CN106315538A - Method for preparing porous carbon - Google Patents
Method for preparing porous carbon Download PDFInfo
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- CN106315538A CN106315538A CN201510373564.4A CN201510373564A CN106315538A CN 106315538 A CN106315538 A CN 106315538A CN 201510373564 A CN201510373564 A CN 201510373564A CN 106315538 A CN106315538 A CN 106315538A
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- porous carbon
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Abstract
The invention provides a method for preparing porous carbon. The method comprises the following steps: pyrolyzing metal alkoxides at a preset temperature so as to obtain a mixture of the porous carbon and an inorganic salt or an oxide; and washing the mixture with a solvent so as to remove the inorganic salt or the oxide from the mixture, and carrying out collecting, thereby obtaining the porous carbon. According to the method for preparing the porous carbon, provided by the invention, the process conditions are mild, and the steps are simple; and by mainly utilizing the pyrolytic carbon and the inorganic salt or the oxide which are simultaneously produced during the pyrolysis of the metal alkoxides, and the pyrolytic carbon and the inorganic salt or the oxide are uniformly mixed in a molecular scale, the inorganic salt or the oxide which is produced in situ serves as a pore former and an activator, a porous carbon material which has a uniform micro-/nano-pore structure and a high specific surface area is obtained. The porous carbon prepared by the method has the characteristic of uniform and controllable pore structure, so that the method is particularly applicable to the scale production of high-quality porous carbon.
Description
Technical field
The invention belongs to nano-carbon material preparing technical field, relate to the preparation method of a kind of porous carbon.
Background technology
Porous carbon is the functional type nano-carbon material of a quasi-representative.Porous carbon is mainly used in clean energy resource and stores (hydrogen, natural
Gas and the medium of electrical power storage (such as ultracapacitor), catalyst carrier, clean reagent in drinking water, the high-efficiency adsorbent of poison and
The aspects such as the filler in chromatographic column.Research and development porous carbon materials and application thereof cause the very big concern of Chinese scholars, mesh
Front porous carbon has become the new carbon competitively developed in Jin20Nian Lai world material with carbon element industry the most.
The method preparing porous carbon at present mainly has activation method and template etc..Wherein the main flow route of activation method is to utilize activator
Corrasion to material with carbon element forms loose structure.The kind of activator is a lot, mainly includes KOH, NaOH, K2CO3、
CO2With air etc..Wherein KOH pore-creating effect is best, and relatively KOH in terms of pore structure ability of regulation and control is poor for other activator.Cause
This is for the preparation of porous carbon, the most mostly uses KOH to activate raw material.Although KOH activating carbonaceous forerunner physical ability
Enough prepare the longest research history of porous carbon, but its industrialized production still exists technical problem, safety problem and environmental problem.
Such as KOH activation method produces in porous carbon activation process, has substantial amounts of simple substance potassium and generates.And the activation temperature of KOH activation
General at about 800 DEG C, higher than the boiling point of potassium, therefore production process has a large amount of simple substance potassium effusion activation furnace.Potassium is a kind of
The most active metal simple-substance, runs into the moisture in air and reacts generation hydrogen, and discharge substantial amounts of heat, so that producing quick-fried
Fried, bring huge potential safety hazard to the production of porous carbon.Meanwhile, simple substance potassium, during effusion, can partial condensation activate
In the pipeline of stove, block pipeline, also can bring hidden danger to safety in production.
Template is before carbon source precursor species high temperature cabonization, or is mixed into specific material in carbon source precursor species forming process
As template, form the mixture of carbon source presoma and template so that carbonization is carried out in the spatial network that template is formed,
Template agent removing is removed, it is thus achieved that there is the material with carbon element of loose structure after carbonization.There is not security hidden trouble in template, but and activation method
Comparing, template there is problems of the uniformity of pore-creating and is difficult to control to, before this depends greatly on template and carbon source
Drive the mixing uniformity of body, and this point is difficulty with in extensive preparation.
Therefore, how to provide that a kind of technique is simple, the porous carbon technology of preparing of safety and environmental protection, ensure active carbon pore structure simultaneously
Uniformity and controllability, to realize the large-scale production of porous carbon, become the important skill that those skilled in the art are urgently to be resolved hurrily
Art problem.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide the preparation method of a kind of porous carbon, is used for solving
In prior art of determining, porous carbon prepares inadequate environmental protection, the unmanageable problem of pore-creating uniformity.
For achieving the above object and other relevant purposes, the present invention provides the preparation method of a kind of porous carbon, comprises the following steps:
Pyrogenic metal alkoxide under preset temperature, it is thus achieved that porous carbon and inorganic salt or hopcalite；
Washing described mixture with solvent, to remove the inorganic salt in described mixture or oxide, and collection obtains described porous
Carbon.
Alternatively, described metal alkoxide includes Feldalat KM, Feldalat NM, Feldalat KM, Sodium ethylate, sodium glycollate, potassium ethoxide, second
One or more in magnesium alkoxide.
Alternatively, the scope of described preset temperature is 200～3100 DEG C, and pyrolysis time is 1～600min.
Alternatively, one or more during described solvent includes water, dilute hydrochloric acid, ethanol, methanol, isopropanol.
Alternatively, the method for pyrogenic metal alkoxide includes: is placed in container by metal alkoxide powder body, and passes through heating devices heat.
Alternatively, described heater includes Muffle furnace or microwave oven.
Alternatively, pyrolysis atmosphere includes air atmosphere, inert gas atmosphere or vacuum atmosphere.
Alternatively, it is collected by filtration and obtains described porous carbon.
Alternatively, further described porous carbon is dried.
Alternatively, described dry method include directly drying, be vacuum dried, lyophilization or spray drying.
As it has been described above, the preparation method of the porous carbon of the present invention, have the advantages that the preparation side of the porous carbon of the present invention
Method process conditions are gentle, step is simple, mainly utilize metal alkoxide to generate pyrolytic carbon and inorganic salt or oxygen in pyrolytic process simultaneously
Compound, the two is mix homogeneously on molecular scale, and generated in-situ inorganic salt or oxide serve as pore creating material and activator, thus
Obtain and there is uniform micro-nano hole structure and the porous carbon materials of high-specific surface area.The porous carbon prepared due to the present invention has hole knot
The feature that structure is uniform, controlled, is therefore particularly suitable for the large-scale production of high-quality porous carbon.
Accompanying drawing explanation
Fig. 1 is shown as the process chart of the preparation method of the porous carbon of the present invention.
Fig. 2 is shown as the preparation method of the porous carbon of the present invention and prepares the SEM figure of gained porous carbon in embodiment one.
Fig. 3 is shown as the preparation method of the porous carbon of the present invention and prepares the TEM figure of gained porous carbon in embodiment one.
Fig. 4 is shown as the preparation method of the porous carbon of the present invention and prepares nitrogen adsorption-desorption song of gained porous carbon in embodiment one
Line.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by disclosed by this specification
Content understand other advantages and effect of the present invention easily.The present invention can also be added by the most different detailed description of the invention
To implement or application, the every details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention
Various modification or change is carried out under god.
Refer to Fig. 1 to Fig. 4.It should be noted that the diagram provided in the present embodiment illustrates the present invention the most in a schematic way
Basic conception, the most graphic in component count time only display with relevant assembly in the present invention rather than is implemented according to reality, shape
And size drafting, during its actual enforcement, the kenel of each assembly, quantity and ratio can be a kind of random change, and its assembly layout
Kenel is likely to increasingly complex.
The present invention provides the preparation method of a kind of porous carbon, comprises the following steps:
Pyrogenic metal alkoxide under preset temperature, it is thus achieved that porous carbon and inorganic salt or hopcalite；
Washing described mixture with solvent, to remove the inorganic salt in described mixture or oxide, and collection obtains described porous
Carbon.
Concrete, described metal alkoxide includes Feldalat KM, Feldalat NM, Feldalat KM, Sodium ethylate, sodium glycollate, potassium ethoxide, second
One or more in magnesium alkoxide.During pyrogenic metal alkoxide, metal alkoxide powder body can be placed in container, and be added by heater
Heat.Described container is heat-resisting material, such as pottery, graphite, metal, carborundum etc., container described in heating process can opening,
Can also add a cover.Described heater includes but not limited to Muffle furnace or microwave oven.Wherein, Muffle furnace is a kind of general heating
Equipment, can be divided into batch-type furnace, tube furnace, crucible furnace according to face shaping.When using microwave-oven-heating, the material of described container
Preferably employing carborundum, carborundum (SiC) is the material that a kind of chemism is relatively low, has high-termal conductivity, it is possible to strongly absorb
Microwave energy, can improve microwave-oven-heating effect.
During pyrolysis, the scope of described preset temperature is 200～3100 DEG C, and pyrolysis time is 1～600min.Pyrolysis atmosphere can be
Air atmosphere, inert gas atmosphere, vacuum atmosphere or other mixed-gas atmosphere, as long as porous carbon can be generated during pyrolysis,
Should too not limit the scope of the invention.
Owing to the method for the present invention generates pyrolytic carbon and inorganic salt or oxide in pyrolytic process simultaneously, the two is on molecular scale
Mix homogeneously, generated in-situ inorganic salt or oxide serve as pore creating material and activator, remove described inorganic salt subsequently through washing
Or oxide, can obtain and there is uniform micro-nano hole structure and the porous carbon materials of high-specific surface area.
Concrete, when pyrolysis is washed after terminating, the solvent used can include that (i.e. mass fraction is less than 20% for water, dilute hydrochloric acid
Hydrochloric acid), ethanol, methanol, one or more in isopropanol.Thermal decomposition product can be directly placed in solvent and wash, wash
Wash number of times at least one times.In washing process, inorganic salt or oxide that pyrolysis produces will be dissolved in solvent, and porous carbon
For insoluble matter, can collect after washing and obtain porous carbon.
Concrete, can be collected by filtration and obtain described porous carbon, and further described porous carbon is dried, obtain porous carbon dust
Body.As it is shown in figure 1, be shown as the process chart of the preparation method of the porous carbon of the present invention.Described dry method includes directly
Connect drying, vacuum drying, lyophilization or spray drying.Wherein, directly drying refers to use under air atmosphere, normal pressure dry
Case is dried, and oven temperature is preferably no more than 150 DEG C；Vacuum drying, also known as drying under reduced pressure, is vacuumizing in airtight container,
A kind of method reduced pressure and be dried；Lyophilization is also known as sublimation drying, and material can be first freezing in refrigerating plant, then carries out
Vacuum drying, it is possible to directly through being evacuated rapidly and freezing, required in sublimation process heat of vaporization, typically in hothouse
Supply with heat radiation；Spray drying be in hothouse by solvent or diluent after atomization, with in the contacting of hot-air, the rapid vapour of moisture
Change, i.e. obtain dry products, this method can directly make solution, emulsion be dried to powdery or particulate preparation, can save devaporation,
The operations such as pulverizing.Certainly, it is possible to use other conventional drying methods, should too not limit the scope of the invention.
The preparation method process conditions of the porous carbon of the present invention are gentle, step is simple, the porous carbon pore structure prepared uniformly,
Controlled, it is particularly suitable for the large-scale production of high-quality porous carbon.
Technical scheme is described in detail below by specific embodiment.
Embodiment one
A certain amount of Feldalat KM powder body is positioned in ceramic crucible, is placed in 400 DEG C of Muffle furnaces being incubated 4h, it is thus achieved that Lycoperdon polymorphum Vitt is solid
Body product, this product includes potassium carbonate and porous carbon.Then utilize the above-mentioned solid product of ionized water cyclic washing, be collected by filtration
To black solid product.The above-mentioned solid product of lyophilization, obtains the porous carbon powder body of black.
Refer to Fig. 2 and 3, be respectively indicated as SEM figure and the TEM figure of gained porous carbon powder body in the present embodiment, it is seen then that
Described powder structure exists a large amount of nano pore.
Referring to Fig. 4, be shown as the nitrogen adsorption-desorption curve of gained porous carbon powder body in the present embodiment, its abscissa is relative
Pressure P/P0, wherein P is the true pressure of gas, P0For gas saturated vapor pressure at a temperature of measuring；Vertical coordinate is standard
Adsorb the volume of nitrogen molecule in porous carbon duct under temperature and pressure, i.e. adsorbance, wherein, cm3Stand for volume unit
Square centimetre, g is mass unit gram.
Test result shows, the BET specific surface area of gained powder structure is 2800m2/ g, wherein, BET specific surface area is BET
The abbreviation of specific surface area method of testing, BET is the acronym of three scientists (Brunauer, Emmett and Teller),
BET specific surface area test can be used for surveying the specific surface area of granule, pore volume, pore-size distribution and nitrogen adsorption desorption curve.This reality
Executing in example, the pore-size distribution of gained porous carbon powder body is 0.5～10nm, and average pore size is 3nm.
Embodiment two
A certain amount of Feldalat KM powder body is placed in 800 DEG C of Muffle furnaces insulation 5h, it is thus achieved that gray solid product, this product includes carbon
Acid potassium and porous carbon.Utilize the ion above-mentioned solid product of ethanol cyclic washing, be collected by filtration and obtain black solid product.Vacuum is done
Dry above-mentioned solid product, obtains the porous carbon powder body of black.
Embodiment three
A certain amount of Diethoxymagnesium is placed in 1500 DEG C of Muffle furnaces insulation 8h, it is thus achieved that gray solid product, this product includes magnesium oxide
And porous carbon.Utilize the above-mentioned solid product of dilute hydrochloric acid cyclic washing, be collected by filtration and obtain black solid product.Dry above-mentioned solid
Product, obtains the porous carbon powder body of black.
Embodiment four
A certain amount of potassium ethoxide is placed in 2100 DEG C of Muffle furnaces insulation 2h, it is thus achieved that gray solid product, this product includes potassium carbonate
And porous carbon.Utilize the above-mentioned solid product of ionized water cyclic washing, be collected by filtration and obtain black solid product.It is vacuum dried above-mentioned
Solid product, obtains the porous carbon powder body of black.
In sum, the preparation method process conditions of the porous carbon of the present invention are gentle, step is simple, mainly utilize metal alkoxide to exist
Generating pyrolytic carbon and inorganic salt or oxide in pyrolytic process, the two is mix homogeneously on molecular scale simultaneously, generated in-situ nothing
Machine salt or oxide serve as pore creating material and activator, thus obtain and have uniform micro-nano hole structure and the porous carbon of high-specific surface area
Material.It is uniform, controlled that the porous carbon prepared due to the present invention has pore structure, is therefore particularly suitable for high-quality porous carbon
Large-scale production.So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any it is familiar with this skill
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage of art.Therefore, such as
All that in art, tool usually intellectual is completed under without departing from disclosed spirit and technological thought etc.
Effect is modified or changes, and must be contained by the claim of the present invention.
Claims (10)
1. the preparation method of a porous carbon, it is characterised in that comprise the following steps:
Pyrogenic metal alkoxide under preset temperature, it is thus achieved that porous carbon and inorganic salt or hopcalite；
Washing described mixture with solvent, to remove the inorganic salt in described mixture or oxide, and collection obtains described many
Hole carbon.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: described metal alkoxide includes Feldalat KM, methanol
One or more in sodium, Feldalat KM, Sodium ethylate, sodium glycollate, potassium ethoxide, Diethoxymagnesium.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: the scope of described preset temperature is 200～3100
DEG C, pyrolysis time is 1～600min.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: described solvent include water, dilute hydrochloric acid, ethanol,
One or more in methanol, isopropanol.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: the method for pyrogenic metal alkoxide includes: by gold
Belong to alkoxide powder body to be placed in container, and pass through heating devices heat.
The preparation method of porous carbon the most according to claim 5, it is characterised in that: described heater includes Muffle furnace or microwave
Stove.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: pyrolysis atmosphere includes air atmosphere, indifferent gas
Bromhidrosis atmosphere or vacuum atmosphere.
The preparation method of porous carbon the most according to claim 1, it is characterised in that: it is collected by filtration and obtains described porous carbon.
The preparation method of porous carbon the most according to claim 8, it is characterised in that: further described porous carbon is dried.
The preparation method of porous carbon the most according to claim 9, it is characterised in that: described dry method includes directly drying,
Vacuum drying, lyophilization or spray drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110803700A (en) * | 2019-12-12 | 2020-02-18 | 中国科学院化学研究所 | Porous carbon material and method for preparing porous carbon material by utilizing microwave hot-zone effect |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008044816A (en) * | 2006-08-17 | 2008-02-28 | Tokai Carbon Co Ltd | Porous carbon material production method |
| CN101740231A (en) * | 2010-01-12 | 2010-06-16 | 山东理工大学 | Preparation method of mesoporous carbon electrode material for supercapacitor |
| JP2013220980A (en) * | 2012-04-18 | 2013-10-28 | Okayama Univ | Method of manufacturing oxide |
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- 2015-06-30 CN CN201510373564.4A patent/CN106315538A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008044816A (en) * | 2006-08-17 | 2008-02-28 | Tokai Carbon Co Ltd | Porous carbon material production method |
| CN101740231A (en) * | 2010-01-12 | 2010-06-16 | 山东理工大学 | Preparation method of mesoporous carbon electrode material for supercapacitor |
| JP2013220980A (en) * | 2012-04-18 | 2013-10-28 | Okayama Univ | Method of manufacturing oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110803700A (en) * | 2019-12-12 | 2020-02-18 | 中国科学院化学研究所 | Porous carbon material and method for preparing porous carbon material by utilizing microwave hot-zone effect |
| CN110803700B (en) * | 2019-12-12 | 2021-09-21 | 中国科学院化学研究所 | Porous carbon material and method for preparing porous carbon material by utilizing microwave hot-zone effect |
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