CN105129768A - Method for preparing nitrogen-doped porous carbon material based on folic acid - Google Patents
Method for preparing nitrogen-doped porous carbon material based on folic acid Download PDFInfo
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- CN105129768A CN105129768A CN201510502169.1A CN201510502169A CN105129768A CN 105129768 A CN105129768 A CN 105129768A CN 201510502169 A CN201510502169 A CN 201510502169A CN 105129768 A CN105129768 A CN 105129768A
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- carbon material
- porous carbon
- folic acid
- template
- nitrogen
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- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 title claims abstract description 40
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 27
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229960000304 folic acid Drugs 0.000 title claims abstract description 20
- 235000019152 folic acid Nutrition 0.000 title claims abstract description 20
- 239000011724 folic acid Substances 0.000 title claims abstract description 20
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004246 zinc acetate Substances 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 238000003763 carbonization Methods 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000007833 carbon precursor Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing a nitrogen-doped porous carbon material based on folic acid, which takes folic acid as a carbon source and a nitrogen source and zinc acetate as a template agent and prepares the nitrogen-doped porous carbon material through a direct template-carbonization-nitridation route. According to the invention, by regulating and controlling the mass ratio of folic acid to zinc acetate, the carbonization temperature, the carbonization time, the heating rate and other factors, the synthesis of the nitrogen-doped porous carbon material by the template-carbonization-nitridation process can be realized by a one-step method (without subsequent treatment processes such as acid washing and the like). The production process method provided by the invention has the advantages of simplicity, easiness in operation, short synthesis period and the like, and is suitable for large-scale industrial production of the electrode porous carbon material of the supercapacitor.
Description
One, technical field
The present invention relates to a kind of method preparing N doping porous carbon material based on folic acid, belong to electrode of super capacitor field of charcoal material.
Two, background technology
Ultracapacitor, as a kind of novel energy storage device, has superpower, has extended cycle life, charge/discharge rates is fast, efficiency is high, environmentally safe, use temperature wide ranges and security high, becomes the application focus of new energy field.And electrode materials is as the most important integral part of ultracapacitor, its performance of the Nomenclature Composition and Structure of Complexes on ultracapacitor plays vital impact.Carbon electrode material, as electrode for super capacitor material, is study the electrode materials that technology is the most ripe the earliest.
At present, the synthetic method of porous carbon material is diversified, but major part all needs physically activated or chemical activation, has the shortcomings such as high energy consumption, high pollution, high corrosion.Template charring is a kind of method preparing porous carbon material for supercapacitor of rising recently.The method selects the material of nanoaperture structure as template, in its hole, inject carbon precursor, and by high temperature carbonization and removal template, can obtain the porous carbon material with microcosmic and macroscopical controlled architecture.
Prepare in the technique of porous carbon material in template charing, choose suitable carbon precursor and very important impact is served for the stuctures and properties of product.Folic acid is yellow or orange-yellow crystalline powder, and its structural representation is as follows, containing elements such as more carbon, nitrogen, oxygen, hydrogen, can be prepared the porous carbon material of N doping by charing route.
Patent CN102976305A is template by synthesis mesoporous silica ball, and the resol of synthesis is as carbon precursor; Prepare resol/template composite; Prepare charcoal/template matrix material.Remove template further again, obtained Mesoporous Carbon Materials.But such silicon oxide template needs the caustic acid such as hydrofluoric acid to carry out template to remove usually, not green, environmental protection.
In the present invention, adopt zinc acetate as template, can at high temperature (>950 DEG C) directly to volatilize removal (boiling point of metallic zinc is 908 DEG C), without the need to last handling processes such as further pickling, greatly optimize the synthesis technique of N doping porous carbon material.
Three, summary of the invention
The present invention aims to provide a kind of method preparing N doping porous carbon material based on folic acid; take folic acid as Carbon and nitrogen sources; zinc acetate is template; prepare N doping porous carbon material by direct template-charing-nitrogenize route, present method be easy and simple to handle, electrochemical capacitance excellent performance, be easy to large-scale industrial produce.
The present invention is based on the method that folic acid prepares N doping porous carbon material, comprise the steps:
The ratio of 5:1 ~ 1:5 takes folic acid and zinc acetate in mass ratio, move in horizontal pipe furnace porcelain boat after grinding evenly, pass into argon gas 30min, subsequently horizontal pipe furnace is heated to 950 ~ 1400 DEG C with the temperature rise rate of 5 ~ 20 DEG C/min, and be incubated 2 ~ 10h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
The making of experimental electrode:
Take ethanol as solvent, tetrafluoroethylene (PTFE) tackiness agent of the Carbon Materials sample of 80 mass parts, the acetylene black of 15 mass parts and 5 mass parts is mixed and obtains mix slurry, under 20MPa pressure, this mix slurry is pressed onto in collector nickel foam subsequently, vacuum-drying 24 hours at 120 DEG C subsequently, obtains carbon material electrode.
Electrochemical property test:
In three-electrode system, with platinum electrode (6cm
2) for supporting electrode, saturated calomel electrode be reference electrode, carbon material electrode is working electrode, utilizes KOH solution (6mol/L) to be electrolytic solution.Electrochemical workstation is adopted to carry out the electro-chemical tests such as cyclic voltammetric, constant current charge-discharge and alternating-current impedance.
The present invention, by factors such as the mass ratio of regulation and control folic acid and zinc acetate, carbonization temperature, carbonization time and temperature rise rates, single stage method can realize template-charing-nitriding process synthetic nitrogen and to adulterate porous carbon material (without the need to treatment process such as follow-up pickling).
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention is with folic acid that is cheap, that be easy to get for Carbon and nitrogen sources, directly single stage method can realize charing and the nitrogenize of Carbon Materials, without the need to the further nitriding treatment in later stage.
2, zinc acetate can thermolysis be ZnO in carbonization process, and then is reduced to metallic zinc by Carbon Materials, and next exceed the boiling point of metallic zinc at carbonization temperature after (908 DEG C), the mode can volatilized by metal gas discharges tube furnace along with argon gas.The materials such as this quasi-metal oxides (ZnO) or metal simple-substance (Zn) all act as good template action in the forming process of porous carbon material, are conducive to the vesicular structure forming Carbon Materials.
3, the present invention adopts zinc acetate to be template, without the need to last handling processes such as further pickling, greatly optimizes the synthesis technique of N doping porous carbon material.
4, the porous carbon material that the present invention obtains has pore size distribution$ evenly and simply adjustable, the feature such as ratio capacitance is high, good cycle.Under the current density of 1A/g, discharge and recharge ratio capacitance can reach 259.6F/g.Circulate after 5000 times, discharge and recharge ratio capacitance conservation rate is up to 97.4%.
5, reaction time of the present invention is short, and easy handling is less demanding to reaction conditions, and the large-scale industrial that can realize porous carbon material for supercapacitor is produced.
Four, accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of the Carbon Materials sample that embodiment 1 obtains.As can be seen from Figure 1 Carbon Materials presents amorphous vesicular structure.
Fig. 2 is transmission electron microscope (TEM) photo of the Carbon Materials sample that embodiment 2 obtains.As can be seen from Figure 2 Carbon Materials presents amorphous vesicular structure.
Five, embodiment
Embodiment 1:
3:1 takes folic acid and zinc acetate fully grinds in mass ratio, is then moved in horizontal pipe furnace porcelain boat, passes into argon gas 30min, subsequently horizontal pipe furnace is heated to 1000 DEG C with the temperature rise rate of 5 DEG C/min, and is incubated 4h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
Embodiment 2:
1:2 takes folic acid and zinc acetate fully grinds in mass ratio, is then moved in horizontal pipe furnace porcelain boat, passes into argon gas 30min, subsequently horizontal pipe furnace is heated to 1200 DEG C with the temperature rise rate of 10 DEG C/min, and is incubated 2h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
Embodiment 3:
1:5 takes folic acid and zinc acetate fully grinds in mass ratio, is then moved in horizontal pipe furnace porcelain boat, passes into argon gas 30min, subsequently horizontal pipe furnace is heated to 950 DEG C with the temperature rise rate of 15 DEG C/min, and is incubated 10h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
Embodiment 4:
5:1 takes folic acid and zinc acetate fully grinds in mass ratio, is then moved in horizontal pipe furnace porcelain boat, passes into argon gas 30min, subsequently horizontal pipe furnace is heated to 1400 DEG C with the temperature rise rate of 20 DEG C/min, and is incubated 6h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. prepare a method for N doping porous carbon material based on folic acid, it is characterized in that comprising the steps:
Take folic acid and zinc acetate, move in horizontal pipe furnace porcelain boat after grinding evenly, pass into argon gas, subsequently horizontal pipe furnace is warming up to 950 ~ 1400 DEG C, and be incubated 2 ~ 10h in argon gas atmosphere; By after products therefrom deionized water wash in 120 DEG C of vacuum-dryings 12 hours, the porous carbon material of N doping can be obtained.
2. method according to claim 1, is characterized in that:
The mass ratio of folic acid and zinc acetate is 5:1 ~ 1:5.
3. method according to claim 1, is characterized in that:
The temperature rise rate of horizontal pipe furnace is 5 ~ 20 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845457A (en) * | 2016-05-26 | 2016-08-10 | 江苏大学 | Preparation method and application of porous carbon material |
| CN106744786A (en) * | 2016-11-10 | 2017-05-31 | 上海应用技术大学 | A kind of preparation method of metal N doping porous carbon microsphere |
| CN107146894A (en) * | 2017-05-23 | 2017-09-08 | 南京师范大学 | A kind of ultra-thin porous Co/Fe N C nano composites and its preparation method and application |
| JP2020189760A (en) * | 2019-05-20 | 2020-11-26 | 学校法人 関西大学 | Method for producing porous carbon material |
| JP2023079774A (en) * | 2021-11-29 | 2023-06-08 | 星和電機株式会社 | Porous carbon material and method for producing the same, precursor of porous carbon material, and electrode material using porous carbon material |
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| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
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| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
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| RUIZHONG ZHANG ET AL.: "Nitrogen-doped carbon quantum dots : Facile synthesis and application as a "turn off" fluorescent probe for detection of Hg2+ ions", 《BIOSENSORS AND BIOELECTRONICS》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845457A (en) * | 2016-05-26 | 2016-08-10 | 江苏大学 | Preparation method and application of porous carbon material |
| CN106744786A (en) * | 2016-11-10 | 2017-05-31 | 上海应用技术大学 | A kind of preparation method of metal N doping porous carbon microsphere |
| CN106744786B (en) * | 2016-11-10 | 2018-08-10 | 上海应用技术大学 | A kind of preparation method of metal-N doping porous carbon microsphere |
| CN107146894A (en) * | 2017-05-23 | 2017-09-08 | 南京师范大学 | A kind of ultra-thin porous Co/Fe N C nano composites and its preparation method and application |
| JP2020189760A (en) * | 2019-05-20 | 2020-11-26 | 学校法人 関西大学 | Method for producing porous carbon material |
| JP2023079774A (en) * | 2021-11-29 | 2023-06-08 | 星和電機株式会社 | Porous carbon material and method for producing the same, precursor of porous carbon material, and electrode material using porous carbon material |
| JP7293320B2 (en) | 2021-11-29 | 2023-06-19 | 星和電機株式会社 | Porous carbon material, method for producing the same, precursor of porous carbon material, and electrode material using porous carbon material |
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Application publication date: 20151209 |