CN105845457A - Preparation method and application of porous carbon material - Google Patents
Preparation method and application of porous carbon material Download PDFInfo
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- CN105845457A CN105845457A CN201610357629.0A CN201610357629A CN105845457A CN 105845457 A CN105845457 A CN 105845457A CN 201610357629 A CN201610357629 A CN 201610357629A CN 105845457 A CN105845457 A CN 105845457A
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- porous carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a preparation method and application of a porous carbon material. The preparation method is carried out according to the following steps of placing potassium acetate in a nickel crucible, placing the nickel crucible in a high-temperature quartz tubular furnace, carrying out high-temperature pyrolysis under the protection of an inert gas, obtaining a product after pyrolysis, removing impurities in the product with an acid solution, immersing the product in the acid solution for magnetic stirring, washing the product with a large amount of deionized water to a neutral condition, and carrying out vacuum drying to obtain the porous carbon material. The prepared material is favorable in porous structure, high in specific area, large in pore volume and favorable in electrochemical performance, and also can be applied to other aspects.
Description
Technical field
The invention belongs to electrode material for super capacitor preparation field, be specifically related to the preparation method of a kind of porous carbon materials.
Background technology
Now, fast-developing global economy has caused serious environmental problem, and causes consuming excessively of fossil fuel, this
Survival and development to the mankind constitute incomparable threat.Therefore, develop sustainable clean energy resource and the conversion of effective energy and
Storing technology is the huge challenge faced this century.Ultracapacitor (also known as electrochemical capacitor) is as a kind of uniqueness
Electrical energy storage, it is to connect the important bridge between traditional sucrose capacitor and battery, the most in recent years by world wide
Interior increasing attention, ultracapacitor is provided that the energy density higher than the several order of magnitude of traditional sucrose capacitor, has simultaneously
There is the power density bigger than battery and preferably recycle ability.The example of envisioned large-scale application ultracapacitor
Son is that deposit solar energy, wind energy and other renewable sources of energy are in the braking of electric vehicle.
The electric capacity of ultracapacitor is mainly derived from the surface reaction of electrode material, is included in the surface electricity of electrode and electrolyte interface
Lotus separates (i.e. electric double layer capacitance characteristic) and surface faraday's redox reaction (i.e. fake capacitance characteristic).Electrode material generally quilt
Think in ultracapacitor, serve most important effect.In numerous electrode materials, material with carbon element most widely used general, city
The ultracapacitor sold exceedes and is produced from.Due to its abundance, wide variety, specific surface area is big and electric conductivity is high, carbon
Based super capacitor has higher power density, good cyclic reversibility has extremely low cost simultaneously.
Typically, the electrode carbon material of ultracapacitor needs to exist hierarchical porous structure material with carbon element, and micropore strengthens the storage of electric charge
Ability, mesoporous existence can accelerate the diffusion of electrode intermediate ion to strengthen electric conductivity, and macropore can be as ion Buffer Pool.
Material with carbon element prepared by Conventional activation methods is difficult to the feature with hierarchical porous structure.Therefore, current existing shortcoming is overcome to develop
A kind of relatively simple method preparation have excellent conductive capability, suitable porosity material with carbon element for electrode material for super capacitor
Have important practical significance.
Summary of the invention
The present invention relates to a kind of utilize organic molecule salt as precursor by silica-based template regulation and control prepare orderly hierarchical porous structure
The preparation of carbon-based electrode material and modulation process.With potassium acetate (CH3COOK) it is raw material, is prepared by a step pyrolysis and have
The orderly pore structure material with carbon element that specific surface area is high, pore volume is big, possesses excellent chemical property.
The technical solution used in the present invention is:
The preparation method of a kind of porous carbon materials, is carried out as steps described below:
Potassium acetate is put in nickel crucible, is placed in high quartz tube furnace, under inert gas is protected, carry out high temperature pyrolysis, warp
Obtain product after crossing pyrolysis, wash away the impurity in product with acid solution, then product is immersed in magnetic agitation in acid solution, then
By a large amount of deionized waters by product washing to neutral, vacuum drying i.e. obtains porous carbon materials.
Described inert gas is N2, the one of Ar；Flow velocity is 20～100mL/min.
Described high temperature pyrolysis mode is: heating rate is 3～8 DEG C/min, is warming up to 700～900 DEG C, and at 700～900 DEG C
Keep 0.5～3h.
Described acid solution is hydrochloric acid or nitric acid, and volume fraction is 5～10%, and described stir speed (S.S.) is 200～1000r/min, stirs
The time of mixing is 2～6h.
Described vacuum drying temperature is 60～110 DEG C, and the time is 6～24h.
Described porous carbon materials is used for electrode material for super capacitor.
The invention has the beneficial effects as follows:
(1) by potassium acetate as precursor, abundant raw material source, cheap.
(2) the special construction self-activation containing carboxyl by potassium acetate self prepares multi-stage porous carbon, eliminates extra activation step,
Have great importance.
(2) material prepares preparation method simply, strong operability, it is possible to use the characteristic such as pyrolysis temperature, heating rate is special to material
Property regulates and controls.
(3) the material permeability well-formed prepared, specific surface area is high, pore volume is big, and chemical property is good, and at other
Aspect also can be applied.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the material with carbon element that embodiment 1 prepares；
Fig. 2 is that the prepared material with carbon element of embodiment 1 is according to N2The graph of pore diameter distribution that adsorption-desorption isothermal obtains；
Fig. 3 is the cyclic voltammetry curve of the material with carbon element that embodiment 1 prepares.
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention will be further described:
Embodiment 1
Weigh 10g potassium salt and be put in nickel crucible, be placed in high quartz tube furnace at Ar air-flow that (gas flow rate is 40
ML/min) under protection, it is warming up to 800 DEG C with the heating rate of 5 DEG C/min, maintains cooling naturally after 1.5h, through pyrolysis
After obtain the complex carbon material of black, be subsequently adding excess 10%HNO3(v/v) solution, makes complex carbon material submergence, sets
Rotating speed is 500r/min magnetic agitation 3h, then with the washing of a large amount of deionized waters to neutral, and 80 DEG C of vacuum drying 18h, to obtain final product
To porous carbon materials.
The method of testing using it for electrode material for super capacitor is:
First by porous carbon materials through the levigate powder being less than 30 μm to particle diameter of agate mortar, in mass ratio 85: 10: 5 weigh
State porous carbon, acetylene black and Kynoar (Poly (vinylidene fluoride), PVDF), add appropriate N-crassitude
Ketone (N-Methyl pyrrolidone, NMP) is sufficiently mixed and sizes mixing, and is uniformly coated on the foam of a size of 1.2 × 2.0cm
On nickel, treat that it is dried, hand oil-pressure machine covers with 10MPa pressure and makes electrode, and vacuum drying is stand-by further.
Electrode test uses three-electrode system, is wherein Pt sheet to electrode, and reference electrode is saturated calomel electrode (Hg/HgO), uses
The 6M KOH aqueous solution is electrolyte.
By scan image (Fig. 1) it can be seen that this material is uneven bulk, rough surface, it is scattered with crackle.According to
Nitrogen adsorption-desorption isotherm, the BET specific surface area of this material is 2144m2/ g, pore volume is 1.31cm3/ g, wherein,
It is 1465m according to the micropore specific area that t-plot method calculates2/ g, micropore volume is 0.85cm3/ g, has obvious mesoporous knot
Structure (Fig. 2), average pore diameter is 2.88nm.Using it for electro-chemical test, Fig. 3 is when sweep speed is 10mV/s
Cyclic voltammetry curve, it can be seen that material has preferable electrochemistry cycle performance.Further, this material is at 1A/g electricity
It is 125.1F/g than electric capacity under current density.
Embodiment 2
Weigh 10g potassium salt and be put in nickel crucible, be placed in high quartz tube furnace at N2(gas flow rate is 20 to air-flow
ML/min) under protection, it is warming up to 700 DEG C with the heating rate of 3 DEG C/min, maintains cooling naturally after 3h, after pyrolysis
Obtain the complex carbon material of black, be subsequently adding excess 5%HCl (v/v) solution, make complex carbon material submergence, setting speed
For 1000r/min magnetic agitation 2h, then with the washing of a large amount of deionized waters to neutral, 60 DEG C of vacuum drying 24h, i.e. obtain
Porous carbon materials.
Use it for electro-chemical test, be 96.4F/g than electric capacity under 1A/g current density.
Embodiment 3
Weigh 10g potassium salt and be put in nickel crucible, be placed in high quartz tube furnace at N2(gas flow rate is 100 to air-flow
ML/min) under protection, it is warming up to 900 DEG C with the heating rate of 8 DEG C/min, maintains cooling naturally after 0.5h, through pyrolysis
After obtain the complex carbon material of black, be subsequently adding excess 7%HCl (v/v) solution, make complex carbon material submergence, set and turn
Speed is 200r/min magnetic agitation 6h, then with the washing of a large amount of deionized waters to neutral, and 110 DEG C of vacuum drying 6h, i.e. obtain
Porous carbon materials.
Use it for electro-chemical test, be 102.9F/g than electric capacity under 1A/g current density.
Claims (6)
1. the preparation method of a porous carbon materials, it is characterised in that carry out as steps described below:
Potassium acetate is put in nickel crucible, is placed in high quartz tube furnace, under inert gas is protected, carry out high temperature pyrolysis, warp
Obtain product after crossing pyrolysis, wash away the impurity in product with acid solution, then product is immersed in magnetic agitation in acid solution, then
By a large amount of deionized waters by product washing to neutral, vacuum drying i.e. obtains porous carbon materials.
The preparation method of a kind of porous carbon materials the most according to claim 1, it is characterised in that described inert gas is
N2, the one of Ar；Flow velocity is 20～100mL/min.
The preparation method of a kind of porous carbon materials the most according to claim 1, it is characterised in that described high temperature pyrolysis side
Formula is: heating rate is 3～8 DEG C/min, is warming up to 700～900 DEG C, and keeps 0.5～3h at 700～900 DEG C.
The preparation method of a kind of porous carbon materials the most according to claim 1, it is characterised in that described acid solution is salt
Acid or nitric acid, volume fraction is 5～10%, and described stir speed (S.S.) is 200～1000r/min, and mixing time is 2～6h.
The preparation method of a kind of porous carbon materials the most according to claim 1, it is characterised in that described vacuum drying temperature
Degree is 60～110 DEG C, and the time is 6～24h.
6. the purposes of porous carbon materials prepared by the method described in Claims 1 to 5 any one, it is characterised in that described porous
Material with carbon element is used for electrode material for super capacitor.
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| CN201610357629.0A CN105845457A (en) | 2016-05-26 | 2016-05-26 | Preparation method and application of porous carbon material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107068423A (en) * | 2017-04-24 | 2017-08-18 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
Citations (4)
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|---|---|---|---|---|
| CN1907847A (en) * | 2006-08-17 | 2007-02-07 | 暨南大学 | Novel charcoal material and method of synthesizing the same |
| CN101740231A (en) * | 2010-01-12 | 2010-06-16 | 山东理工大学 | Preparation method of mesoporous carbon electrode material for supercapacitor |
| CN104916447A (en) * | 2014-03-12 | 2015-09-16 | 中国科学院大连化学物理研究所 | High-rate porous carbon electrode material for super capacitor and preparation method |
| CN105129768A (en) * | 2015-08-14 | 2015-12-09 | 安徽大学 | Method for preparing nitrogen-doped porous carbon material on the basis of folic acid |
-
2016
- 2016-05-26 CN CN201610357629.0A patent/CN105845457A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907847A (en) * | 2006-08-17 | 2007-02-07 | 暨南大学 | Novel charcoal material and method of synthesizing the same |
| CN101740231A (en) * | 2010-01-12 | 2010-06-16 | 山东理工大学 | Preparation method of mesoporous carbon electrode material for supercapacitor |
| CN104916447A (en) * | 2014-03-12 | 2015-09-16 | 中国科学院大连化学物理研究所 | High-rate porous carbon electrode material for super capacitor and preparation method |
| CN105129768A (en) * | 2015-08-14 | 2015-12-09 | 安徽大学 | Method for preparing nitrogen-doped porous carbon material on the basis of folic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107068423A (en) * | 2017-04-24 | 2017-08-18 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
| CN107068423B (en) * | 2017-04-24 | 2019-01-08 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
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Application publication date: 20160810 |