon material and preparation method thereof.
The technical solution adopted in the present invention is specifically described as follows.
The present invention provides a kind of preparation method of meso-porous carbon material, comprises the following steps that：
(1) mesoporous nano silicon dioxide is scattered in polar non-solute, ultrasonically treated 2-5h obtains dispersion liquid；
(2) Kynoar is added in dispersion liquid, 4~24h is stirred at a temperature of 20~80 DEG C, baking oven is placed into quiet
Put 1~5h and obtain uniform casting solution；
(3) casting solution by blade applicator blade coating generation primary membrane, primary membrane is immersed in coagulating bath, be then transferred to from
Film-forming is soaked in sub- water-bath, is dried naturally, polyvinylidene fluoride film is obtained；
(4) polyvinylidene fluoride film obtains carbon material by carbonization, passes through hydrofluoric acid wash again afterwards, obtains mesoporous carbon materials
Material.
In the present invention, described polar non-solute is DMF.
In the present invention, Kynoar, mesoporous nano silicon dioxide, the weight ratio of polar non-solute are (10-18):
(2-5):(70-84)。
In the present invention, in step (2), whipping temp is 60~70 DEG C, and mixing time is 10~12h.
In the present invention, in step (3), coagulating bath is 0~60wt% ethanol solution.Coagulating bath is 0~60wt% second
Alcoholic solution；Primary membrane is immersed in 4~6min in coagulating bath；It is transferred in deionization water-bath and soaks 3~5 days.
In the present invention, in step (4), carburizing temperature is 600-900 DEG C, and carbonization time is 1.5~3h.
In the present invention, in step (4), described hydrofluoric acid concentration is 10%.
The present invention further provides the meso-porous carbon material that a kind of above-mentioned preparation method is obtained.
Compared to the prior art, the beneficial effects of the present invention are：
The present invention prepares the mesoporous carbon of high-specific surface area by mesoporous nano silicon dioxide and the proportion of Kynoar
Material.The inventive method preparation method is simple, and the carbon material of preparation has in fields such as ultracapacitor, lithium ion battery, catalysis
There is good application prospect.
Brief description of the drawings
Fig. 1 is the adsorption desorption curve map that the embodiment of the present invention 1 obtains nitrogen-doped porous carbon material.
Fig. 2 is the graph of pore diameter distribution that the embodiment of the present invention 1 obtains nitrogen-doped porous carbon material.
Embodiment
The following examples can make those skilled in the art that the present invention is more fully understood, but not limit in any form
The present invention.
Embodiment 1
2g mesoporous nano silicon dioxides are scattered in 41g DMF solvents first, ultrasonically treated 2h,
Obtain dispersion liquid；Then 7g Kynoar is dissolved in dispersion liquid at 70 DEG C, stirs 12h, baking oven standing is put into afterwards
3h obtains uniform casting solution；Casting solution is by blade applicator blade coating generation primary membrane, and the ethanol that primary membrane is immersed in into 50% coagulates
Gu 5min in bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film.It is poly- inclined
Fluoride film is 800 DEG C by high temperature cabonization, carburizing temperature, and the time is 2h, obtains carbon material, passes through 10% hydrogen fluorine again afterwards
Acid elution, obtains meso-porous carbon material.The specific surface area of the meso-porous carbon material is 812m2/ g, mean pore size is 7.4nm, Fig. 1
For the adsorption desorption curve map of the meso-porous carbon material, Fig. 2 is the graph of pore diameter distribution of the meso-porous carbon material.
Embodiment 2
1g mesoporous nano silicon dioxides are scattered in 41g DMF solvents first, ultrasonically treated 2h,
Obtain dispersion liquid；Then 8g Kynoar is dissolved in dispersion liquid at 70 DEG C, stirs 12h, baking oven standing is put into afterwards
3h obtains uniform casting solution；Casting solution is by blade applicator blade coating generation primary membrane, and the ethanol that primary membrane is immersed in into 50% coagulates
Gu 5min in bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film.It is poly- inclined
Fluoride film is 600 DEG C by high temperature cabonization, carburizing temperature, and the time is 2h, obtains carbon material, passes through 10% hydrogen fluorine again afterwards
Acid elution, obtains meso-porous carbon material.The specific surface area of the meso-porous carbon material is 723m2/ g, mean pore size is 6.4nm.
Embodiment 3
2.5g mesoporous nano silicon dioxides are scattered in 41g DMF solvents first, it is ultrasonically treated
2h, obtains dispersion liquid；Then 6.5g Kynoar is dissolved in dispersion liquid at 70 DEG C, stirs 12h, baking oven is put into afterwards
Stand 3h and obtain uniform casting solution；Casting solution generates primary membrane by blade applicator blade coating, and primary membrane is immersed in 50% second
5min in alcohol coagulating bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film.
Polyvinylidene fluoride film is 900 DEG C by high temperature cabonization, carburizing temperature, and the time is 2h, obtains carbon material, afterwards again by 10%
Hydrofluoric acid wash, obtains meso-porous carbon material.The specific surface area of the meso-porous carbon material is 762m2/ g, mean pore size is
9.7nm。
Embodiment 4
1.5g mesoporous nano silicon dioxides are scattered in 41g DMF solvents first, it is ultrasonically treated
2h, obtains dispersion liquid；Then 7.5g Kynoar is dissolved in dispersion liquid at 70 DEG C, stirs 12h, baking oven is put into afterwards
Stand 3h and obtain uniform casting solution；Casting solution generates primary membrane by blade applicator blade coating, and primary membrane is immersed in 50% second
5min in alcohol coagulating bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film.
Polyvinylidene fluoride film is 700 DEG C by high temperature cabonization, carburizing temperature, and the time is 2h, obtains carbon material, afterwards again by 10%
Hydrofluoric acid wash, obtains meso-porous carbon material.The specific surface area of the meso-porous carbon material is 786m2/ g, mean pore size is
7.0nm。
Embodiment 5
2g mesoporous nano silicon dioxides are scattered in 41g DMF solvents first, ultrasonically treated 2h,
Obtain dispersion liquid；Then 7g Kynoar is dissolved in dispersion liquid at 70 DEG C, stirs 12h, baking oven standing is put into afterwards
3h obtains uniform casting solution；Casting solution is by blade applicator blade coating generation primary membrane, and the ethanol that primary membrane is immersed in into 50% coagulates
Gu 5min in bath, is then transferred to 4 days film-formings of immersion in deionization water-bath, dries naturally, obtain polyvinylidene fluoride film.It is poly- inclined
Fluoride film is 900 DEG C by high temperature cabonization, carburizing temperature, and the time is 2h, obtains carbon material, passes through 10% hydrogen fluorine again afterwards
Acid elution, obtains meso-porous carbon material.The specific surface area of the meso-porous carbon material is 802m2/ g, mean pore size is 7.8nm.
Described above is only the citing of embodiments of the present invention, it is noted that made according to technical scheme
Any equivalent transformation, protection scope of the present invention all should be belonged to.
Claims (8)
1. a kind of preparation method of meso-porous carbon material, it is characterised in that comprise the following steps that：
(1) mesoporous nano silicon dioxide is scattered in polar non-solute, ultrasonically treated 2-5h obtains dispersion liquid；
(2) Kynoar is added in dispersion liquid, 4~24h is stirred at a temperature of 20~80 DEG C, placed into baking oven and stand 1
~5h obtains uniform casting solution；
(3) primary membrane is immersed in coagulating bath by blade applicator blade coating generation primary membrane, is then transferred to deionized water by casting solution
Film-forming is soaked in bath, is dried naturally, polyvinylidene fluoride film is obtained；
(4) polyvinylidene fluoride film obtains carbon material by carbonization, passes through hydrofluoric acid wash again afterwards, obtains meso-porous carbon material.
2. preparation method according to claim 1, it is characterised in that in step (1), described polar non-solute is
N,N-dimethylformamide.
3. preparation method according to claim 1, it is characterised in that Kynoar, mesoporous nano silicon dioxide, polarity
The weight ratio of aprotic solvent is (10-18):(2-5):(70-84).
4. preparation method according to claim 1, it is characterised in that in step (2), whipping temp is 60~70 DEG C, stir
The time is mixed for 10~12h.
5. preparation method according to claim 1, it is characterised in that in step (3), coagulating bath is 0~60wt% second
Alcoholic solution；Primary membrane is immersed in 4~6min in coagulating bath；It is transferred in deionization water-bath and soaks 3~5 days.
6. preparation method according to claim 1, it is characterised in that in step (4), carburizing temperature is 600-900 DEG C, carbon
The change time is 1.5~3h.
7. preparation method according to claim 1, it is characterised in that in step (4), described hydrofluoric acid concentration is
10%.
8. the meso-porous carbon material that a kind of preparation method according to one of claim 1~7 is obtained.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973287A (en) * | 2017-12-04 | 2018-05-01 | 吉林大学 | A kind of meso-porous carbon material and preparation method thereof |
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| CN104760944A (en) * | 2015-03-16 | 2015-07-08 | 同济大学 | One-step preparation method of double-surface heterogeneous net carbon film |
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| CN105731416A (en) * | 2014-12-09 | 2016-07-06 | 中国科学院大连化学物理研究所 | Porous carbon membrane for lithium-sulfur batteries and application of porous carbon membrane |
| CN106564868A (en) * | 2016-10-09 | 2017-04-19 | 上海应用技术大学 | Preparation method of nitrogen-doped porous carbon material |
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| CN103140278A (en) * | 2010-09-30 | 2013-06-05 | 海绵股份有限公司 | Thin film composite membranes for forward osmosis, and their preparation methods |
| CN102157731A (en) * | 2011-03-18 | 2011-08-17 | 上海交通大学 | Silicon and carbon compound anode material of lithium ion battery and preparation method of silicon and carbon compound anode material |
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| CN107973287B (en) * | 2017-12-04 | 2020-08-07 | 吉林大学 | Mesoporous carbon material and preparation method thereof |
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