CN107746055A - A kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope - Google Patents
A kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope Download PDFInfo
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- CN107746055A CN107746055A CN201711005002.XA CN201711005002A CN107746055A CN 107746055 A CN107746055 A CN 107746055A CN 201711005002 A CN201711005002 A CN 201711005002A CN 107746055 A CN107746055 A CN 107746055A
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Abstract
The invention discloses a kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope, using with special laminar structured agaric as raw material, hydro-thermal is handled agaric first, is then freeze-dried, and keeps the lamellar structure of agaric, then low-temperature carbonization and high-temperature activation in tube furnace, afterwards using thiocarbamide as N, S sources and the mixing of porous carbon nanosheet, further activated in high temperature, it can obtain N, the multi-stage porous carbon nanometer sheet of S doping.The N of functionalization prepared by the present invention, S adulterate multi-stage porous carbon nanometer sheet material, and preparation method is simple, easy to operate, and obtained Carbon Materials have abundant multi-stage artery structure, are the good electrode materials of capacitor.
Description
Technical field
The present invention relates to a kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope, and in particular to freezing is dry
Dry, low-temperature carbonization, high-temperature activation and then N, S doping prepare multi-stage porous carbon nanometer sheet.
Background technology
Ultracapacitor is a kind of new energy storage device, possess high power density and energy density, have extended cycle life,
The advantages that environment friendly and pollution-free, gather around and have broad application prospects and commercial value in electrochemical energy storage field.Porous carbon electrodes
Can remarkable be the outstanding figure in electrode material for super capacitor.Use suitable rich carbon matrix precursor such as activated carbon, CNT, graphite
Carbon derived from alkene, carbon aerogels and carbide.In above-mentioned carbon material, activated carbon is recognized due to its high surface area and low cost
To be the first choice of business super capacitor device.Nevertheless, conventional activated carbon electric capacity and power characteristic due to its it is improper and
The pore structure of obstruction and be restricted, and then limit the permeability of electrolyte ion under charge/discharge rates.Many institute's weeks
Know, the key for obtaining excellent power-performance is to reduce the ion haulage time in electrode material.Therefore, there is two-dimentional (2D) and open
The carbon material for putting loose structure has superiority due to the less of the time of Ion transfer.Particularly graphene and graphene mixes
Condensation material has high electrical conductivity on two-dimensional material surface, has the performance of the power density and energy density better than activated carbon.
The current two-dimentional wide variety of synthetic method of carbon material mainly has a chemical vapor deposition, electronation, and arc discharge synthesis is high-strength
Degree ultrasound is peeled off and microwave radiation.Even however, cost and facility most economical, that most easily prepare grapheme material
There is no direct pyrolytic carbon precursor (such as biological waste or containing cellulose, the biomass of hemicellulose and lignin polymer)
It is more competitive to be directly translated into the PCN with graphene form.Abundant biomass carbon is super capacitor carbon electrode material
Rich carbon matrix precursor selection provide green, cheap and sufficient reserves new way.But not all life
Material can be taken as raw material to go to prepare rich carbon matrix precursor, and biomass carbon source of the selection with special construction is particularly important.And
Agaric has the design feature of fluffy multilayer, while has hole and the duct of prosperity, and pore-size distribution is from nanoscale to grade.
Its obtained porous carbon materials after being carbonized has high porosity, forms unimodal or multimodal feature pore-size distribution, effectively carries
Rise its ion permeability and electric conductivity as electrode material.Hetero atom is mixed into carbon material for adjusting its electron donor property
And the chemical property for then adjusting its surface is most important.Introducing hetero-atoms can reduce the resistance of electric charge transfer and improve profit
It is moist, so as to strengthen capacitive property.Representational hetero atom such as nitrogen (N), phosphorus (P), sulphur (S) and boron (B) can be adulterated with single or
Codope mode is mixed with modified carbonaceous components.With only carry high performance one side it is single it is atom doped compared with, due to collaboration
Effect, codope can improve the overall performance of material.Therefore, it is increasing in recent years to make great efforts to concentrate on the more hetero atoms of research
Doping.N, S are co-doped with carbon material and have been applied to oxygen reduction reaction (ORR), but there has been no patent and document report using agaric as
Carbon source prepares N, the multi-stage porous carbon nanometer sheet of S codopes.This patent agaric prepares electrode of super capacitor as rich carbon matrix precursor
The active material of material, it can be pyrolyzed by a step and activation prepares multi-stage porous charcoal nanometer sheet.
The content of the invention
To realize that technical scheme provided by the present invention is：
(1) agaric for weighing certain mass uses deionized water repeatedly, is subsequently placed in air dry oven, 100 DEG C of dryings
12h, dry agaric and the solid-to-liquid ratio 1: 25 of the aqueous solution of 0~30% alkali, mixing are put into reactor, 120 DEG C of reaction 6h,
Reaction is cooled to room temperature.The freeze-dried 24h of sample, produce the agaric of pretreatment；
(2) agaric for the pretreatment that step (1) obtains is weighed, is placed in tube furnace and is carbonized, 5 DEG C of programming rate/
Min, calcining heat are 400 DEG C, time 1h, then heat to 700~900 DEG C, activate 1h, are subsequently cooled to room temperature, solid is washed
To neutrality, 100 DEG C of dry 12h, produce multi-stage porous carbon nanometer sheet in air dry oven；
(3) the multi-stage porous carbon nanometer sheet that step (2) obtains accurately is weighed, is stirred vigorously down molten with 5~30mg/ml thiocarbamide
Liquid mixes, static 12h, obtained solution is dried in vacuo at 80 DEG C, then 850 DEG C of high temperature carbonizations in tube furnace, argon gas are protected
Shield, programming rate is 5 DEG C/mim, constant temperature 3h, is then activated under 300 DEG C of air atmospheres, produces the multi-stage porous carbon of nitrogen sulfur doping
Nanometer sheet.
To be best understood from the present invention, the present invention will be described in further detail with reference to the following examples, but of the invention
Claimed scope is not limited to the scope of embodiment expression.
Embodiment 1：
(1) agaric for weighing 1g uses deionized water repeatedly, is subsequently placed in air dry oven, 100 DEG C of dry 12h, dries
Agaric mixed with the 5% KOH aqueous solution, solid-to-liquid ratio 1: 25, be put into reactor, 120 DEG C reaction 6h, reaction be cooled to room
Temperature.The freeze-dried 24h of sample, produce the agaric of pretreatment；
(2) agaric for the pretreatment that step (1) obtains is weighed, is placed in tube furnace and is carbonized, 5 DEG C of programming rate/
Min, calcining heat are 400 DEG C, time 1h, then heat to 800 DEG C, activate 1h, room temperature are subsequently cooled to, during solid is washed till
Property, 100 DEG C of dry 12h in air dry oven, produce multi-stage porous carbon nanometer sheet；
(3) the multi-stage porous carbon nanometer sheet 0.5g that step (2) obtains accurately is weighed, is stirred vigorously down and 100ml 10mg/ml
Thiourea solution mixing, static 12h, by obtained solution in 60 DEG C of vacuum drying, then 800 DEG C of pyrocarbons in tube furnace
Change, argon gas protection, programming rate is 5 DEG C/mim, constant temperature 3h, is then activated under 300 DEG C of air atmospheres, produces nitrogen sulfur doping
Multi-stage porous carbon nanometer sheet.
Embodiment 2：The concentration for changing the KOH aqueous solution is 10%, and other steps produce nitrating sulfur doping with embodiment 1
Multi-stage porous carbon nanometer sheet.
Embodiment 3：Change the concentration 15mg/ml of thiourea solution, other steps produce nitrating sulfur doping with embodiment 1
Multi-stage porous carbon nanometer sheet.
Embodiment 4：It is 700 DEG C to change calcining heat, and other steps produce the multi-stage porous of nitrating sulfur doping with embodiment 1
Carbon nanosheet.
Claims (2)
1. a kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope, is comprised the following steps that：
(1) agaric for weighing certain mass uses deionized water repeatedly, is subsequently placed in air dry oven, 100 DEG C of dry 12h, does
Dry agaric and the solid-to-liquid ratio 1: 25 of the aqueous solution of 0~30% alkali, mixing are put into reactor, 120 DEG C of reaction 6h, and reaction is cold
But to room temperature, the freeze-dried 24h of sample, the agaric of pretreatment is produced；
(2) agaric for the pretreatment that step (1) obtains is weighed, is placed in tube furnace and is carbonized, 5 DEG C/min of programming rate, forged
It is 400 DEG C, time 1h to burn temperature, then heats to 700~900 DEG C, activates 1h, is subsequently cooled to room temperature, and solid is washed till neutrality,
100 DEG C of dry 12h, produce multi-stage porous carbon nanometer sheet in air dry oven；
(3) the multi-stage porous carbon nanometer sheet that step (2) obtains accurately is weighed, is stirred vigorously down and is mixed with 5~30mg/ml thiourea solution
Close, static 12h, obtained solution is dried in vacuo at 80 DEG C, then 850 DEG C of high temperature carbonizations in tube furnace, argon gas protection, risen
Warm speed is 5 DEG C/mim, constant temperature 3h, is then activated under 300 DEG C of air atmospheres, produces the multi-stage porous carbon nanometer of nitrogen sulfur doping
Piece.
2. a kind of new method of the preparation of the multi-stage porous carbon nanometer sheet of nitrogen sulphur codope as claimed in claim 1, its feature exist
In：Alkali source can be KOH, NaOH.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244413A (en) * | 2018-09-21 | 2019-01-18 | 合肥工业大学 | A kind of sulphur anode composite material and preparation method thereof based on multiporous biological matter carbon |
| CN109354017A (en) * | 2018-10-17 | 2019-02-19 | 西安理工大学 | It is a kind of original position sulphur, nitrogen co-doped biomass carbon nanometer sheet preparation method |
| CN109941995A (en) * | 2019-04-04 | 2019-06-28 | 济南大学 | A kind of preparation and application of the heteroatom doping biomass carbon material producing hydrogen peroxide for electro-catalysis |
| CN110504414A (en) * | 2018-05-16 | 2019-11-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Defect metal oxide/porous nano carbonaceous composite material and preparation method and application |
| CN110759343A (en) * | 2019-12-04 | 2020-02-07 | 桂林理工大学 | N, S co-doped bagasse nano-sheet mesoporous structure biomass charcoal and preparation method thereof |
| CN110759326A (en) * | 2019-10-10 | 2020-02-07 | 延边大学 | Doped porous carbon material, preparation method thereof and porous carbon-based electrode material |
| CN111115629A (en) * | 2019-12-27 | 2020-05-08 | 暨南大学 | High-specific-surface-area carbon material based on waste tobacco stems and preparation method and application thereof |
| CN111498845A (en) * | 2020-04-14 | 2020-08-07 | 浙江科技学院 | Preparation method and application of nitrogen-sulfur double-doped biochar |
| CN112062125A (en) * | 2020-09-09 | 2020-12-11 | 艾思尔信息科技(上海)有限公司 | Hierarchical pore doped carbon material and preparation method and application thereof |
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| CN106882799A (en) * | 2017-03-04 | 2017-06-23 | 桂林理工大学 | Sisal fiber base nitrogen, sulphur are co-doped with miscellany graphene carbon material and preparation method |
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| CN106882799A (en) * | 2017-03-04 | 2017-06-23 | 桂林理工大学 | Sisal fiber base nitrogen, sulphur are co-doped with miscellany graphene carbon material and preparation method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110504414A (en) * | 2018-05-16 | 2019-11-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Defect metal oxide/porous nano carbonaceous composite material and preparation method and application |
| CN110504414B (en) * | 2018-05-16 | 2022-07-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Defect metal oxide/porous nano carbon composite material and preparation method and application thereof |
| CN109244413A (en) * | 2018-09-21 | 2019-01-18 | 合肥工业大学 | A kind of sulphur anode composite material and preparation method thereof based on multiporous biological matter carbon |
| CN109354017A (en) * | 2018-10-17 | 2019-02-19 | 西安理工大学 | It is a kind of original position sulphur, nitrogen co-doped biomass carbon nanometer sheet preparation method |
| CN109941995A (en) * | 2019-04-04 | 2019-06-28 | 济南大学 | A kind of preparation and application of the heteroatom doping biomass carbon material producing hydrogen peroxide for electro-catalysis |
| CN110759326A (en) * | 2019-10-10 | 2020-02-07 | 延边大学 | Doped porous carbon material, preparation method thereof and porous carbon-based electrode material |
| CN110759326B (en) * | 2019-10-10 | 2021-06-29 | 延边大学 | Doped porous carbon material, preparation method thereof and porous carbon-based electrode material |
| CN110759343A (en) * | 2019-12-04 | 2020-02-07 | 桂林理工大学 | N, S co-doped bagasse nano-sheet mesoporous structure biomass charcoal and preparation method thereof |
| CN111115629A (en) * | 2019-12-27 | 2020-05-08 | 暨南大学 | High-specific-surface-area carbon material based on waste tobacco stems and preparation method and application thereof |
| CN111498845A (en) * | 2020-04-14 | 2020-08-07 | 浙江科技学院 | Preparation method and application of nitrogen-sulfur double-doped biochar |
| CN111498845B (en) * | 2020-04-14 | 2021-12-21 | 浙江科技学院 | Preparation method and application of nitrogen-sulfur double-doped biochar |
| CN112062125A (en) * | 2020-09-09 | 2020-12-11 | 艾思尔信息科技(上海)有限公司 | Hierarchical pore doped carbon material and preparation method and application thereof |
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Application publication date: 20180302 |