CN105084351A - Preparation method for nitrogen-doped graphene hydrogel - Google Patents
Preparation method for nitrogen-doped graphene hydrogel Download PDFInfo
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- CN105084351A CN105084351A CN201510388228.7A CN201510388228A CN105084351A CN 105084351 A CN105084351 A CN 105084351A CN 201510388228 A CN201510388228 A CN 201510388228A CN 105084351 A CN105084351 A CN 105084351A
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Abstract
The invention discloses a preparation method for a nitrogen-doped graphene hydrogel and relates to a preparation method for nitrogen-doped graphene hydrogel in a low temperature condition. The preparation method comprises: take graphene oxide to prepare a solution with a certain concentration; in the preparation process, ensuring full stirring and ultrasonic treatment to form a uniformly dispersed sheet graphite oxide solution; adding the prepared solution into ammonium hydrogen carbonate; then carrying out stirring and ultrasonic treatment to fully mix the mixture; adding sodium sulfate into the prepared solution to be stirred so as to dissolve the sodium sulfate; then putting the solution in an oven to be heated; taking out a sample from the oven; and cleaning the sample by clean water for many times to obtain the nitrogen-doped graphene hydrogel material.
Description
Technical field
The present invention relates to the inner doping field of Graphene hydrogel, is a kind of preparation method producing nitrogen-doped graphene hydrogel under cryogenic.Be applicable to the field such as ultracapacitor, Chu Qing.
Background technology
At present, Graphene can be called as the two-dimension nano materials having using value most, not only there is very unique internal structure in it, and has very excellent optical property, mechanical property, thermal property and electrical properties, and then cause investigators' interest greatly.But because himself size of grapheme material of two dimension is less, increase in some cases and carry out processing the difficulty used to it, this is very large to a certain extent limits the application of grapheme material in real life.Three-dimensional grapheme material has higher specific surface area, be rich in pore texture, have good electroconductibility, thermostability and other aspect character, therefore, in fields such as ultracapacitor, Chu Qing, biomedicine, water treatment and new catalytics, there is important potential using value.In recent years, research finds, N doping method is a kind of important means improving the conductivity of Graphene self.N doping process is introduced in the process preparing Graphene hydrogel, its internal structure is modified, be expected to prepare the relatively better nitrogen-doped graphene hydrogel of chemical property.
This patent is intended to provide a kind of new type low temperature N doping method, and preparation condition is relatively more simple, safety.
Summary of the invention
The object of the present invention is to provide a kind of preparation condition relatively simple nitrogen-doped graphene hydrogel material of gentleness, technique and preparation method thereof relatively.
Technical scheme of the present invention:
A preparation method for nitrogen-doped graphene hydrogel, the detailed process of this preparation method is:
Step one, prepares certain density graphene oxide solution, ensures to stir fully and ultrasonic in process for preparation, forms finely dispersed lamella graphite oxide solution;
Step 2, adds bicarbonate of ammonia in step one obtain solution, carries out stirring and ultrasonic afterwards, makes it mix fully;
Step 3, adds sodium sulphite in step 2 institute obtain solution, stirs, make it dissolve;
Step 4, puts into baking oven by step 3 gained solution and heats;
Step 5, takes out sample from baking oven, and the cleaning carrying out repeatedly to sample with clear water, obtains nitrogen-doped graphene hydrogel material.
Advantage of the present invention is: (1) three-dimensional grapheme material is rich in pore texture, there is higher specific surface area, lower density and good electroconductibility, and by N doping method, it is modified, the size of its internal void can be promoted, make nitrogen-doped graphene hydrogel material have important using value in ultracapacitor, Chu Qing field.(2) when preparing material, required medicine is comparatively common, and cost is lower, and preparation condition is comparatively gentle simultaneously, preparation technology is comparatively simple, easy handling.
Accompanying drawing explanation
Fig. 1 is the SEM figure of nitrogen-doped graphene hydrogel of the present invention
Fig. 2 is the XPS figure of nitrogen-doped graphene hydrogel of the present invention
Embodiment
Following instance further illustrates the present invention, but not as a limitation of the invention.According to following preparation flow, carry out the preparation of nitrogen-doped graphene hydrogel.
Embodiment 1
Step one, utilizes the Hummers legal system improved for graphene oxide;
Step 2, graphene oxide step one obtained is formulated as the graphene oxide solution of 2mg/mL, and carries out stirring fully and ultrasonic, and stirring and ultrasonic time are respectively 30min;
Step 3, gets 1mL graphene oxide solution that step 2 is prepared, preparation 79g/L ammonium bicarbonate soln, and gets in the graphene oxide solution of 30 μ L instillation 1mL, stirs 30min, makes its Homogeneous phase mixing;
Step 4, the sodium sulfide solution of preparation 240g/L, and get 52 μ L instillations in step 3 gained solution, stir 30min, make its Homogeneous phase mixing;
Step 5, puts into baking oven by step 4 gained solution, with the heating temperatures 10 hours of 90 DEG C;
Step 6, after having heated, take out sample from baking oven, clean with deionized water, after cleaning 5-6 time, the material that obtains is nitrogen-doped graphene hydrogel material;
Embodiment 2
Step one, as in embodiment 1, step one prepares graphene oxide;
Step 2, graphene oxide step one obtained is formulated as the graphene oxide solution of 1mg/mL, and carries out stirring fully and ultrasonic, and stirring and ultrasonic time are respectively 30min;
Step 3, gets 1mL graphene oxide solution that step 2 is prepared, preparation 79g/L ammonium bicarbonate soln, and gets in the graphene oxide solution of 30 μ L instillation 1mL, stirs 30min, makes its Homogeneous phase mixing;
Step 4, the sodium sulfide solution of preparation 240g/L, and get 52 μ L instillations in step 3 gained solution, stir 30min, make its Homogeneous phase mixing;
Step 5, puts into baking oven by step 4 gained solution, with the heating temperatures 10 hours of 90 DEG C;
Step 6, after having heated, take out sample from baking oven, clean with deionized water, after cleaning 5-6 time, the material that obtains is nitrogen-doped graphene hydrogel material.
Embodiment 3
Step one, as in embodiment 1, step one prepares graphene oxide;
Step 2, graphene oxide step one obtained is formulated as the graphene oxide solution of 2mg/mL, and carries out stirring fully and ultrasonic, and stirring and ultrasonic time are respectively 30min;
Step 3, gets 1mL graphene oxide solution that step 2 is prepared, preparation 79g/L ammonium bicarbonate soln, and gets in the graphene oxide solution of 60 μ L instillation 1mL, stirs 30min, makes its Homogeneous phase mixing;
Step 4, the sodium sulfide solution of preparation 240g/L, and get 52 μ L instillations in step 3 gained solution, stir 30min, make its Homogeneous phase mixing;
Step 5, puts into baking oven by step 4 gained solution, with the heating temperatures 10 hours of 90 DEG C;
Step 6, after having heated, take out sample from baking oven, clean with deionized water, after cleaning 5-6 time, the material that obtains is nitrogen-doped graphene hydrogel material.
Embodiment 4
Step one, as in embodiment 1, step one prepares graphene oxide;
Step 2, graphene oxide step one obtained is formulated as the graphene oxide solution of 2mg/mL, and carries out stirring fully and ultrasonic, and stirring and ultrasonic time are respectively 30min;
Step 3, gets 1mL graphene oxide solution that step 2 is prepared, preparation 79g/L ammonium bicarbonate soln, and gets in the graphene oxide solution of 30 μ L instillation 1mL, stirs 30min, makes its Homogeneous phase mixing;
Step 4, the sodium sulfide solution of preparation 240g/L, and get 26 μ L instillations in step 3 gained solution, stir 30min, make its Homogeneous phase mixing;
Step 5, puts into baking oven by step 4 gained solution, with the heating temperatures 10 hours of 90 DEG C;
Step 6, after having heated, take out sample from baking oven, clean with deionized water, after cleaning 5-6 time, the material that obtains is nitrogen-doped graphene hydrogel material.
Claims (6)
1. a preparation method for nitrogen-doped graphene hydrogel, is characterized in that, the step of this preparation method comprises:
Step one, prepares certain density graphene oxide solution, ensures to stir fully and ultrasonic in process for preparation, forms finely dispersed lamella graphite oxide solution;
Step 2, adds bicarbonate of ammonia in step one obtain solution, carries out stirring and ultrasonic afterwards, makes it mix fully;
Step 3, adds sodium sulphite in step 2 institute obtain solution, stirs, make it dissolve;
Step 4, puts into baking oven by step 3 gained solution and heats;
Step 5, takes out sample from baking oven, and the cleaning carrying out repeatedly to sample with clear water, obtains nitrogen-doped graphene hydrogel material.
2. the preparation method of a kind of nitrogen-doped graphene hydrogel material according to claim 1, is characterized in that, the concentration of described graphene oxide solution is 1mg/mL ~ 5mg/mL.
3. the preparation method of a kind of nitrogen-doped graphene hydrogel material according to claim 1, is characterized in that, described nitrogenous source is bicarbonate of ammonia.
4. the preparation method of a kind of nitrogen-doped graphene hydrogel material according to claim 1, is characterized in that, described reductive agent is sodium sulphite.
5. the preparation method of a kind of nitrogen-doped graphene hydrogel material according to claim 1, is characterized in that, described Heating temperature is 90 DEG C-120 DEG C.
6. the preparation method of a kind of nitrogen-doped graphene hydrogel material according to claim 1, it is characterized in that, the amount ratio of graphene oxide and nitrogenous source bicarbonate of ammonia is 2:1 ~ 8:1, and the amount ratio of graphene oxide and reductive agent sodium sulphite is that wherein amount ratio is mass ratio 1:4 ~ 4:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946247A (en) * | 2017-02-27 | 2017-07-14 | 天津大学 | A kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689896A (en) * | 2012-03-15 | 2012-09-26 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene oxide through simultaneously performing reduction and nitrogen doping functionalization |
| CN102757029A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Nitrogen doped graphene material and preparation method thereof |
| CN103165866A (en) * | 2011-12-14 | 2013-06-19 | 海洋王照明科技股份有限公司 | Nitrogen doped graphene/metal composite electrode and its preparation method |
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| CN103840160A (en) * | 2012-11-23 | 2014-06-04 | 海洋王照明科技股份有限公司 | Nitrogen-doped graphene composite material and preparation method thereof |
| CN104607228A (en) * | 2015-01-23 | 2015-05-13 | 哈尔滨工业大学 | Preparation method for alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material |
-
2015
- 2015-07-03 CN CN201510388228.7A patent/CN105084351A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757029A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Nitrogen doped graphene material and preparation method thereof |
| CN103165866A (en) * | 2011-12-14 | 2013-06-19 | 海洋王照明科技股份有限公司 | Nitrogen doped graphene/metal composite electrode and its preparation method |
| CN102689896A (en) * | 2012-03-15 | 2012-09-26 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene oxide through simultaneously performing reduction and nitrogen doping functionalization |
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| CN103840160A (en) * | 2012-11-23 | 2014-06-04 | 海洋王照明科技股份有限公司 | Nitrogen-doped graphene composite material and preparation method thereof |
| CN104607228A (en) * | 2015-01-23 | 2015-05-13 | 哈尔滨工业大学 | Preparation method for alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material |
Non-Patent Citations (1)
| Title |
|---|
| HAO XIN ET AL: "Low-temperature preparation of macroscopic nitrogen-doped graphene hydrogel for high performance ultrafast supercapacitors", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946247A (en) * | 2017-02-27 | 2017-07-14 | 天津大学 | A kind of preparation method of many active sites nitrogen-doped graphenes of laser irradiation synthesis |
| CN106946247B (en) * | 2017-02-27 | 2019-02-19 | 天津大学 | A kind of laser irradiation synthesizes the preparation method of more active sites nitrogen-doped graphenes |
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