CN105776199A - Method for reducing graphene oxide - Google Patents
Method for reducing graphene oxide Download PDFInfo
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- CN105776199A CN105776199A CN201610336253.5A CN201610336253A CN105776199A CN 105776199 A CN105776199 A CN 105776199A CN 201610336253 A CN201610336253 A CN 201610336253A CN 105776199 A CN105776199 A CN 105776199A
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- graphene oxide
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- hydrazine hydrate
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Abstract
The invention discloses a method for reducing graphene oxide. The method comprises the following steps: preparing a solution, namely, mixing N,N-dimethyl benzene methanamine and hydrazine hydrate according to a volume ratio less than or equal to 1:3; putting thin graphene oxide and the mixed solution in the step a into a reflux unit, wherein the pressure intensity in the container is not less than minus 0.1MPa; and enabling the components to react in an oil bath environment of 60-80 DEG C for no less than 24 hours. The method is simple to operate, materials are easy to obtain and low in price, and a product (graphene) obtained after reduction is relatively large in area and uniform in texture.
Description
Technical field
The invention belongs to materials science field, a kind of method relating generally to redox graphene, it is particularly well-suited to the reduction of lamella graphene oxide.
Background technology
Graphene is found first by An Delie Jim and Ke Siteyanuowoxiaoge husband, is one of the most popular material.The single layer crystal that it is made up of carbon atom, its lattice is the hexagon surrounded by six carbon atom, and thickness is an atomic layer.Between carbon atom bonded by σ, hybrid form is sp2 hydridization.Although Graphene is the thinnest, but its intensity is the highest, has extraordinary pliability simultaneously.
The C atom constituting Graphene is in sp2 hybridization state, and the pi-electron delocalization of each C atom forms big π key.Therefore the good conductor that Graphene can provide substantial amounts of free electron, i.e. Graphene to be electricity.And the stable electrical properties of Graphene, change hardly being heated, in the case of pressurized；After modifying Graphene, Graphene electric capacity changes little in tens of rear capacitances of repeated charge, thus Graphene may make up stable vast capacity electric capacity, provides stable electric current for a long time.
In cell experiment and organizational project, often different base materials and living cells are combined as biological substitution product and repair, and finally improve the function of tissue.Graphite provides a kind of promising biocompatible substrate.Owing to differentiation rate and common somatomedin are suitable, illustrate Graphene potentiality in terms of stem-cell research, i.e. Graphene and can accelerate stem cell and break up in a controlled manner.
At present all kinds of method of reducing effect deviations of graphene oxide are very big, it is impossible to good control reduction functional group, the method that this technology is applied, for graphene oxide carbonyl reduction effect substantially, the reducing property being expected to realize graphene oxide is controlled.
Summary of the invention
Solve the technical problem that:The present invention provides a kind of method of redox graphene, and its reduction effect is good, and reaction condition is gentle, and controllability is strong.
Technical scheme:A kind of method of redox graphene, preparation process is: (a) prepares solution: N, N-dimethyl-benzyl amine and hydrazine hydrate are mixed less than or equal to 1:3 according to volume ratio；B mixed solution described in thin-layer graphene oxide and step a is placed in reflux by (), in container, pressure is not less than-0.1MPa；C () is reacted in 60 DEG C ~ 80 DEG C oil bath environment again, the response time is no less than 24h.
Preferably, the volume ratio of described N, N-dimethyl-benzyl amine and hydrazine hydrate is 1:4.
Preferably, described reaction pressure is-0.1MPa.
Preferably, described reaction temperature is 60 DEG C.
Preferably, the described response time is 24h.
Beneficial effect:During preparing material, simple to operate, reaction condition is gentle, and the graphene sheet layer integrity prepared is good.This method of reducing is obvious for the carbonyl functional group's reduction effect in graphene oxide, is expected to develop the method for reducing of the controlled graphene oxide of a class performance.
Accompanying drawing explanation
Fig. 1: graphene oxide infared spectrum；
Fig. 2: N, N-dimethyl-benzyl amine and hydrazine hydrate mixed liquor reduzate infared spectrum I；
Fig. 3: N, N-dimethyl-benzyl amine and hydrazine hydrate mixed liquor reduzate infared spectrum II.
Detailed description of the invention
The following examples can make those skilled in the art can be apparent from the present invention, but limits the present invention never in any form.Thin-layer graphene oxide used herein all utilizes following methods to obtain, the graphene oxide solution of 0.8 ~ 1.0mg/mL, in clean glass sheet surface, 600r/min spin coating is placed in vacuum drying oven not less than the sheet glass that 4min prepares and is dried at least 2h, prepares thin-layer graphene oxide.
Embodiment
1
:
Preparation solution, the mixed liquor of 10mLN, N-dimethyl-benzyl amine and 40mL hydrazine hydrate is placed in the flask being provided with reflux；
The sheet glass of attachment coating graphene oxide is placed in reflux, not contact liq, and by flask evacuation-0.1MPa；60 DEG C of oil bath reaction 24h.Reduction afterproduct carries out Infrared Characterization, and characterization result such as Fig. 2, this reaction gained reduction peak area is little for optimum.
Embodiment
2
:
Preparation solution, the mixed liquor of 5mLN, N-dimethyl-benzyl amine and 15mL hydrazine hydrate is placed in the flask being provided with reflux；The sheet glass of attachment coating graphene oxide is placed in reflux, not contact liq；80 DEG C of oil bath reaction 24h.Reduction afterproduct carries out Infrared Characterization, characterization result such as Fig. 3.
Embodiment
3
:
Preparation solution, the mixed liquor of 10mLN, N-dimethyl-benzyl amine and 45mL hydrazine hydrate is placed in the flask being provided with reflux；The sheet glass of attachment coating graphene oxide is placed in reflux, not contact liq；And by flask evacuation-0.05MPa；70 DEG C of oil bath reaction 10h.Reduction afterproduct carries out Infrared Characterization, and reduction effect is the best.
Embodiment
4
:
Preparation solution, the mixed liquor of 10mLN, N-dimethyl-benzyl amine and 50mL hydrazine hydrate is placed in the flask being provided with reflux；The sheet glass of attachment coating graphene oxide is placed in reflux, not contact liq；65 DEG C of oil bath reaction 35h.Reduction afterproduct carries out Infrared Characterization, and reduction effect is the best.
Embodiment
5
:
Preparation solution, the mixed liquor of 5mLN, N-dimethyl-benzyl amine and 10mL hydrazine hydrate is placed in the flask being provided with reflux；The sheet glass of attachment coating graphene oxide is placed in reflux, not contact liq；30 DEG C of oil bath reaction 24h.Finally do not obtain Graphene, test unsuccessful.
Interpretation of result:
Comparing Fig. 1, Fig. 2, Fig. 3 are at 2370cm-1Neighbouring peak area significantly reduces, and the peak of this position is C=O key.In graphene oxide, the content of C=O is the highest, and after reduction, C=O almost disappears.Therefore, use our method of reducing can effectively reduce the content of oxygen atom in graphene oxide, especially C=O is had high reduction effect.
Claims (5)
1. the method for a redox graphene, it is characterised in that preparation process is:
A) preparation solution: N, N-dimethyl-benzyl amine and hydrazine hydrate are mixed less than or equal to 1:3 according to volume ratio；
B) being placed in reflux by mixed solution described in thin-layer graphene oxide and step a, in container, pressure is not less than-0.1MPa；
C) reacting in 60 DEG C ~ 80 DEG C oil bath environment, the response time is no less than 24h again.
2. the method wanting redox graphene described in 2 according to right, it is characterised in that the volume ratio of described N, N-dimethyl-benzyl amine and hydrazine hydrate is 1:4.
The method of redox graphene the most according to claim 2, it is characterised in that described reaction pressure is-0.1MPa.
The method of redox graphene the most according to claim 2, it is characterised in that described reaction temperature is 60 DEG C.
The method of redox graphene the most according to claim 2, it is characterised in that the described response time is 24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610336253.5A CN105776199A (en) | 2016-05-20 | 2016-05-20 | Method for reducing graphene oxide |
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| CN201610336253.5A CN105776199A (en) | 2016-05-20 | 2016-05-20 | Method for reducing graphene oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243379A (en) * | 2016-07-23 | 2016-12-21 | 天津大学 | A kind of electromagnetic shielding foamed composite based on graphene oxide and polymer and preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633256A (en) * | 2012-04-16 | 2012-08-15 | 中国科学院上海硅酸盐研究所 | Preparation method of graphene colloid dispersion solution |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN103880000A (en) * | 2014-03-07 | 2014-06-25 | 中南大学 | Preparation method of ultralight graphene powder |
| CN104098087A (en) * | 2014-06-17 | 2014-10-15 | 华南理工大学 | Method for reduction of graphene oxide by metal/tea polyphenol as reducing agent |
| CN104617300A (en) * | 2015-02-09 | 2015-05-13 | 天津师范大学 | Method for preparing lithium ion battery anode/cathode material from reduced graphene oxide |
-
2016
- 2016-05-20 CN CN201610336253.5A patent/CN105776199A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633256A (en) * | 2012-04-16 | 2012-08-15 | 中国科学院上海硅酸盐研究所 | Preparation method of graphene colloid dispersion solution |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN103880000A (en) * | 2014-03-07 | 2014-06-25 | 中南大学 | Preparation method of ultralight graphene powder |
| CN104098087A (en) * | 2014-06-17 | 2014-10-15 | 华南理工大学 | Method for reduction of graphene oxide by metal/tea polyphenol as reducing agent |
| CN104617300A (en) * | 2015-02-09 | 2015-05-13 | 天津师范大学 | Method for preparing lithium ion battery anode/cathode material from reduced graphene oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243379A (en) * | 2016-07-23 | 2016-12-21 | 天津大学 | A kind of electromagnetic shielding foamed composite based on graphene oxide and polymer and preparation method |
| CN106243379B (en) * | 2016-07-23 | 2019-10-18 | 天津大学 | A kind of electromagnetic shielding foamed composite and preparation method based on graphene oxide and polymer |
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Application publication date: 20160720 |