CN107892292A - A kind of method that microwave solid source quickly prepares nitrogen-doped graphene - Google Patents
A kind of method that microwave solid source quickly prepares nitrogen-doped graphene Download PDFInfo
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- CN107892292A CN107892292A CN201711140129.2A CN201711140129A CN107892292A CN 107892292 A CN107892292 A CN 107892292A CN 201711140129 A CN201711140129 A CN 201711140129A CN 107892292 A CN107892292 A CN 107892292A
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- nitrogen
- graphene
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- doped graphene
- graphite oxide
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Abstract
The present invention relates to inorganic chemistry applied technical field, and in particular to a kind of method for rapidly and efficiently preparing nitrogen-doped graphene as the solid phase microwave radiation technology of nitrogen source using ethylenediamine.A kind of method that microwave solid source quickly prepares nitrogen-doped graphene, using following steps：Step 1：The preparation of graphite oxide is completed by low temperature, medium temperature and high temperature three phases；Step 2：The preparation of nitrogen-doped graphene：Functionalization graphene is first made, back flow reaction is then carried out to it and the preparation of nitrogen-doped graphene is completed in microwave heating.The present invention carries out functionalization to graphite oxide using ethylenediamine, and the N doping to graphene is successfully realized by the process of solid phase microwave treatment ethylenediamine functionalization graphene.Relative to traditional N doping method, this method avoid highly corrosive and highly toxic ammonia is used, the characteristics of environment-friendly is shown.In addition, this method also has the features such as efficient and highly doped amount concurrently.
Description
Technical field
The present invention relates to inorganic chemistry applied technical field, and in particular to a kind of micro- as the solid phase of nitrogen source using ethylenediamine
The method that ripple auxiliary rapidly and efficiently prepares nitrogen-doped graphene.
Background technology
Nitrogen-doped graphene is prepared mainly by two approach such as directly synthesizing and post-processing.Directly synthesis refers to changing
Nitrogen source is passed through when learning vapour deposition synthesizing graphite alkene makes nitrogen-atoms doping in situ during graphene growth enter its lattice；
And it is then to be handled at high temperature using nitrogen-containing molecules graphene to post-process, nitrogen atom doping is set to enter the crystalline substance of graphene
In lattice.At present, it is that raw material prepares graphene on a large scale that researcher, which has been realized using graphite oxide, therefore post-processes the approach of nitrating
With more the potentiality of practical application.In order to realize the efficient N doping to graphene, there is the NH of higher level of reactivity3Often it is selected as
Nitrogen source.But ammonia is poisonous and has strong corrosivity, very high requirement is proposed to equipment and is unfavorable for realizing on a large scale
Preparation.
The content of the invention
The present invention is directed to propose a kind of rapidly and efficiently prepare N doping using solid phase microwave radiation technology of the ethylenediamine as nitrogen source
The method of graphene.
Technical program of the present invention lies in：
A kind of method that microwave solid source quickly prepares nitrogen-doped graphene, using following steps：
Step 1：The preparation of graphite oxide：
（1）The low-temp reaction stage：The 130mL concentrated sulfuric acids and 5g crystalline flake graphites are added in 1000mL beaker, and in condition of ice bath
Lower mechanical agitation 2h；15g potassium permanganate is slowly added into above-mentioned system, and maintains and continues to stir 2h under condition of ice bath, this
One stage was the low-temp reaction stage；
（2）The medium temperature stage of reaction：Ice bath is removed, continues to stir lh under 35 DEG C of water-baths；
（3）The pyroreaction stage：230mL deionized waters are added dropwise into beaker, and is warming up to 980 DEG C and continues to react 30min；
（4）Pyroreaction adds 400mL deionized waters thereto after terminating, and centrifuge washing to neutrality obtains graphite oxide and disperseed
Liquid；
Step 2：The preparation of nitrogen-doped graphene：
（1）The graphite oxide dispersion of above-mentioned preparation is diluted to 1 mgmL-1Concentration, measure the 120mL dispersion liquids simultaneously
The h of back flow reaction 6 at 95 DEG C is added to 250mL single-necked flasks with 1.5mL ethylenediamines；
（2）Solid phase FGS is obtained by freeze-drying after the completion of reaction（Functionalization graphene)；
（3）Resulting FGS is placed in micro-wave oven and obtains N doping stone after full power microwave treatment l min under an ar atmosphere
Black alkene.
The technical effects of the invention are that：
The present invention carries out functionalization using ethylenediamine to graphite oxide, and passes through solid phase microwave treatment ethylenediamine functionalization graphene
Process successfully realize N doping to graphene.Relative to traditional N doping method, this method avoid use high corrosion
Property and highly toxic ammonia, show the characteristics of environment-friendly.In addition, this method also has efficient and highly doped amount etc. concurrently
Feature.
Embodiment
A kind of method that microwave solid source quickly prepares nitrogen-doped graphene, using following steps：
Step 1：The preparation of graphite oxide：
（1）The low-temp reaction stage：The 130mL concentrated sulfuric acids and 5g crystalline flake graphites are added in 1000mL beaker, and in condition of ice bath
Lower mechanical agitation 2h；15g potassium permanganate is slowly added into above-mentioned system, and maintains and continues to stir 2h under condition of ice bath, this
One stage was the low-temp reaction stage；
（2）The medium temperature stage of reaction：Ice bath is removed, continues to stir lh under 35 DEG C of water-baths；
（3）The pyroreaction stage：230mL deionized waters are added dropwise into beaker, and is warming up to 980 DEG C and continues to react 30min；
（4）Pyroreaction adds 400mL deionized waters thereto after terminating, and centrifuge washing to neutrality obtains graphite oxide and disperseed
Liquid；
Step 2：The preparation of nitrogen-doped graphene：
（1）The graphite oxide dispersion of above-mentioned preparation is diluted to 1 mgmL-1Concentration, measure the 120mL dispersion liquids simultaneously
The h of back flow reaction 6 at 95 DEG C is added to 250mL single-necked flasks with 1.5mL ethylenediamines；
（2）Solid phase FGS is obtained by freeze-drying after the completion of reaction（Functionalization graphene)；
（3）Resulting FGS is placed in micro-wave oven and obtains N doping stone after full power microwave treatment l min under an ar atmosphere
Black alkene.
Claims (1)
1. a kind of method that microwave solid source quickly prepares nitrogen-doped graphene, it is characterised in that：Using following steps：
Step 1：The preparation of graphite oxide：
（1）The low-temp reaction stage：The 130mL concentrated sulfuric acids and 5g crystalline flake graphites are added in 1000mL beaker, and in condition of ice bath
Lower mechanical agitation 2h；15g potassium permanganate is slowly added into above-mentioned system, and maintains and continues to stir 2h under condition of ice bath, this
One stage was the low-temp reaction stage；
（2）The medium temperature stage of reaction：Ice bath is removed, continues to stir lh under 35 DEG C of water-baths；
（3）The pyroreaction stage：230mL deionized waters are added dropwise into beaker, and is warming up to 980 DEG C and continues to react 30min；
（4）Pyroreaction adds 400mL deionized waters thereto after terminating, and centrifuge washing to neutrality obtains graphite oxide and disperseed
Liquid；
Step 2：The preparation of nitrogen-doped graphene：
（1）The graphite oxide dispersion of above-mentioned preparation is diluted to 1 mgmL-1Concentration, measure the 120mL dispersion liquids and with
1.5mL ethylenediamines add to 250mL single-necked flasks the h of back flow reaction 6 at 95 DEG C；
（2）Solid phase FGS is obtained by freeze-drying after the completion of reaction（Functionalization graphene)；
（3）Resulting FGS is placed in micro-wave oven and obtains N doping stone after full power microwave treatment l min under an ar atmosphere
Black alkene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711140129.2A CN107892292A (en) | 2017-11-16 | 2017-11-16 | A kind of method that microwave solid source quickly prepares nitrogen-doped graphene |
Applications Claiming Priority (1)
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| CN201711140129.2A CN107892292A (en) | 2017-11-16 | 2017-11-16 | A kind of method that microwave solid source quickly prepares nitrogen-doped graphene |
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| CN107892292A true CN107892292A (en) | 2018-04-10 |
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| CN201711140129.2A Withdrawn CN107892292A (en) | 2017-11-16 | 2017-11-16 | A kind of method that microwave solid source quickly prepares nitrogen-doped graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099578A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped three-dimensional graphene material |
| CN111591981A (en) * | 2020-04-21 | 2020-08-28 | 东北大学 | Preparation method of low-layer gauze-shaped nitrogen-doped graphene |
-
2017
- 2017-11-16 CN CN201711140129.2A patent/CN107892292A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099578A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped three-dimensional graphene material |
| CN111591981A (en) * | 2020-04-21 | 2020-08-28 | 东北大学 | Preparation method of low-layer gauze-shaped nitrogen-doped graphene |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180410 |
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| WW01 | Invention patent application withdrawn after publication |