CN107055531A - A kind of preparation method of biomass-based nitrogen-doped porous carbon material - Google Patents
A kind of preparation method of biomass-based nitrogen-doped porous carbon material Download PDFInfo
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- CN107055531A CN107055531A CN201710378312.XA CN201710378312A CN107055531A CN 107055531 A CN107055531 A CN 107055531A CN 201710378312 A CN201710378312 A CN 201710378312A CN 107055531 A CN107055531 A CN 107055531A
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention discloses a kind of preparation method of biomass-based nitrogen-doped porous carbon material.The preparation method is comprised the following steps that：First, biomass material is mixed in proportion with polymer with nitrogen；Then, high temperature cabonization is carried out in a nitrogen atmosphere；Finally, carbonized product and activator are mixed, carries out high-temperature activation, obtain nitrogen-doped porous carbon material.Compared to the prior art, the beneficial effects of the present invention are：Preparation method of the present invention is simple, environment-friendly, be easy to large-scale production；Nitrogen-doped porous carbon material has high nitrogen content, high specific surface area and homogeneous pore-size distribution, is had a good application prospect in carbon dioxide adsorption and electrochemical field.
Description
Technical field
The invention belongs to carbon material technical field, it is related to a kind of preparation method of N doping porous carbon, specifically one
Plant the preparation method of biomass-based nitrogen-doped porous carbon material.
Background technology
Porous carbon materials have controllable pore structure and surface chemical property, be widely used in catalysis, adsorbing separation,
The fields such as sensing, electrochemistry, the performance of porous carbon materials can be further improved by methods such as modification, doping, and improving it should
With value.Wherein nitrogen is the element at infinity of carbon material doping, can effectively improve physics, the chemistry of carbon material by N doping
Etc. property.
Being presently used for the method for nitrogenous porous carbon materials synthesis has a lot, can substantially be summarized as two classes：Original position doping and
Two kinds of post processing.The porous carbon materials for obtaining high nitrogen-containing generally need to be with nitriding in situ, in hard template method or soft template method
Prepare and introduce nitrogenous precursor during porous carbon.The most frequently used nitrogenous precursor includes amido carbohydrate, melamine, benzene methanamine
Deng.Although the porous carbon of high nitrogen-containing can be obtained by the method for nitrating in situ, there is also it is many problem of, such as：
Preparation process needs to use many organic chemical reagents, and price is relatively expensive；Removing template procedure needs to use hydrofluoric acid etc. by force
Corrosive agent, process very complicated and environment is unfriendly, therefore this method is not suitable for commercial Application.Therefore, how it is simple and
The porous carbon materials for effectively preparing high nitrogen-containing are the problem of still needing to make great efforts to solve at present.
The problem of for current environmental pollution, energy scarcity, reasonably develop renewable resources, synthesize the energy of some energy property
Source has great importance with environment-friendly materials.The main component of natural biomass materials is natural organic high-molecular, is carbonaceous material
The important presoma of material.Research on carbon material is a lot, but the carbon material that controlledly synthesis has specific structure and property still has
There is certain challenge.Because the presoma and synthetic method of carbon material are to influence two key factors of carbon material property, therefore,
The synthesis of carbonaceous material, property under comparative study difference system, the exploitation and application study to carbonaceous material are significant.
The content of the invention
It is simple it is an object of the invention to provide a kind of preparation method in order to overcome the deficiencies in the prior art, it is easy to extensive
Production, the preparation method of high content nitrogen doped porous carbon material.
In order to solve the above-mentioned technical problem, the present invention uses following technical scheme.
A kind of preparation method of biomass-based nitrogen-doped porous carbon material, is comprised the following steps that：First, by the life after crushing
Raw material of substance is mixed in proportion with polymer with nitrogen；Then, after sample after mixing is carbonized under an inert atmosphere；Finally,
Carbonized product is activated with activator, biomass-based nitrogen-doped porous carbon material is obtained；Wherein：Biomass material is water chestnut
Shepherd's purse.
In the present invention, polymer with nitrogen is melamine.
In the present invention, the mass ratio of biomass material and polymer with nitrogen is 1:1~3~2, carburizing temperature is 495~505
℃。
In the present invention, activator is KOH, and the mass ratio of carbonized product and activator is 1：1-1：4.
In the present invention, activation temperature is 600-900 DEG C, and soak time is 1-3 hours.
In the present invention, the hole in resulting biomass-based nitrogen-doped porous carbon material is micropore, and its pore-size distribution is 0.4
Between~6nm；The specific surface area of material is in 1600~3500g/m2Between；Nitrogen content is between 5~9wt%.
The present invention compared with the existing technology, has the advantages that：
1st, the present invention is using natural biomass raw material as carbon source, and polymer with nitrogen is that nitrogen source prepares porous carbon materials, and raw material comes
Source is extensively, with low cost；The method activated by high temperature cabonization prepares nitrogen-doped porous carbon material, and preparation method is easy.
2nd, the nitrogen-doped porous carbon material that method of the invention is prepared has high nitrogen content, high specific surface area, hole
Footpath distribution is homogeneous, and typical pore characteristics are presented, and has in fields such as absorption, ultracapacitor, lithium ion batteries and widely should
Use prospect.
Brief description of the drawings
Fig. 1 is the adsorption desorption curve map that embodiment 1 obtains nitrogen-doped porous carbon material.
Fig. 2 is the graph of pore diameter distribution that embodiment 1 obtains nitrogen-doped porous carbon material.
Fig. 3 is the SEM figures that embodiment 1 obtains nitrogen-doped porous carbon material.
Fig. 4 is the TEM figures that embodiment 1 obtains nitrogen-doped porous carbon material.
Embodiment
The following examples can make those skilled in the art that the present invention is more fully understood, but not limit in any form
The present invention.
Embodiment 1
A kind of preparation method of biomass-based nitrogen-doped porous carbon material, comprises the following steps：Biomass material water chestnut is first
First pass through and dry, crush；Then dried biomass and melamine in mass ratio 1 are taken:1 ratio mixing, by aggregate sample
Product carry out high temperature cabonization in a nitrogen atmosphere, and carburizing temperature is 500 DEG C, and the time is 2 hours, and carbonization production is obtained after natural cooling
Thing, then press 1 with KOH:3 mass ratio mixing, then carries out high temperature cabonization activation, temperature is in a nitrogen atmosphere by biased sample
800 DEG C, the time is 2 hours, obtains high content nitrogen doped porous carbon material.The specific surface area of the nitrogen-doped porous carbon material is
3400m2/ g, aperture integrated distribution is in 0.4-4nm, and nitrogen content is 7.4%.
As shown in Figure 1 to 4, Fig. 1 is the nitrogen adsorption desorption curve for the nitrogen-doped porous carbon material that embodiment 1 is obtained, can
To find out this curve as typical I type thermoisopleth, this explanation material shows typical pore characteristics, the specific surface area of the material
Reach 3400m2/g.Fig. 2 is the pore size distribution curve for the nitrogen-doped porous carbon material that embodiment 1 is obtained, as can be seen from Fig., should
Material pore structure is main based on micropore, and aperture is mainly distributed between 0.4-4nm.Fig. 3 is that the N doping that embodiment 1 is obtained is more
The SEM figures of hole carbon material.Fig. 4 is the TEM figures for the nitrogen-doped porous carbon material that embodiment 1 is obtained, as can be seen from Fig., the material
With obvious microcellular structure.
Embodiment 2
A kind of preparation method of biomass-based nitrogen-doped porous carbon material, comprises the following steps：Biomass material water chestnut is first
First pass through and dry, crush；Then dried biomass and melamine in mass ratio 1 are taken:1 ratio mixing, by aggregate sample
Product carry out high temperature cabonization in a nitrogen atmosphere, and carburizing temperature is 500 DEG C, and the time is 2 hours, and carbonization production is obtained after natural cooling
Thing, then press 1 with KOH:1 mass ratio mixing, then carries out high temperature cabonization activation, temperature in a nitrogen atmosphere by biased sample
For 600 DEG C, the time is 1 hour, obtains high content nitrogen doped porous carbon material.The specific surface area of the nitrogen-doped porous carbon material is
1621m2/ g, aperture integrated distribution is in 0.6-3nm, and nitrogen content is 9.2%.
Embodiment 3
A kind of preparation method of biomass-based nitrogen-doped porous carbon material, comprises the following steps：Biomass material water chestnut is first
First pass through and dry, crush；Then dried biomass and melamine in mass ratio 1 are taken:1 ratio mixing, by aggregate sample
Product carry out high temperature cabonization in a nitrogen atmosphere, and carburizing temperature is 500 DEG C, and the time is 2 hours, and carbonization production is obtained after natural cooling
Thing, then press 1 with KOH:4 ratio mixing, then carries out high temperature cabonization activation, temperature is in a nitrogen atmosphere by biased sample
900 DEG C, the time is 3 hours, obtains high content nitrogen doped porous carbon material.The specific surface area of the nitrogen-doped porous carbon material is
2730m2/ g, aperture integrated distribution is in 0.4-6nm, and nitrogen content is 5.3%.
Embodiment 4
A kind of preparation method of biomass-based nitrogen-doped porous carbon material, comprises the following steps：Biomass material water chestnut is first
First pass through and dry, crush；Then dried biomass and melamine in mass ratio 1 are taken:1 ratio mixing, by aggregate sample
Product carry out high temperature cabonization in a nitrogen atmosphere, and carburizing temperature is 500 DEG C, and the time is 2 hours, and carbonization production is obtained after natural cooling
Thing, then press 1 with KOH:2 mass ratio mixing, then carries out high temperature cabonization activation, temperature in a nitrogen atmosphere by biased sample
For 700 DEG C, the time is 2 hours, obtains high content nitrogen doped porous carbon material.The specific surface area of the nitrogen-doped porous carbon material is
3100m2/ g, aperture integrated distribution is in 0.6-4nm, and nitrogen content is 8.1%.
Claims (6)
1. a kind of preparation method of biomass-based nitrogen-doped porous carbon material, it is characterised in that comprise the following steps that：First, will
Biomass material after crushing is mixed in proportion with polymer with nitrogen；Then, sample after mixing is subjected to carbon under an inert atmosphere
Change；Finally, carbonized product is activated with activator, obtains biomass-based nitrogen-doped porous carbon material；Wherein：Biomass is former
Expect for water chestnut.
2. preparation method according to claim 1, it is characterised in that：Polymer with nitrogen is melamine.
3. preparation method according to claim 1, it is characterised in that：The mass ratio of biomass material and polymer with nitrogen is
1:1~3:2, carburizing temperature is 495~505 DEG C.
4. preparation method according to claim 1, it is characterised in that：Activator is KOH, carbonized product and activator matter
Amount is than being 1：1-1：4.
5. preparation method according to claim 1, it is characterised in that：Activation temperature is 600-900 DEG C, and soak time is 1-
3 hours.
6. a kind of preparation method according to one of Claims 1 to 5, it is characterised in that resulting biomass-based nitrogen is mixed
Hole in miscellaneous porous carbon materials is micropore, and its pore-size distribution is between 0.4~6nm；The specific surface area of material 1600~
3500g/m2Between；Nitrogen content is between 5~9wt%.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455597A (en) * | 2018-05-12 | 2018-08-28 | 中国科学院新疆理化技术研究所 | A kind of method and application preparing N doping porous carbon using cotton seed hulls as raw material |
| CN108922794A (en) * | 2018-06-05 | 2018-11-30 | 江苏海基新能源股份有限公司 | A kind of preparation method of N doping biology base active carbon electrode material |
| CN109534341A (en) * | 2019-01-30 | 2019-03-29 | 中国矿业大学 | A kind of preparation method and applications of N doping pericarp base porous carbon material |
| CN109761234A (en) * | 2019-03-27 | 2019-05-17 | 青岛科技大学 | A kind of preparation method of the porous wooden base Carbon Materials of richness nitrogen |
| CN110078046A (en) * | 2019-05-14 | 2019-08-02 | 江西省科学院应用化学研究所 | A kind of preparation and application of nitrogen-doped porous carbon material |
| CN110104647A (en) * | 2019-05-07 | 2019-08-09 | 吉林农业大学 | A kind of preparation method and applications of biomass-based nitrating micro-pore carbon material |
| CN110342512A (en) * | 2019-07-12 | 2019-10-18 | 华中科技大学 | A kind of method of organic solid castoff nitrating hydro-thermal and activation preparation high-performance porous carbon materials |
| CN110395731A (en) * | 2019-07-27 | 2019-11-01 | 大连理工大学 | A kind of preparation method and applications of starch base porous carbon with high specific surface area |
| CN110562976A (en) * | 2019-09-19 | 2019-12-13 | 深圳大学 | High-efficiency electrocatalytic material and preparation method thereof |
| CN110975813A (en) * | 2019-12-18 | 2020-04-10 | 内蒙古大学 | Salix psammophila-based porous carbon and preparation method and application thereof |
| CN111072026A (en) * | 2020-01-20 | 2020-04-28 | 上海应用技术大学 | Hemicellulose-based nitrogen-doped porous carbon material and preparation method and application thereof |
| CN111453726A (en) * | 2019-08-12 | 2020-07-28 | 山东大学 | Nitrogen-doped porous carbon material and preparation method and application thereof |
| CN112299391A (en) * | 2020-10-15 | 2021-02-02 | 南京师范大学 | Water chestnut derived oxygen-doped carbon material and preparation method and application thereof |
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| CN106517197A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing nitrogen-doped porous carbon material for supercapacitor |
| CN106684396A (en) * | 2016-12-21 | 2017-05-17 | 北京化工大学 | Method for preparing bifunctional catalyst from peanut hull |
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Patent Citations (2)
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| CN106517197A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing nitrogen-doped porous carbon material for supercapacitor |
| CN106684396A (en) * | 2016-12-21 | 2017-05-17 | 北京化工大学 | Method for preparing bifunctional catalyst from peanut hull |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455597A (en) * | 2018-05-12 | 2018-08-28 | 中国科学院新疆理化技术研究所 | A kind of method and application preparing N doping porous carbon using cotton seed hulls as raw material |
| CN108922794A (en) * | 2018-06-05 | 2018-11-30 | 江苏海基新能源股份有限公司 | A kind of preparation method of N doping biology base active carbon electrode material |
| CN109534341A (en) * | 2019-01-30 | 2019-03-29 | 中国矿业大学 | A kind of preparation method and applications of N doping pericarp base porous carbon material |
| CN109534341B (en) * | 2019-01-30 | 2021-02-26 | 中国矿业大学 | Preparation method and application of nitrogen-doped pericarp-based porous carbon material |
| CN109761234A (en) * | 2019-03-27 | 2019-05-17 | 青岛科技大学 | A kind of preparation method of the porous wooden base Carbon Materials of richness nitrogen |
| CN110104647A (en) * | 2019-05-07 | 2019-08-09 | 吉林农业大学 | A kind of preparation method and applications of biomass-based nitrating micro-pore carbon material |
| CN110078046B (en) * | 2019-05-14 | 2020-09-08 | 江西省科学院应用化学研究所 | Preparation and application of nitrogen-doped porous carbon material |
| CN110078046A (en) * | 2019-05-14 | 2019-08-02 | 江西省科学院应用化学研究所 | A kind of preparation and application of nitrogen-doped porous carbon material |
| CN110342512A (en) * | 2019-07-12 | 2019-10-18 | 华中科技大学 | A kind of method of organic solid castoff nitrating hydro-thermal and activation preparation high-performance porous carbon materials |
| CN110342512B (en) * | 2019-07-12 | 2021-04-16 | 华中科技大学 | Method for preparing high-performance porous carbon material by nitrogen-doped hydrothermal and activation of organic solid waste |
| CN110395731A (en) * | 2019-07-27 | 2019-11-01 | 大连理工大学 | A kind of preparation method and applications of starch base porous carbon with high specific surface area |
| CN111453726A (en) * | 2019-08-12 | 2020-07-28 | 山东大学 | Nitrogen-doped porous carbon material and preparation method and application thereof |
| WO2021027100A1 (en) * | 2019-08-12 | 2021-02-18 | 山东大学 | Nitrogen-doped porous carbon material, preparation method therefor and use thereof |
| CN110562976A (en) * | 2019-09-19 | 2019-12-13 | 深圳大学 | High-efficiency electrocatalytic material and preparation method thereof |
| CN110975813A (en) * | 2019-12-18 | 2020-04-10 | 内蒙古大学 | Salix psammophila-based porous carbon and preparation method and application thereof |
| CN111072026A (en) * | 2020-01-20 | 2020-04-28 | 上海应用技术大学 | Hemicellulose-based nitrogen-doped porous carbon material and preparation method and application thereof |
| CN112299391A (en) * | 2020-10-15 | 2021-02-02 | 南京师范大学 | Water chestnut derived oxygen-doped carbon material and preparation method and application thereof |
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