CN109626363A - The method for preparing graphene quantum dot using maltose - Google Patents
The method for preparing graphene quantum dot using maltose Download PDFInfo
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- CN109626363A CN109626363A CN201910082011.1A CN201910082011A CN109626363A CN 109626363 A CN109626363 A CN 109626363A CN 201910082011 A CN201910082011 A CN 201910082011A CN 109626363 A CN109626363 A CN 109626363A
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- maltose
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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
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
Abstract
The invention discloses a kind of methods for preparing graphene quantum dot using maltose.Using maltose as carbon source, deionized water is prepared for solvent.Specifically the preparation method comprises the following steps: the deionized water of certain mass is added in (1) in the container with agitating device, the maltose of certain mass is added, stirring 10-30min is allowed to be completely dissolved；(2) water heating kettle reactor is added in lysate obtained above, is gradually heated to 150-250 DEG C, keep pressure within 10Mpa, carry out hydro-thermal reaction, discharged after reacting 2-15h；(3) the dark brown material that (2) step obtains is centrifuged in centrifuge with the speed of 6000-12000r/min, bottom is dark brown precipitating, and upper layer is light yellow transparent liquid, which is the aqueous solution of graphene quantum dot.It is uniform using graphene quantum dot particle size prepared by this method, it can preferably be dissolved in water, and there is good fluorescence property, and preparation process is simple, product separation is easy, and environmentally protective, to environment without any pollution.
Description
Technical field
The present invention relates to a kind of methods for preparing graphene quantum dot of field of nanometer material technology, more specifically refer to a kind of using wheat
Bud sugar prepares the green method of graphene quantum dot, and obtained graphene is of uniform size, and obtained graphene quantum dot has
Good water solubility, particle size is uniform, while having good fluorescence property.
Background technique
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) carries out oxidation cutting, has 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 semiconductor material from semi-metallic, is caused
The common concern of people.Currently, one is carry out chemistry to graphene to mix there are mainly two types of the methods of opening graphene band gap
It is miscellaneous to destroy its pi-electron conjugated system.Another be based on quantum effect, by graphene be cut into nanobelt, nanometer sieve or
Quantum dot (GQDs).Graphene quantum dot (GQDs) is graphene film of the two-dimentional lateral dimensions less than 100 nm, because quantum limits
Domain effect and boundary effect and show special physicochemical properties, be a kind of semiconductor material with band gap.Compared to
Conventional semiconductors quantum dot, GQDs toxicity is low, good water solubility, chemical activity is low and photoluminescent property is stablized.In addition, GQDs has
Monoatomic layer planar conjugate structure and biggish 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, leads in solar battery, opto-electronic device, biological medicine etc.
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 mainly includes from top to bottom
Strong acid oxidizing process, hydrothermal/solvent thermal method, electrochemical oxidation process etc..Self-absorption Correction Factor mainly includes that controlledly synthesis and carbonization are anti-
It answers.Complicated for the various GQDs preparation method common problems reported at present, such as preparation process, reaction condition is severe
It carves, the present invention is prepared the second best in quality as raw material using maltose using deionized water as solvent using green method
GQDs.Other preparation methods are compared to, the reaction system of this method is green safe, and reaction condition is mild, and reaction rate is very fast,
Product postprocessing process is simple, the magnanimity preparation of the simple green of GQDs may be implemented, before having important application value and application
Scape.
Summary of the invention
It is an object of the invention to solve current GQDs preparation method common problem, using maltose as former
Material, prepare the uniform GQDs of particle size, the reaction system of this method is green safe, and reaction condition is mild, reaction rate compared with
Fastly, product postprocessing process is simple, and the magnanimity preparation of the simple green of GQDs may be implemented, with important application value and
Application prospect.Its technical solution is as follows:
(1) deionized water of certain mass is added in the container with agitating device, is added further according to above-mentioned ratio range
Suitable maltose stirs at 25-80 DEG C to being completely dissolved uniformly；
(2) water heating kettle is added in solution obtained in (1) step, is gradually heated to 150-250 DEG C, keep pressure 10Mpa with
It is interior, hydro-thermal reaction is carried out, is discharged after reacting 2-15h；
(3) the dark brown material that (2) step obtains is subjected to centrifugation point in centrifuge with the speed of 6000-12000r/min
From, isolate dark brown precipitating, upper layer is light yellow transparent liquid, as the aqueous solution of graphene quantum dot.
A kind of green method being prepared graphene quantum dot using maltose is gone using maltose as carbon source
For ionized water as solvent, preparation process is simple and does not add any chemical reagents, environmentally protective, without any environmental pollution.
A kind of green method preparing graphene quantum dot using maltose, the quality of deionized water and maltose
It is 50 ~ 200:2 ~ 10 than range, preferred value is 100 ~ 150:5 ~ 7.Compared with the existing technology, the present invention has the following advantages: of the invention
Using maltose as raw material, using deionized water as solvent, GQDs is prepared using green method.It is GQDs obtained
Diameter is of uniform size, and has good water-soluble and fluorescence property.By Optimizing Technical, this method prepares the receipts of GQDs
Rate can achieve 60%, can be applied to electronic device, imaging biological cells, the various technical fields such as bio-sensing.It is compared to it
Its GQDs preparation method, the reaction system of this method is green safe, and reaction condition is mild, and reaction rate is very fast, product postprocessing
Process is simple, and the magnanimity preparation of the simple green of GQDs may be implemented, have important application value and application prospect.
Detailed description of the invention
Fig. 1 is the TEM photo of graphene quantum dot prepared by embodiment 1.
Fig. 2 is the XRD spectra of graphene quantum dot prepared by embodiment 1.
Fig. 3 is the fluorescence photo of GQDs in the UV lamp prepared by embodiment 1.
Fig. 4 is the fluorescence spectrum of the GQDs of preparation in embodiment 1 at excitation wavelength 365nm.
Specific embodiment
Embodiment 1
1kg deionized water is added in the container with agitating device, adds 35g maltose, is heated to 60 DEG C, stirring
20min is to being completely dissolved；Water heating kettle is added in the solution of maltose, is gradually heated to 180 DEG C, keeps pressure within 8Mpa,
Hydro-thermal reaction is carried out, is discharged after reacting 10h；By obtained dark brown material in centrifuge with the speed of 8000r/min into
Dark brown precipitating is isolated in row centrifuge separation, and the light yellow transparent liquid that upper layer obtains, as graphene quantum dot is water-soluble
Liquid.
Embodiment 2
1kg deionized water is added in the container with agitating device, adds 40g maltose, is heated to 70 DEG C, stirring
20min extremely dissolves；Water heating kettle is added in solution containing maltose, is gradually heated to 170 DEG C, keeps pressure within 8Mpa,
Hydro-thermal reaction is carried out, is discharged after reacting 12h；By obtained dark brown material in centrifuge with the speed of 10000r/min into
Dark brown precipitating is isolated in row centrifuge separation, and the light yellow transparent liquid that upper layer obtains, as graphene quantum dot is water-soluble
Liquid.
Embodiment 3
1kg deionized water is added in the container with agitating device, adds 30g maltose, is heated to 55 DEG C, stirring
25min is to being completely dissolved；Water heating kettle is added in solution containing maltose, is gradually heated to 180 DEG C, keeps pressure in 10Mpa
Within, hydro-thermal reaction is carried out, is discharged after reacting 8h；By obtained dark brown material with the speed of 11000r/min in centrifuge
Degree is centrifuged, and isolates dark brown precipitating, the light yellow transparent liquid that upper layer obtains, the as water of graphene quantum dot
Solution.
Claims (4)
1. a kind of method for preparing graphene quantum dot using maltose, which comprises the steps of:
(1) deionized water is added in the container with agitating device, adds maltose, at 25-80 DEG C, stirring is to completely molten
Solution；
(2) water heating kettle is added in solution obtained in step (1), pressure control is temperature control within 10Mpa in water heating kettle
It is to discharge after carrying out hydro-thermal reaction 2-15h at 150-250 DEG C, obtains dark brown material；
(3) dark brown material obtained in step (2) is subjected to centrifugation point in centrifuge with the speed of 6000-12000r/min
From, removal bottom dark brown precipitating, the upper layer light yellow transparent liquid isolated, the as aqueous solution of graphene quantum dot.
2. the method according to claim 1 for preparing graphene quantum dot using maltose, which is characterized in that deionized water
It than range is 50 ~ 200:2 ~ 10 with the quality of maltose.
3. the method according to claim 1 for preparing graphene quantum dot using maltose, which is characterized in that deionized water
It than range is 100 ~ 150:5 ~ 7 with the quality of maltose.
4. the method according to claim 1 for preparing graphene quantum dot using maltose, which is characterized in that hydro-thermal reaction
Temperature is 180 DEG C, reaction pressure 8MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111039280A (en) * | 2019-12-16 | 2020-04-21 | 华南理工大学 | Lignin-based graphene quantum dot and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190296A (en) * | 2011-06-15 | 2011-09-21 | 昆明物理研究所 | Hydrothermal method for preparing water-soluble graphene quantum dots |
| CN102660270A (en) * | 2012-05-03 | 2012-09-12 | 吉林大学 | Method for preparing fluorescent graphene quantum dots by solvothermal method |
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
-
2019
- 2019-01-28 CN CN201910082011.1A patent/CN109626363A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190296A (en) * | 2011-06-15 | 2011-09-21 | 昆明物理研究所 | Hydrothermal method for preparing water-soluble graphene quantum dots |
| CN102660270A (en) * | 2012-05-03 | 2012-09-12 | 吉林大学 | Method for preparing fluorescent graphene quantum dots by solvothermal method |
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN111039280A (en) * | 2019-12-16 | 2020-04-21 | 华南理工大学 | Lignin-based graphene quantum dot and preparation method and application thereof |
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Application publication date: 20190416 |