CN104250003B - A kind of preparation method of nitrogen doping porous carbon nanometer sheet - Google Patents
A kind of preparation method of nitrogen doping porous carbon nanometer sheet Download PDFInfo
- Publication number
- CN104250003B CN104250003B CN201410461866.2A CN201410461866A CN104250003B CN 104250003 B CN104250003 B CN 104250003B CN 201410461866 A CN201410461866 A CN 201410461866A CN 104250003 B CN104250003 B CN 104250003B
- Authority
- CN
- China
- Prior art keywords
- charing
- preparation
- nanometer sheet
- aeroge
- porous carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to a kind of preparation method of nitrogen doping porous carbon nanometer sheet. The present invention, taking natural biomass as raw material, adopts low-temperature hydrothermal method to process original biomass, obtains the hydrogel of hydro-thermal charing, wash, freeze drying, obtain the aeroge of charing, the aeroge of charing is used to ammonia atmosphere heat treatment in tube furnace, obtain product. The present invention is carbon source with plant, and source nature, can circulate, non-environmental-pollution, and this biological quality is large. Whole material preparation method is simple, and raw material, as long as plant does not need other organic solvents, are easy to realize industrialization.
Description
Technical field
The invention belongs to carbon nanomaterial field, relate in particular to a kind of preparation method of nitrogen doping porous carbon nanometer sheet.
Background technology
Can change very many-sided performance of material with carbon element because nitrogen adulterates, nitrogen-doped carbon material has potential application in a lot of fields. At present, chemical vapour deposition (CVD) is sent out, the method such as Ammonia gas disposal is sent out, Cement Composite Treated by Plasma is for the synthesis of nitrogen-doped carbon material. Porous carbon materials, owing to having large specific area, is widely used at aspects such as electro-catalysis, organic catalysis, ultracapacitor, photocatalysis, sewage disposal, gas absorption. Develop simple to operate, raw material source cheaply and widely method prepare nitrogen doping porous carbon nano material, particularly nanometer sheet is significant.
Summary of the invention
In view of this, the technical problem to be solved in the present invention be to provide a kind of with natural biomass be the method that raw material is prepared nitrogen doping porous carbon nanometer sheet, nitrogen doping porous carbon nanometer sheet provided by the invention shows significant oxygen Electrochemical Properties.
The present invention adopts following technical scheme to achieve these goals:
A preparation method for nitrogen doping porous carbon nanometer sheet, is characterized in that: comprise the following steps:
A) adopt low-temperature hydrothermal method to process natural biomass, obtain the hydrogel of hydro-thermal charing;
B) hydrogel of hydro-thermal charing wash, freeze drying, obtain the aeroge of charing;
C) aeroge of charing is used to ammonia atmosphere heat treatment in tube furnace, obtain product.
The preparation method of described a kind of nitrogen doping porous carbon nanometer sheet, is characterized in that: described step a) specifically comprises: take appropriate natural biomass, put in reactor, then add distilled water, hydrothermal temperature is 160-210oC, time 7-16h.
The preparation method of described a kind of nitrogen doping porous carbon nanometer sheet, is characterized in that: described step c) specifically comprises: the aeroge of charing is used to ammonia atmosphere heat treatment in tube furnace, temperature: 750-850oC, time 0.5-2.5h, obtains product.
The preparation method of described a kind of nitrogen doping porous carbon nanometer sheet, is characterized in that: while often taking 4-8 gram of natural biomass in described step a), add distilled water 12-25ml.
The preparation method's of described nitrogen doping porous carbon nanometer sheet preparation method, is characterized in that: described natural biomass refers to plant.
Described natural biomass refers to cattail rod.
After crushing, cattail rod obtains cattail suede fiber.
Compared with prior art, the invention provides the carbon nanosheet preparation method of a kind of high nitrogen content, large specific area and a large amount of micropores, the present invention has following features:
1. be carbon source with plant, source nature, can circulate, non-environmental-pollution, and this biological quality is large. Whole material preparation method is simple, and raw material, as long as plant does not need other organic solvents, are easy to realize industrialization.
2. synthetic carbon plate, has very outstanding oxygen electrical catalyze reduction performance, in alkaline medium, shows the performance of the platinum carbon (20%) of similar business.
3. synthetic carbon plate, BET surface area is very large, has a large amount of micropores, and the nitrogen element content of doping is high. This material probably also can have potential using value in various fields such as ultracapacitor, lithium ion battery, organic catalysis, photocatalysis, gas absorption.
Described nitrogen-doped carbon nanometer sheet utilizes natural biomass for carbon source, prepares nanometer sheet, and described nitrogen-doped carbon nanometer sheet has very high nitrogen content, and described nitrogen-doped carbon nanometer sheet has large specific area and a large amount of micropore.
Nitrogen doping porous carbon nanometer sheet provided by the invention shows has very outstanding oxygen electrical catalyze reduction performance, in alkaline medium, shows the performance of the platinum carbon (20%) of similar business.
Method prepared by the present invention is carbon source with plant, and source nature, can circulate, non-environmental-pollution, and this biological quality is large. Whole material preparation method is simple, and raw material, as long as plant does not need other organic solvents, are easy to realize industrialization.
Carbon nanosheet prepared by the present invention has large specific area and a large amount of micropore, activator activation is not used in the generation of these micropores, also do not use template, but the method for utilizing original biomass oneself to produce vegetable oil in heat treatment obtains micropore and large specific area.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of the product for preparing of the embodiment of the present invention 1;
Fig. 2 is the transmission electron microscope photo of the product for preparing of the embodiment of the present invention 1;
Fig. 3 is the photoelectron spectroscopy figure of the product for preparing of the embodiment of the present invention 1;
Fig. 4 is the BET result of the product for preparing of the embodiment of the present invention 1;
Fig. 5 is the oxygen electroreduction catalytic performance of the product for preparing of the embodiment of the present invention 1.
Detailed description of the invention、
In order to further illustrate the present invention, below in conjunction with embodiment, product preparation method provided by the invention is described in detail.
Embodiment 1
Take 4 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 50mL, then to add 12mL distilled water, hydrothermal temperature be 180oC, time 8h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 800 in tube furnaceoC, time 1.5h. Obtain product.
Embodiment 2
Take 8 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 100mL, then to add 25mL distilled water, hydrothermal temperature be 160oC, time 12h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 820 in tube furnaceoC, time 1.5h. Obtain product.
Embodiment 3
Take 4 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber,, put in the reactor of 50mL, then to add 12mL distilled water, hydrothermal temperature be 160oC, time 15h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 800 in tube furnaceoC, time 2.5h. Obtain product.
Embodiment 4
Take 4 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber,, put in the reactor of 50mL, then to add 12mL distilled water, hydrothermal temperature be 180oC, time 13h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 780 in tube furnaceoC, time 2h. Obtain product.
Embodiment 5
Take 4 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 50mL, then to add 12mL distilled water, hydrothermal temperature be 190oC, time 7h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 750 in tube furnaceoC, time 2h. Obtain product.
Embodiment 6
Take 8 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 100mL, then to add 25mL distilled water, hydrothermal temperature be 160oC, time 16h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 850 in tube furnaceoC, time 2h. Obtain product.
Embodiment 7
Take 8 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 100mL, then to add 25mL distilled water, hydrothermal temperature be 180oC, time 11h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 820 in tube furnaceoC, time 1.2h. Obtain product.
Embodiment 8
Take 8 grams of natural biomass (cattail rod), after crushing, obtain cattail suede fiber, put in the reactor of 100mL, then to add 25mL distilled water, hydrothermal temperature be 170oC, time 10h. Distillation washing for product, filtered through gauze, obtains the hydrogel of hydro-thermal charing. To the hydrogel freeze drying of hydro-thermal charing, obtain the aeroge of charing. The aeroge of charing is used to ammonia atmosphere heat treatment, 800 in tube furnaceoC, time 2.5h. Obtain product.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for nitrogen doping porous carbon nanometer sheet, is characterized in that: comprise the following steps:
A) adopt low-temperature hydrothermal method to process natural biomass, obtain the hydrogel of hydro-thermal charing; Described natural biomass is cattail suede fiber;
B) hydrogel of hydro-thermal charing wash, freeze drying, obtain the aeroge of charing;
C) aeroge of charing is used to ammonia atmosphere heat treatment in tube furnace, obtain product.
2. the preparation method of a kind of nitrogen doping porous carbon nanometer sheet according to claim 1, it is characterized in that: described step a) specifically comprises: take appropriate natural biomass, put in reactor, then add distilled water, hydrothermal temperature is 160-210 DEG C, time 7-16h.
3. the preparation method of a kind of nitrogen doping porous carbon nanometer sheet according to claim 1 and 2, it is characterized in that: described step c) specifically comprises: the aeroge of charing is used to ammonia atmosphere heat treatment in tube furnace, temperature: 750-850 DEG C, time 0.5-2.5h, obtains product.
4. the preparation method of a kind of nitrogen doping porous carbon nanometer sheet according to claim 2, is characterized in that: while often taking 4-8 gram of natural biomass in described step a), add distilled water 12-25ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410461866.2A CN104250003B (en) | 2014-09-11 | 2014-09-11 | A kind of preparation method of nitrogen doping porous carbon nanometer sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410461866.2A CN104250003B (en) | 2014-09-11 | 2014-09-11 | A kind of preparation method of nitrogen doping porous carbon nanometer sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104250003A CN104250003A (en) | 2014-12-31 |
| CN104250003B true CN104250003B (en) | 2016-05-25 |
Family
ID=52185294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410461866.2A Active CN104250003B (en) | 2014-09-11 | 2014-09-11 | A kind of preparation method of nitrogen doping porous carbon nanometer sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104250003B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785283A (en) * | 2015-03-25 | 2015-07-22 | 江西师范大学 | Method for preparing efficient oxygen reduction catalyst from straw and application of efficient oxygen reduction catalyst to neutral battery |
| CN105084358A (en) * | 2015-07-23 | 2015-11-25 | 南昌航空大学 | Nitrogen and sulfur-co-doped active carbon for supercapacitor and preparation method for nitrogen and sulfur-co-doped active carbon for supercapacitor |
| CN105854801A (en) * | 2016-05-10 | 2016-08-17 | 江苏大学 | Nitrogen-doped porous carbon material and preparation method and application thereof |
| CN107369563B (en) * | 2016-05-12 | 2021-01-26 | 复旦大学 | Preparation method of nickel sulfide particle/cellulose-based composite carbon aerogel material |
| CN106252673B (en) * | 2016-08-22 | 2019-06-25 | 首都师范大学 | A kind of preparation method of the Fe-N/C oxygen reduction reaction catalyst based on natural plants tissue |
| CN106684396A (en) * | 2016-12-21 | 2017-05-17 | 北京化工大学 | Method for preparing bifunctional catalyst from peanut hull |
| CN107331865B (en) * | 2017-05-31 | 2019-12-13 | 郑州轻工业学院 | Preparation method of cellulose nanofiber/silk fibroin-based porous nitrogen-doped 2D carbon nanosheet electrode material |
| CN107522198A (en) * | 2017-07-31 | 2017-12-29 | 西安理工大学 | The preparation method of biomass porous carbon and carbon sulphur composite based on oriental cherry |
| CN107555412A (en) * | 2017-09-07 | 2018-01-09 | 江苏福瑞士电池科技有限公司 | A kind of preparation method of N doping porous carbon and its application on lithium ion battery |
| CN107824797B (en) * | 2017-10-10 | 2020-02-11 | 广州盈思传感科技有限公司 | Porous high-specific-surface-area bismuth nanoparticle modified nitrogen-doped carbon nanosheet material and preparation method and application thereof |
| CN107583665A (en) * | 2017-10-20 | 2018-01-16 | 南京大学 | A kind of preparation method of the porous nitrogen-doped carbon nanometer sheet of two dimension and application thereof |
| CN108083261B (en) * | 2018-01-02 | 2019-12-17 | 中国科学院上海硅酸盐研究所 | three-dimensional porous carbon material, three-dimensional porous nitrogen-doped carbon material, and preparation method and application thereof |
| CN108630942B (en) * | 2018-05-11 | 2020-06-23 | 东莞理工学院 | Nitrogen-doped carbon foam negative electrode material and preparation method and application thereof |
| CN109850871B (en) * | 2019-01-28 | 2022-06-28 | 安徽大学 | Nitrogen-doped porous carbon nanosheet and preparation method thereof |
| CN112079352B (en) * | 2019-06-13 | 2021-12-14 | 南京林业大学 | Preparation method and application of biomass-based porous nitrogen-doped carbon material |
| US11124415B2 (en) | 2019-09-25 | 2021-09-21 | King Fahd University Of Petroleum And Minerals | Nitrogen enriched carbon derived from Albizia procera leaves |
| CN111326755A (en) * | 2019-12-09 | 2020-06-23 | 中国人民解放军军事科学院军事医学研究院 | Banana peel-derived ribbed porous carbon as electrode material for fully oxidizing methanol and methanol fuel cells |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627268B (en) * | 2011-09-28 | 2013-10-23 | 兰州理工大学 | Preparation method of nitrogen-doped carbon material |
| CN103406096B (en) * | 2013-07-17 | 2015-06-03 | 国家纳米科学中心 | Nitrogen-doped porous carbon material, preparation method and use thereof |
-
2014
- 2014-09-11 CN CN201410461866.2A patent/CN104250003B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104250003A (en) | 2014-12-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104250003B (en) | A kind of preparation method of nitrogen doping porous carbon nanometer sheet | |
| Chakraborty et al. | Recent advancement of biomass-derived porous carbon based materials for energy and environmental remediation applications | |
| Li et al. | Green conversion of bamboo chips into high-performance phenol adsorbent and supercapacitor electrodes by simultaneous activation and nitrogen doping | |
| Zhang et al. | Microbial targeted degradation pretreatment: a novel approach to preparation of activated carbon with specific hierarchical porous structures, high surface areas, and satisfactory toluene adsorption performance | |
| Li et al. | A critical review on the application and recent developments of post-modified biochar in supercapacitors | |
| Luo et al. | Synthesis of 3D-interconnected hierarchical porous carbon from heavy fraction of bio-oil using crayfish shell as the biological template for high-performance supercapacitors | |
| Zhou et al. | Upgrading earth-abundant biomass into three-dimensional carbon materials for energy and environmental applications | |
| CN104009242B (en) | The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load | |
| Tatrari et al. | Solid waste-derived carbon nanomaterials for supercapacitor applications: a recent overview | |
| Ndlwana et al. | Sustainable hydrothermal and solvothermal synthesis of advanced carbon materials in multidimensional applications: A review | |
| Zeng et al. | Seaweed-derived nitrogen-rich porous biomass carbon as bifunctional materials for effective electrocatalytic oxygen reduction and high-performance gaseous toluene absorbent | |
| CN104045077A (en) | Graphene three-dimensional hierarchical porous carbon material and preparation method thereof | |
| Li et al. | Osmanthus fragrans-derived N-doped porous carbon for supercapacitor applications | |
| CN103922305A (en) | Preparation method of high nitrogen content-doped porous carbon with high specific surface area | |
| CN104909363B (en) | A kind of preparation method of meshed nano structure material with carbon element | |
| CN103601913A (en) | Graphene/polypyrrole hybrid aerogel and preparation method thereof | |
| Shen et al. | A facile synthesis of nitrogen-doped porous carbons from lignocellulose and protein wastes for VOCs sorption | |
| CN103990485A (en) | Carbon nitride nano particle modified pucherite composite photocatalyst and preparation method thereof | |
| CN107902653A (en) | For air purification and the shaddock peel activated carbon one-step preppn process of sewage disposal | |
| Saka | Sulphur and nitrogen-doped metal-free microalgal carbon catalysts for very active dehydrogenation of sodium borohydride in methanol | |
| Ma et al. | Preparation of nitrogen-doped hierarchical porous carbon aerogels from agricultural wastes for efficient pollution adsorption | |
| Taer et al. | Averrhoa bilimbi leaves-derived oxygen doped 3D-linked hierarchical porous carbon as high-quality electrode material for symmetric supercapacitor | |
| CN106207197A (en) | A kind of method using hair to prepare bifunctional electrocatalyst | |
| CN106115688A (en) | A kind of method that natural cryptogam self-template method prepares Porous hollow activated carbon microballon | |
| CN105731446A (en) | Preparation method and product of ultrahigh-specific-area sulphur-nitrogen-co-doped porous graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20141231 Assignee: Chizhou Kecheng new material development Co., Ltd. Assignor: Anhui University Contract record no.: X2019340000004 Denomination of invention: Method for preparing nitrogen-doped porous carbon nanoflakes Granted publication date: 20160525 License type: Exclusive License Record date: 20190926 |