CN110451497A - A kind of method of quick free from admixture redox graphene - Google Patents
A kind of method of quick free from admixture redox graphene Download PDFInfo
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- CN110451497A CN110451497A CN201910789873.8A CN201910789873A CN110451497A CN 110451497 A CN110451497 A CN 110451497A CN 201910789873 A CN201910789873 A CN 201910789873A CN 110451497 A CN110451497 A CN 110451497A
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- admixture
- graphene oxide
- vacuum drying
- drying oven
- redox graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The invention discloses a kind of methods of quick free from admixture redox graphene, comprise the following steps: Step 1: graphene oxide is placed in vacuum drying oven, vacuumizing under normal temperature environment to baking oven；Step 2: setting vacuum drying oven temperature is 150~300 DEG C, graphene oxide is heated；Step 3: oven temperature keeps 0.5~5h, keep graphene oxide sufficiently heated；Step 4: stopping heating, it is cooled to room temperature to oven temperature, opens vacuum valve and collects powder, obtains redox graphene.
Description
Technical field
The present invention relates to the relevant technical fields of graphene, provide the oxygen reduction of quick one kind, low energy consumption and free from admixture
The method of graphite alkene.
Background technique
Graphene has an excellent mechanics, electricity, the performances such as optically and thermally, extensive in research in recent years
It has been applied to the fields such as material, electronics, chemistry, the energy and biological medicine.The common preparation method of graphene have mechanical stripping method,
Chemical vapour deposition technique, solid phase epitaxial growth and chemistry redox method etc..The preparation-obtained graphene of first three methods
With relatively complete structure, but preparation process is complicated and expensive；Although the graphene film that chemistry redox method obtains
Layer has fewer defects, but its low production cost also can be realized continuous, the large-scale production of factory, in actual application
In, the resulting graphene of chemistry redox method also shows better compatibility and stability.In process of production, stone is aoxidized
The preparation of black alkene generally passes through the methods of Hummers progress, but the reduction of a graphene oxide really more scabrous problem.
Currently, common and most study is to be restored by sodium borohydride to graphene oxide, although existing a large amount of research gram
The disadvantages of energy consumption in the reduction process is high, time-consuming is taken, but because of the use of the reagents such as sodium borohydride, meeting in the reduction process
A large amount of impurity are introduced, to reduce the quality of obtained graphene, application subsequent to graphene also produces many limits
System.
Summary of the invention
In order to overcome the shortcomings of the prior art, the main purpose of invention is to provide a kind of quick free from admixture oxygen reduction
The method of graphite alkene.
To realize above method purpose, the invention provides the following technical scheme: a kind of quick free from admixture reduction-oxidation graphite
The method of alkene, comprises the following steps:
Step 1: graphene oxide is placed in vacuum drying oven, baking oven is vacuumized under normal temperature environment；
Step 2: setting vacuum drying oven temperature is 150~300 DEG C, graphene oxide is heated；
Step 3: oven temperature keeps 0.5~5h, keep graphene oxide sufficiently heated；
Step 4: stopping heating, it is cooled to room temperature to oven temperature, opens vacuum valve and collects powder, obtains oxygen reduction
Graphite alkene.
Further, graphene oxide described in step 1 is to pass through Brodie method, Staudenmaier method or Hummers
The graphene oxide powder that method is prepared, or by dry through Brodie method, Staudenmaier method or Hummers method
The obtained obtained graphene oxide powder of graphene oxide slurries.
Further, the pressure of vacuum drying oven described in step 1 is 200~20000Pa.
Further, the pressure of vacuum drying oven described in step 1 is 5000~20000Pa.
Further, the pressure of vacuum drying oven described in step 1 is 10000Pa.
Further, the heating rate of vacuum drying oven is (1~10) DEG C/min in step 2.
Further, oven temperature keeps 0.5~2h in step 3.
Further, oven temperature keeps 1h in step 3.
Further, it is 250 DEG C that vacuum drying oven temperature is arranged in step 2, and heating rate is 10 DEG C/min.
The present invention also provides the nothings being prepared according to a kind of method of quick free from admixture redox graphene
Impurity redox graphene.
A kind of method of quick free from admixture redox graphene, the beneficial effect is that:
1, the implementation temperature of the method for the present invention is lower, and the processing time is shorter, is a kind of low energy consumption, quick reduction-oxidation graphite
The method of alkene；
2, the method for the present invention does not need addition any chemical reagents in implementation process, and can be effectively removed oxygen
The impurity such as remaining sulfuric acid, water in graphite alkene, and implementation process of the present invention is the process of an anhydrous and oxygen-free, it will not be to gained
Graphene carry out secondary oxidation, obtained redox graphene purity is higher, performance is more stable；
3, to be applicable in graphene oxide, there is no limit by any raw material, any preparation method, appoint the method for the present invention
The graphene oxide slurries or graphene oxide powder of what concentration, any diameter, can be restored by the method for the invention
Processing, the method for the present invention have wide applicability；
4, the method for the present invention mild condition, obtained redox graphene defect is less, and graphene sheet layer is not easy to roll into a ball
It is poly-, there is higher specific surface area and better electric conductivity.
Detailed description of the invention
Fig. 1 is the electron micrograph of the untreated graphene oxide of control group；From fig. 1, it can be seen that untreated
Graphene oxide shows serious agglomeration；
Fig. 2 is the electron micrograph of the graphene oxide after embodiment 1 is processed by the invention；As can be seen from Figure 2, through this
Graphene oxide layer after invention reduction is unfolded, and does not occur agglomeration.
Specific embodiment
Control group embodiment
One, 5g graphene oxide is placed in vacuum drying oven, baking oven internal pressure is evacuated to baking oven under normal temperature environment
By force to 5000Pa；
Two, vacuum drying oven temperature is set and heating rate is respectively 25 DEG C and 0 DEG C/min, graphene oxide is added
Heat；
Three, oven temperature keeps 2h, keeps graphene oxide sufficiently heated；
Four, stop heating, be cooled to room temperature to oven temperature, open vacuum valve and collect powder, obtain oxygen reduction fossil
Black alkene.
Embodiment 1
The method of quick free from admixture redox graphene, comprises the following steps:
One, 5g graphene oxide is placed in vacuum drying oven, baking oven internal pressure is evacuated to baking oven under normal temperature environment
By force to 5000Pa；
Two, vacuum drying oven temperature is set and heating rate is respectively 200 DEG C and 10 DEG C/min, graphene oxide is added
Heat；
Three, oven temperature keeps 2h, keeps graphene oxide sufficiently heated；
Four, stop heating, be cooled to room temperature to oven temperature, open vacuum valve and collect powder, obtain oxygen reduction fossil
Black alkene.
Embodiment 2
The method of quick free from admixture redox graphene, comprises the following steps:
One, 5g graphene oxide is placed in vacuum drying oven, baking oven internal pressure is evacuated to baking oven under normal temperature environment
By force to 10000Pa；
Two, vacuum drying oven temperature is set and heating rate is respectively 250 DEG C and 10 DEG C/min, graphene oxide is added
Heat；
Three, oven temperature keeps 1h, keeps graphene oxide sufficiently heated；
Four, stop heating, be cooled to room temperature to oven temperature, open vacuum valve and collect powder, obtain oxygen reduction fossil
Black alkene.
Embodiment 3
The method of quick free from admixture redox graphene, comprises the following steps:
One, 5g graphene oxide is placed in vacuum drying oven, baking oven internal pressure is evacuated to baking oven under normal temperature environment
By force to 5000Pa；
Two, vacuum drying oven temperature is set and heating rate is respectively 250 DEG C and 10 DEG C/min, graphene oxide is added
Heat；
Three, oven temperature keeps 0.5h, keeps graphene oxide sufficiently heated；
Four, stop heating, be cooled to room temperature to oven temperature, open vacuum valve and collect powder, obtain oxygen reduction fossil
Black alkene.
Table 1 is the result that the verifying present invention implements front and back graphene oxide composition transfer.
Table 1
As known from Table 1, the data of the data of the control group measured and the Examples 1 to 3 measured are compared, can be obtained
The present invention significantly redox graphene and can completely remove wherein remaining sulfuric acid impurity out, and be not introduced into
Other impurities.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method of quick free from admixture redox graphene, it is characterised in that: comprise the following steps:
Step 1: graphene oxide is placed in vacuum drying oven, baking oven is vacuumized under normal temperature environment；
Step 2: setting vacuum drying oven temperature is 150~300 DEG C, graphene oxide is heated；
Step 3: oven temperature keeps 0.5~5h, keep graphene oxide sufficiently heated；
Step 4: stopping heating, it is cooled to room temperature to oven temperature, opens vacuum valve and collects powder, obtains oxygen reduction fossil
Black alkene.
2. a kind of method of quick free from admixture redox graphene according to claim 1, it is characterised in that: step 1
Described in graphene oxide be the graphene oxide being prepared by Brodie method, Staudenmaier method or Hummers method
Powder, or pass through the dry graphene oxide slurries institute obtained through Brodie method, Staudenmaier method or Hummers method
Obtained graphene oxide powder.
3. a kind of method of quick free from admixture redox graphene according to claim 1, it is characterised in that: step 1
The pressure of the vacuum drying oven is 200~20000Pa.
4. a kind of method of quick free from admixture redox graphene according to claim 3, it is characterised in that: step 1
The pressure of the vacuum drying oven is 5000~20000Pa.
5. a kind of method of quick free from admixture redox graphene according to claim 4, it is characterised in that: step 1
The pressure of the vacuum drying oven is 10000Pa.
6. a kind of method of quick free from admixture redox graphene according to claim 1, it is characterised in that: step 2
The heating rate of middle vacuum drying oven is (1~10) DEG C/min.
7. a kind of method of quick free from admixture redox graphene according to claim 1, it is characterised in that: step 3
Middle oven temperature keeps 0.5~2h.
8. a kind of method of quick free from admixture redox graphene according to claim 7, it is characterised in that: step 3
Middle oven temperature keeps 1h.
9. a kind of method of quick free from admixture redox graphene according to claim 1, it is characterised in that: step 2
Middle setting vacuum drying oven temperature is 250 DEG C, and heating rate is 10 DEG C/min.
10. a kind of method of -9 any quick free from admixture redox graphenes is prepared according to claim 1
Free from admixture redox graphene.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006613A (en) * | 2016-05-24 | 2016-10-12 | 广州市霆宇能源科技有限责任公司 | Method for preparing graphene |
| CN109534318A (en) * | 2018-11-29 | 2019-03-29 | 北京圣盟科技有限公司 | A kind of graphene preparation method in battery |
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- 2019-08-26 CN CN201910789873.8A patent/CN110451497A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006613A (en) * | 2016-05-24 | 2016-10-12 | 广州市霆宇能源科技有限责任公司 | Method for preparing graphene |
| CN109534318A (en) * | 2018-11-29 | 2019-03-29 | 北京圣盟科技有限公司 | A kind of graphene preparation method in battery |
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Application publication date: 20191115 |
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