CN108455581A - Prepare the green synthesis method of graphene and graphene quantum dot simultaneously using starch - Google Patents
Prepare the green synthesis method of graphene and graphene quantum dot simultaneously using starch Download PDFInfo
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- CN108455581A CN108455581A CN201810301046.5A CN201810301046A CN108455581A CN 108455581 A CN108455581 A CN 108455581A CN 201810301046 A CN201810301046 A CN 201810301046A CN 108455581 A CN108455581 A CN 108455581A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of green synthesis methods preparing graphene and graphene quantum dot simultaneously using starch.Deionized water, soluble starch is specifically added using deionized water as green solvent as carbon source using starch in the preparation of the graphene and graphene quantum dot in the container with agitating device, and 10 30min of stirring are allowed to be completely dissolved；Water heating kettle reactor is added in solution obtained above, is gradually heating to 120 250 DEG C, keeps pressure within 8Mpa, carries out hydro-thermal reaction, is discharged after reacting 1 15h；Obtained dark brown material is centrifuged in centrifuge with the speed of 3000 15000r/min, bottom precipitates for dark brown, obtains graphene after drying, upper layer is light yellow transparent liquid, as the aqueous solution of graphene quantum dot.Uniform using the graphene grain size prepared by this method, obtained graphene quantum dot can be preferably dissolved in water, and grain size is uniform, and have good fluorescence property.
Description
Technical field
The present invention relates to a kind of methods preparing graphene and graphene quantum dot of field of nanometer material technology, more specifically refer to one
Kind prepares the green method of graphene and graphene quantum dot using starch simultaneously, and obtained graphene size uniform obtains
Graphene quantum dot have good water solubility, grain size is uniform, while having good fluorescence property.
Background technology
2004, British scientist was prepared by carbon atom with sp for the first time2The monoatomic layer of hydridization connection constitutes new
Type two-dimensional atomic crystal-graphene, thickness only have 0.3354 nm, are to find most thin material in the world at present.System at present
The conventional method of standby graphene predominantly aoxidizes patterning method, needs using strong oxidizers such as sulfuric acid or nitric acid to various carbon materials
（Graphite, carbon fiber, carbon nanotube）Oxidation cutting is carried out, is had a certain impact to environment.Moreover, after oxidation reaction, it is right
The subsequent processes of product are complicated.Therefore, it finds a kind of environmental-friendly and to be more suitable for industrialized method is that mesh is previous urgently
Problem to be solved.
On the other hand, due to the planar conjugate structure of graphene super large, the pi-electron in graphene is imitated with significant delocalization
It answers.Therefore, the graphene film of larger two-dimensional has the semi-metallic characteristic of zero band gap, and which has limited graphenes in photoelectricity
The application in the fields such as device and semiconductor.Graphene band gap is opened, it is transformed into semi-conducting material from semi-metallic, is caused
The common concern of people.Currently, there are mainly two types of the methods of opening graphene band gap, one is carry out chemistry to graphene to mix
It is miscellaneous to destroy its pi-electron conjugated system.Another be based on quantum effect, by graphene cut into nanobelt, nanometer sieve or
Quantum dot（GQDs）.Graphene quantum dot（GQDs）It is the graphene film that two-dimentional lateral dimensions is less than 100 nm, because quantum limits
Domain effect and boundary effect and show special physicochemical properties, be a kind of semi-conducting material with band gap.Compared to
Conventional semiconductors quantum dot, GQDs toxicity is low, good water solubility, chemism is low and photoluminescent property is stablized.In addition, GQDs has
Monoatomic layer planar conjugate structure and larger specific surface area, surface, which is easy to cover, carries large biological molecule, and the oxygen-containing group on its surface
Group provides active site for the combination of foreign molecules and GQDs, in necks such as solar cell, opto-electronic device, biological medicines
Domain is with a wide range of applications.
The preparation method of GQDs is broadly divided into two methods from top to bottom and from bottom to top.Method includes mainly from top to bottom
Strong acid oxidizing process, the hot method of hydrothermal/solvent, electrochemical oxidation process etc..Self-absorption Correction Factor includes mainly that controlledly synthesis and carbonization are anti-
It answers.Complicated for the various GQDs preparation methods common problems reported at present, such as preparation process, reaction condition is severe
It carves, the present invention, as raw material, using deionized water as solvent, the second best in quality stone is prepared using green method using starch
Black alkene and GQDs.Other preparation methods are compared to, the reaction system of this method is green safe, and reaction condition is mild, reaction speed
Rate is very fast, and product postprocessing process is simple, and prepared by the magnanimity that can be realized simultaneously graphene and the simple green of GQDs, have
Important application value and application prospect.
Invention content
It is an object of the invention to solve current graphene and GQDs preparation method common problems, made using starch
For raw material, while the uniform graphene of grain size and GQDs are prepared, the reaction system of this method is green safe, reaction condition
Mildly, reaction rate is very fast, and product postprocessing process is simple, can be realized simultaneously the macro of the simple green of graphene and GQDs
Prepared by amount, have important application value and application prospect.Its technical solution is as follows：
（1）The deionized water of certain mass is added in the container with agitating device, is added further according to above-mentioned ratio range
Suitable starch does not heat or is heated to 40-70 DEG C, is dispersed with stirring 10-30min, until being completely dissolved or being uniformly dispersed；
（2）By（1）Water heating kettle is added in the solution or suspension obtained in step, is gradually heating to 120-250 DEG C, and pressure is kept to exist
Within 8Mpa, hydro-thermal reaction is carried out, is discharged after reacting 1-15h；
（3）By（2）It walks obtained dark brown material and centrifugation point is carried out with the speed of 3000-15000r/min in centrifuge
From, dark brown precipitation is isolated, graphene is obtained later by drying, the isolated light yellow transparent liquid in upper layer, as
The aqueous solution of graphene quantum dot.
A kind of green method preparing graphene and graphene quantum dot simultaneously using starch, using starch conduct
Carbon source, deionized water is as solvent, and preparation process is simple and does not add any chemical reagents, environmentally protective, without any environment
Pollution.
A kind of green method preparing graphene and graphene quantum dot simultaneously using starch, deionized water and shallow lake
The mass ratio of powder ranging from 50 ~ 200：1 ~ 10, preferred value is 80 ~ 150：2~5.
A kind of green method preparing graphene and graphene quantum dot simultaneously using starch, starch are that straight chain forms sediment
Powder can also be all kinds of plants containing starch, including：Corn, cassava, sweet potato, potato etc., but it is not limited only to this.
Compared with prior art, the present invention its advantage is：The present invention uses starch as raw material, using deionized water conduct
Solvent prepares graphene and GQDs using green method.Obtained graphene and GQDs grain sizes are uniform, and GQDs
With good water-soluble and fluorescence property.It is compared to other GQDs preparation methods, the reaction system green peace of this method
Entirely, reaction condition is mild, and reaction rate is very fast, and product postprocessing process is simple, and the simple green of graphene and GQDs may be implemented
Prepared by the magnanimity of color, have important application value and application prospect.
Description of the drawings
Fig. 1 is the XRD spectra of the graphene quantum dot prepared by embodiment 1.
Fig. 2 is the XRD spectra of the graphene prepared by embodiment 1.
Fig. 3 is the fluorescence photos of GQDs in the UV lamp prepared by embodiment 1.
Fig. 4 is the fluorescence spectrum of the GQDs prepared by embodiment 1-3.
Fig. 5 is the SEM photograph of the graphene prepared by embodiment 1.
Fig. 6 is the SEM photograph of the graphene quantum dot prepared by embodiment 1.
Specific implementation mode
Embodiment 1
1kg deionized waters are added in the container with agitating device, add 20g soluble starches, are heated to 40 DEG C, stirring
10min is to being completely dissolved；Water heating kettle is added in the aqueous solution of starch, is gradually heating to 150 DEG C, keeps pressure within 6Mpa,
Hydro-thermal reaction is carried out, is discharged after reacting 15h；By obtained dark brown material in centrifuge with the speed of 5000r/min into
Row centrifuges, and isolates dark brown precipitation, and freeze-drying obtains graphene powder, the isolated pale yellow transparent liquid in upper layer
Body, the as aqueous solution of graphene quantum dot.
Embodiment 2
1kg deionized waters are added in the container with agitating device, add 5g corn flour, are heated to 60 DEG C, stir 30min
To being uniformly dispersed；Water heating kettle is added in suspension containing corn flour, is gradually heating to 160 DEG C, keeps pressure within 6Mpa,
Hydro-thermal reaction is carried out, is discharged after reacting 10h；By obtained dark brown material in centrifuge with the speed of 10000r/min into
Row centrifuges, and isolates dark brown precipitation, is freeze-dried and obtains graphene, the isolated light yellow transparent liquid in upper layer,
The as aqueous solution of graphene quantum dot.The XRD spectra of graphene quantum dot and the XRD spectra of graphene are the same as 1 collection of illustrative plates of embodiment.
Embodiment 3
1kg deionized waters are added in the container with agitating device, add 10g tapioca starch, are heated to 50 DEG C, stirring
25min is to being uniformly dispersed；Water heating kettle is added in suspension containing tapioca starch, is gradually heating to 170 DEG C, keeps pressure in 6Mpa
Within, hydro-thermal reaction is carried out, is discharged after reacting 12h；By obtained dark brown material with the speed of 9000r/min in centrifuge
Degree is centrifuged, and isolates dark brown precipitation, and freeze-drying obtains graphene powder, isolated faint yellow in upper layer
Prescribed liquid, the as aqueous solution of graphene quantum dot.The XRD spectra of graphene quantum dot and the XRD spectra of graphene are the same as implementation
1 collection of illustrative plates of example.
Claims (4)
1. a kind of green synthesis method preparing graphene and graphene quantum dot simultaneously using starch, which is characterized in that including
Following steps：
（1）Deionized water is added in the container with agitating device, adds soluble starch, room temperature or is heated to 40-
80 DEG C, it is dispersed with stirring 10-30min, until being completely dissolved；
（2）By step（1）In obtained solution water heating kettle is added, keep pressure within 8Mpa, be warming up to 120-250 DEG C, water
It discharges after thermal response 1-15h, obtains dark brown material；
（3）By step（2）In obtained dark brown material centrifugation point is carried out with the speed of 3000-15000r/min in centrifuge
From, isolate dark brown precipitation, by freeze-drying after obtain graphene powder, the upper layer pale yellow transparent liquid isolated
Body, the as aqueous solution of graphene quantum dot.
2. the method described in claim 1 for preparing graphene quantum dot using starch, which is characterized in that deionized water and starch
Mass ratio ranging from 50 ~ 200：1~10.
3. the method described in claim 1 for preparing graphene quantum dot using starch, which is characterized in that deionized water and starch
Mass ratio ranging from 80 ~ 150：2~5.
4. the method described in claim 1 for preparing graphene quantum dot using starch, which is characterized in that starch is soluble shallow lake
Powder or all kinds of plants containing starch, including corn, cassava, sweet potato, potato.
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| CN201810301046.5A CN108455581A (en) | 2018-04-04 | 2018-04-04 | Prepare the green synthesis method of graphene and graphene quantum dot simultaneously using starch |
| CN201811115740.4A CN108892130A (en) | 2018-04-04 | 2018-09-25 | The green synthesis method of graphene quantum dot is prepared using starch |
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Cited By (10)
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| CN109401635A (en) * | 2018-09-21 | 2019-03-01 | 三峡大学 | Graphene Aqueous Adhesives and preparation method thereof |
| CN109592672A (en) * | 2019-01-28 | 2019-04-09 | 三峡大学 | A method of graphene quantum dot is prepared using barley |
| CN109701527A (en) * | 2019-01-28 | 2019-05-03 | 三峡大学 | The preparation method and applications of the stable gold nano grain of graphene quantum dot |
| CN109824035A (en) * | 2019-03-15 | 2019-05-31 | 三峡大学 | A kind of method that cellulose prepares graphene quantum dot |
| CN110052267A (en) * | 2019-05-07 | 2019-07-26 | 三峡大学 | The preparation method and applications of the stable silver of graphene quantum dot and/or rhodium nanoparticles |
| CN110129044A (en) * | 2019-05-20 | 2019-08-16 | 哈尔滨工业大学 | It is a kind of using biomass as the graphene quantum dot preparation method and applications of carbon source |
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| CN111117607A (en) * | 2019-12-03 | 2020-05-08 | 上海理工大学 | Preparation method and application of graphene quantum dots with blue fluorescence characteristics |
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- 2018-09-25 CN CN201811115740.4A patent/CN108892130A/en active Pending
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| CN109401635A (en) * | 2018-09-21 | 2019-03-01 | 三峡大学 | Graphene Aqueous Adhesives and preparation method thereof |
| CN109592672A (en) * | 2019-01-28 | 2019-04-09 | 三峡大学 | A method of graphene quantum dot is prepared using barley |
| CN109701527A (en) * | 2019-01-28 | 2019-05-03 | 三峡大学 | The preparation method and applications of the stable gold nano grain of graphene quantum dot |
| CN109824035A (en) * | 2019-03-15 | 2019-05-31 | 三峡大学 | A kind of method that cellulose prepares graphene quantum dot |
| CN110052267A (en) * | 2019-05-07 | 2019-07-26 | 三峡大学 | The preparation method and applications of the stable silver of graphene quantum dot and/or rhodium nanoparticles |
| CN110129032A (en) * | 2019-05-16 | 2019-08-16 | 闽江学院 | A kind of Fluorescence Identification method of ferritin |
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| CN110129044B (en) * | 2019-05-20 | 2022-04-15 | 哈尔滨工业大学 | Preparation method and application of graphene quantum dots with biomass as carbon source |
| CN110182790A (en) * | 2019-06-17 | 2019-08-30 | 三峡大学 | The method of glucan synthesizing graphite alkene quantum dot |
| CN110194447A (en) * | 2019-06-17 | 2019-09-03 | 三峡大学 | Use DNA for the method for precursor synthesis graphene quantum dot |
| CN111117607A (en) * | 2019-12-03 | 2020-05-08 | 上海理工大学 | Preparation method and application of graphene quantum dots with blue fluorescence characteristics |
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| CN108892130A (en) | 2018-11-27 |
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Application publication date: 20180828 |