CN107572522A - A kind of preparation of N doping multi-stage porous charcoal and its capacitive property research - Google Patents
A kind of preparation of N doping multi-stage porous charcoal and its capacitive property research Download PDFInfo
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- CN107572522A CN107572522A CN201711004820.8A CN201711004820A CN107572522A CN 107572522 A CN107572522 A CN 107572522A CN 201711004820 A CN201711004820 A CN 201711004820A CN 107572522 A CN107572522 A CN 107572522A
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Abstract
The invention discloses a kind of preparation of N doping multi-stage porous charcoal and its capacitive property to study, using biomass rice husk as raw material, mixed alkali is as composite activating agent, through low-temperature carbonization, high-temperature activation produces N doping multi-stage porous charcoal, the present invention is activated to obtain the N doping multi-stage porous Carbon Materials of functionalization using mixed alkali as composite activating agent to biomass, preparation method is simple, it is easy to operate, biomass existing for nature can directly be utilized, obtained Carbon Materials have abundant multi-stage artery structure, it is the good electrode material of capacitor, greatly improve the value of biomass.
Description
Technical field
The present invention relates to a kind of preparation of N doping multi-stage porous charcoal and its capacitive property to study, and in particular to uses compound work
Agent prepares the multi-stage porous charcoal of the nitrogen containing different quality.
Background technology
For the problem such as the low present situation of China's Biomass Energy Utilization rate and huge super capacitor cost be higher, it is proposed that
Nitrating porous carbon materials, and the idea and method using it as electrode material for super capacitor are prepared using biomass rice husk.This
We utilize cheap biomass rice hull material to paper, and by simple technique, easily flow, is prepared for excellent performance
Electrode material for super capacitor.This development policies just with China at this stage runs in the opposite direction, and finds a kind of effective and reasonable rice
Shell Application way, and its existing use value can be played turn into the main direction of studying of the material at this stage.According to most
Statistics in recent years, production porous carbon materials it is more using on crops remaining " useless " crop abandoned produced as raw material,
This porous carbon materials have higher specific surface area and the distribution of pores of densification, due to these performances that it has, so
Used as a kind of stronger more satisfactory sorbing material of availability, can be used for purifying air and water purification.Porous class
The absorption property that active carbon material has as super capacitor material because of it, and excellent electric conductivity, this kind of super capacitor
Device turns into current one big epoch trend.And precursor uses rice hull material, rice hull material is carbonized (in inert gas
Under), the rice husk after carbonization activated with chemical activation method again to obtain the rice husk carbon with high specific surface area afterwards, this
Kind active carbon material is using inexpensive rice husk as raw material, can be obtained with larger after by the processing of a series of measures such as activation
Specific capacitance, controllable pore-size distribution, the porous active carbon material of high-specific surface area, can be with for preparing electrode of super capacitor
Obtain larger specific capacitance.Existing mutual attraction is referred to as Electrostatic Absorption between two electrodes, and this kind of absorption is produced to electric charge
Raw energy is influenceed by many-side, the gathering of electrolyte ion, distally diffusive migration displacement be by the pore size of carbon,
Permeable equal aperture structure control, so as to influence energy specific capacitance, density and power out-put characteristic.And content has two layers of utilization
The mechanism of the capacitor of electro-chemical test is：By energy production caused by interelectrode Electrostatic Absorption electric charge.Because carbon materials
The pore size distribution of material is uneven, so even if the specific surface area of porous carbon material than broad, but gives electrolyte ion
Shuttle diffusion still bring many inconvenience, also hence in so that the utilization rate of specific surface area greatly reduces, only close
The activation process of reason regulation porous carbon materials so that the pore-size distribution of porous carbon materials is excellent, is advantageous to the expansion of electrolyte ion
Dissipate, so as to improve electrochemical discharge speed.Patent CN106179440A N doping multi-stage porous charcoals and its preparation method and application, this
A kind of preparation method of N doping multi-stage porous charcoal of disclosure of the invention, using biomass as raw material, after being mixed with composite activating agent, heating
Calcining, calcined product mixes with deionized water, staticly settles, and is filtrated to get sediment, then post-treated to obtain N doping multistage
Hole charcoal；Described composite activating agent is sodium acid carbonate/nitrogen-containing compound, and the mass ratio of sodium acid carbonate and nitrogen-containing compound is 0.25
~4: 1；Nitrogen-containing compound includes at least one of ammonium oxalate, ammonium hydrogen carbonate, ammonium carbonate, ammonium chloride, ammonium nitrate；Biomass with
The mass ratio of composite activating agent is 1: 2~16.The present invention is activated to obtain functionalization using composite activating agent to biomass
N doping multi-stage porous Carbon Materials, preparation method is simple to operation, can directly utilize biomass existing for nature, obtained raw material of wood-charcoal
Material can prepare high performance nanocatalyst as catalyst carrier, greatly be lifted with abundant multi-stage artery structure
The value of biomass.A kind of preparation methods of N doping multi-stage porous carbon material of patent CN103537262A, the present invention are public
A kind of preparation method of N doping multi-stage porous carbon material is opened, this method is using discarded object banana skin as nitrogen source and carbon source, by perfume (or spice)
Any of several broadleaf plants skin is soaked in certain density aluminum nitrate aqueous solution, by the modified metalloid for forming multi-pore channel of the aluminum ions coordination of metal
Organic backbone complex material, then it is used to build big mesopore mesoscopic structure as template, while uses parental type three
Block copolymer F127 is used for micro-structural as soft template and regulated and controled with being oriented to, and is prepared into a series of high-specific surface areas, big pore capacities
And the N doping multi-stage porous carbon material of average mesopore size adjustable.Raw materials used cheap and easy to get, green, preparation side of the invention
Method is simple, mild condition, and gained multi-stage porous carbon quality of materials is stable, available for high-selectivity adsorption CO2Gas, can also Gao Xuan
Selecting property, big adsorption capacity, good biocompatibility ground adsorbing bilirubin, it is expected to turn into very promising blood in terms of clinical medicine
Purification separation dielectric material.A kind of preparation sides of hierarchical porous structure nitrogen-doped carbon oxygen reduction catalyst of patent CN105186010A
Method, the present invention provide a kind of preparation method of hierarchical porous structure nitrogen-doped carbon oxygen reduction catalyst, belong to fuel cell technology neck
Domain.The present invention prepares the Eutectic molten salt with 3 D stereo macroporous structure using freeze-drying method first, then with eutectic
Salt is template, adulterates nitrogenous precursor, ammonium persulfate is oxidant, and molysite is co-catalyst, using solid phase polymerization method low common
Nitrogenous precursor oxidation polymerization is triggered on fused salt surface, finally carries out high temperature pyrolysis and removes Eutectic molten salt.Prepared using the present invention
Hierarchical porous structure nitrogen-doped carbon oxygen reduction catalyst can effectively avoid polymer with nitrogen presoma during high temperature cabonization
Pyrolysis loss, structure collapses and sintering, improve catalyst production and N doping efficiency, and a large amount of micropores, Jie can be produced
Hole and macropore, improve the mass-transfer efficiency of oxygen and water.The inventive method is simple and easy, low production cost, the catalyst of preparation
Activity is urged with excellent hydrogen reduction, existing commercialization Pt/C catalyst can be substituted.
In above patent, most of patent utilization biomass prepares porous charcoal as carbon source high-temperature activation, has no and utilizes life
Material prepares the patent of the multi-stage porous charcoal rich in nitrogen as the activation of carbon source composite activating agent.
The content of the invention
To realize that technical scheme provided by the present invention is：
(1) rice husk is cleaned, and is placed in air dry oven, 100 DEG C of dry 12h, the mass ratio 1 of dry rice husk and urea:
2-1: 5, the mass ratio of rice husk and mixed alkali is 1: 1-1: 5, and the mass ratio for mixing alkali is 2: 1-1: 4, and water is used as solvent, and three is by necessarily
Ratio is well mixed, soak at room temperature 24h；It is put into air dry oven, in 100 DEG C of dry 12h, produces the rice husk of pretreatment；
(2) rice husk for the pretreatment that step (1) obtains is weighed, is placed in Muffle furnace and is calcined, 5 DEG C of programming rate/
Min, calcining heat are 700-900 DEG C, time 1h, are cooled to room temperature, and solid is washed till neutrality, are done for 100 DEG C in air dry oven
Dry 12h produces the multi-stage porous charcoal of N doping.
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) rice husk is cleaned, and is placed in air dry oven, 100 DEG C of dry 12h, the mass ratio 1 of dry rice husk and urea:
3, the mass ratio of rice husk and mixed alkali is 1: 4, and it is KHCO to mix alkali3And K2CO3Mass ratio is 1: 1, and water presses quality as solvent, three
It is well mixed than 1: 4: 3 ratio, soak at room temperature 24h；It is put into air dry oven, in 100 DEG C of dry 12h, produces pretreatment
Rice husk；
(2) rice husk for the pretreatment that step (1) obtains is weighed, is placed in Muffle furnace and is calcined, 5 DEG C of programming rate/
Min, calcining heat are 800 DEG C, time 1h, are cooled to room temperature, solid is washed till neutrality, 100 DEG C of dry 12h in air dry oven
The multi-stage porous charcoal of N doping is produced, is tested under three-electrode system, when current density is 0.5A/g, specific capacitance 150A/
g。
Embodiment 2：The mass ratio for changing rice husk and urea is 1: 2, and other steps produce the multistage of nitrating with embodiment 1
Hole charcoal, tested under three-electrode system, when current density is 0.5A/g, specific capacitance 150A/g.
Embodiment 3：Change KHCO3And K2CO3Mass ratio is 1: 2, and other steps produce the multi-stage porous of nitrating with embodiment 1
Charcoal, tested under three-electrode system, when current density is 0.5A/g, specific capacitance 125A/g.
Embodiment 4：It is 700 DEG C to change calcining heat, and other steps produce the multi-stage porous charcoal of nitrating, three with embodiment 1
Tested under electrode system, when current density is 0.5A/g, specific capacitance 118A/g.
Claims (3)
1. a kind of preparation of N doping multi-stage porous charcoal and its capacitive property research, are comprised the following steps that：
(1) rice husk is cleaned, and is placed in air dry oven, 100 DEG C of dry 12h, the mass ratio 1: 2~1 of dry rice husk and urea:
5, the mass ratio of rice husk and mixed alkali is 1: 1~1: 5, and the mass ratio for mixing alkali is 2: 1~1: 4, and water is used as solvent, and three is by necessarily comparing
Example is well mixed, soak at room temperature 24h, is put into air dry oven, in 100 DEG C of dry 12h, produces the rice husk of pretreatment；
(2) rice husk for the pretreatment that step (1) obtains is weighed, is placed in Muffle furnace and is calcined, 5 DEG C/min of programming rate, forged
It is 700~900 DEG C to burn temperature, time 1h, is cooled to room temperature, solid is washed till neutrality, 100 DEG C of dry 12h in air dry oven
Produce the multi-stage porous charcoal of N doping.
2. a kind of a kind of preparation of N doping multi-stage porous charcoal as claimed in claim 1 and its capacitive property research, its feature exist
In：Mixed alkali can be KOH and KHCO3, KOH and K2CO3、KHCO3And K2CO3。
3. a kind of a kind of preparation of N doping multi-stage porous charcoal as claimed in claim 1 and its capacitive property research, its feature exist
In：Nitrogen source can be urea, ammonium phosphate, melamine.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678151A (en) * | 2019-01-24 | 2019-04-26 | 中国矿业大学 | A kind of preparation method and application of anthracite-base nitrogen-doped porous carbon material |
| CN109694071A (en) * | 2019-01-24 | 2019-04-30 | 中国矿业大学 | A kind of method and application preparing nitrogen-doped porous carbon material using coconut husk as raw material |
| CN110526243A (en) * | 2019-07-29 | 2019-12-03 | 桂林理工大学 | A kind of preparation method and applications of the biomass porous carbon of supercapacitor |
| CN110627065A (en) * | 2019-10-16 | 2019-12-31 | 中原工学院 | Preparation method and application of jute-based nitrogen-containing porous carbon |
| CN110734063A (en) * | 2019-12-03 | 2020-01-31 | 武汉理工大学 | method for preparing rice hull based nitrogen-doped active carbon |
| CN110835108A (en) * | 2020-01-03 | 2020-02-25 | 南昌师范学院 | Method for preparing multifunctional carbon material by synchronous template activation method under microscale |
| CN111682205A (en) * | 2020-05-30 | 2020-09-18 | 中国海洋大学 | Method for preparing bubble-cushion-like porous carbon material with assistance of double-salt crystal template and potassium storage application of bubble-cushion-like porous carbon material |
| CN111892051A (en) * | 2020-08-27 | 2020-11-06 | 南昌航空大学 | Biomass hierarchical porous carbon for capacitor electrode material and preparation method thereof |
| WO2022052539A1 (en) * | 2020-09-10 | 2022-03-17 | 中国矿业大学 | Crop straw-based nitrogen-doped porous carbon material preparation method and application thereof |
| CN116440868A (en) * | 2023-04-18 | 2023-07-18 | 内蒙古大学 | Preparation method of in-situ nitrogen-doped caragana microphylla porous biochar material |
| CN117923489A (en) * | 2024-01-22 | 2024-04-26 | 东北师范大学 | Nitrogen-doped hierarchical porous carbon material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517197A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing nitrogen-doped porous carbon material for supercapacitor |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
-
2017
- 2017-10-19 CN CN201711004820.8A patent/CN107572522A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517197A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing nitrogen-doped porous carbon material for supercapacitor |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694071B (en) * | 2019-01-24 | 2020-08-18 | 中国矿业大学 | Method for preparing nitrogen-doped porous carbon material by taking coconut shell as raw material and application |
| CN109694071A (en) * | 2019-01-24 | 2019-04-30 | 中国矿业大学 | A kind of method and application preparing nitrogen-doped porous carbon material using coconut husk as raw material |
| CN109678151A (en) * | 2019-01-24 | 2019-04-26 | 中国矿业大学 | A kind of preparation method and application of anthracite-base nitrogen-doped porous carbon material |
| CN110526243A (en) * | 2019-07-29 | 2019-12-03 | 桂林理工大学 | A kind of preparation method and applications of the biomass porous carbon of supercapacitor |
| CN110627065A (en) * | 2019-10-16 | 2019-12-31 | 中原工学院 | Preparation method and application of jute-based nitrogen-containing porous carbon |
| CN110734063A (en) * | 2019-12-03 | 2020-01-31 | 武汉理工大学 | method for preparing rice hull based nitrogen-doped active carbon |
| CN110835108A (en) * | 2020-01-03 | 2020-02-25 | 南昌师范学院 | Method for preparing multifunctional carbon material by synchronous template activation method under microscale |
| CN111682205A (en) * | 2020-05-30 | 2020-09-18 | 中国海洋大学 | Method for preparing bubble-cushion-like porous carbon material with assistance of double-salt crystal template and potassium storage application of bubble-cushion-like porous carbon material |
| CN111892051A (en) * | 2020-08-27 | 2020-11-06 | 南昌航空大学 | Biomass hierarchical porous carbon for capacitor electrode material and preparation method thereof |
| WO2022052539A1 (en) * | 2020-09-10 | 2022-03-17 | 中国矿业大学 | Crop straw-based nitrogen-doped porous carbon material preparation method and application thereof |
| GB2603717A (en) * | 2020-09-10 | 2022-08-10 | Univ China Mining | Crop straw-based nitrogen-doped porous carbon material preparation method and application thereof |
| GB2603717B (en) * | 2020-09-10 | 2023-03-22 | Univ China Mining | Crop straw-based nitrogen-doped porous carbon material preparation method and application thereof |
| CN116440868A (en) * | 2023-04-18 | 2023-07-18 | 内蒙古大学 | Preparation method of in-situ nitrogen-doped caragana microphylla porous biochar material |
| CN117923489A (en) * | 2024-01-22 | 2024-04-26 | 东北师范大学 | Nitrogen-doped hierarchical porous carbon material and preparation method and application thereof |
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Application publication date: 20180112 |