CN108249425A - Using system with molecular sieve for preparing for the method for graphene quantum dot - Google Patents
Using system with molecular sieve for preparing for the method for graphene quantum dot Download PDFInfo
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- CN108249425A CN108249425A CN201810062764.1A CN201810062764A CN108249425A CN 108249425 A CN108249425 A CN 108249425A CN 201810062764 A CN201810062764 A CN 201810062764A CN 108249425 A CN108249425 A CN 108249425A
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Abstract
The present invention provides it is a kind of using system with molecular sieve for preparing for the method for graphene quantum dot, have the feature that, following steps：Predecessor and molecular sieve are mixed to get mixed solution by step 1 with certain proportion；Step 2 is handled by hydro-thermal method mixed solution to obtain synthetic；Synthetic is centrifuged to obtain the graphene quantum dot molecular sieve containing graphene quantum dot by step 3；Graphene quantum dot molecular sieve under conditions of 70~100 DEG C is stirred, is desorbed out graphene quantum dot by step 4.By the graphene quantum dot even size distribution of this method preparation, purity is high, quantum yield is high, solves the problem of graphene quantum dot prepared by hydro-thermal method is uneven there are particle diameter distribution, and impurity content is high.This method is simple for process, easy to operate, and the graphene quantum dot of different-grain diameter can be prepared according to actual needs.
Description
Technical field
The present invention relates to a kind of methods for preparing graphene quantum dot, and in particular to a kind of to utilize system with molecular sieve for preparing for graphene
The method of quantum dot.
Background technology
Graphene quantum dot is the nano material of quasi-zero dimension, and size has significant quantum limit between 1~10nm
Domain effect and boundary effect show good chemical inertness, biocompatibility and relatively low bio-toxicity, be applied to biology into
The fields such as picture, disease detection, photoelectric device be related to the energy.
Hydro-thermal method is one of preparation method of common graphene quantum dot.Hydro-thermal method compared with other preparation methods,
What is prepared is simple for process, does not need to the corrosive liquids such as strong acid and strong base.But there are grain sizes point for the graphene quantum dot of hydro-thermal method preparation
The problem of cloth is uneven, and impurity content is high.This problem not only makes the quality decline of graphene quantum dot, also affects graphene
The quantum yield of quantum dot.
Invention content
The present invention is uneven there are particle diameter distribution in order to solve the graphene quantum dot of hydro-thermal method preparation, and impurity content is high
The problem of and carry out, and it is an object of the present invention to provide a kind of method using system with molecular sieve for preparing for graphene quantum dot.
The present invention provides it is a kind of using system with molecular sieve for preparing for the method for graphene quantum dot, have the feature that, below
Step：Predecessor and molecular sieve are mixed to get mixed solution by step 1 with certain proportion；Step 2 passes through mixed solution
Hydro-thermal method is handled to obtain synthetic；Step 3 is centrifuged synthetic to obtain the graphene containing graphene quantum dot
Quantum dot-molecular sieve；Graphene quantum dot-molecular sieve under conditions of 70~100 DEG C is stirred, is desorbed out by step 4
Graphene quantum dot.
It is provided by the invention using system with molecular sieve for preparing for the method for graphene quantum dot, can also have the feature that：
Wherein, the pore size of molecular sieve is any one size in 3nm, 5nm, 8nm and 10nm.
It is provided by the invention using system with molecular sieve for preparing for the method for graphene quantum dot, can also have the feature that：
Wherein, molecular sieve is any one in MCM-41 molecular sieves, SBA-15 molecular sieves and FDU-12 molecular sieves.
It is provided by the invention using system with molecular sieve for preparing for the method for graphene quantum dot, can also have the feature that：
Wherein, predecessor and molecular sieve are using mass ratio as 1:1~1:Any one ratio mixing in the range of 10.
It is provided by the invention using system with molecular sieve for preparing for the method for graphene quantum dot, can also have the feature that：
Wherein, the treatment temperature of hydro-thermal method is 160 DEG C, processing time 15h.
It is provided by the invention using system with molecular sieve for preparing for the method for graphene quantum dot, can also have the feature that：
Wherein, the mode of heating of step 4 is heated for direct heating water bath or by the way of condensing reflux.
The effect of invention
According to it is according to the present invention using system with molecular sieve for preparing for the method for graphene quantum dot because being added in predecessor
Molecular sieve so that obtaining that graphene quantum dot is only similar to the pore size of molecular sieve after being handled by hydro-thermal method just can be into
Enter and graphene quantum dot-molecular sieve formed inside the hole of molecular sieve, so as to the graphene quantum dot with other scales in solution and
Impurity is detached.Graphene quantum dot-molecular sieve is obtained after centrifugation.Graphene in graphene quantum dot-molecular sieve
Quantum dot can be desorbed away to obtain graphene quantum dot under conditions of 70~100 DEG C inside the hole from molecular sieve.Institute
With by the graphene quantum dot even size distribution of this method preparation, purity is high, quantum yield is high.
This method not only it is simple for process should, it is easy to operate, but also can be realized under 70~100 DEG C of cryogenic conditions de-
Attached, energy consumption is relatively low.
Description of the drawings
Fig. 1 is transmission electron microscope (TEM) spectrum of the nitrogen-doped graphene quantum dot obtained in the embodiment of the present invention
Figure；
Fig. 2 is the nitrogen-doped graphene quantum dot that in the present embodiment prepared by original nitrogen-doped graphene quantum dot and embodiment
Fluorescence spectrum.
Specific embodiment
It is real below in order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention
Example combination attached drawing is applied to be specifically addressed the present invention for the method for graphene quantum dot using system with molecular sieve for preparing.
Graphene quantum dot can be not only prepared, but also element can be prepared using system with molecular sieve for preparing for the method for graphene quantum dot
Doped graphene quantum dot.In the present embodiment, it is described in detail for preparing nitrogen-doped graphene quantum dot.
Step 1 weighs the MCM-41 molecular sieves 1g that average pore size is 3nm.
Step 2 cleans MCM-41 molecular sieves：First add in 100ml deionized waters, ultrasonic disperse 20 minutes；It adds
100ml absolute ethyl alcohols, ultrasonic disperse 20.
Step 3 weighs predecessor citric acid 0.5g, weighs dopant urea 0.55g.Citric acid and urea are mixed, and
Distilled water 30ml is added in be dissolved.
Step 4, cleaned MCM-41 molecular sieves are added in into the citric acid and urea of dissolving, and stirring 30min is mixed
Solution is closed, mixed solution is transferred in hydrothermal reaction kettle.
Step 5 in hydrothermal reaction kettle, mixed solution is handled by hydro-thermal method to obtain synthetic, wherein, place
It is 160 DEG C to manage temperature, processing time 15h.Nitrogen of the synthetic comprising nitrogen-doped graphene quantum dot-molecular sieve, other sizes
Doped graphene quantum dot and impurity.
Synthetic is centrifuged to obtain the nitrogen-doped graphene quantum containing nitrogen-doped graphene quantum dot by step 6
Point-molecular sieve.
Step 7 cleans nitrogen-doped graphene quantum dot-molecular sieve with 100ml ethyl alcohol, is centrifuged off ethyl alcohol.
Step 8 adds in distilled water 30ml, directly while stirring in nitrogen-doped graphene quantum dot-molecular sieve after cleaning
Water receiving bath is heated to 95 DEG C and keeps 5h at such a temperature, during which keeps stirring, is desorbed out nitrogen-doped graphene quantum dot.
In the present embodiment, the average pore size of molecular sieve is 3nm, and in practical applications, the average pore size of molecular sieve may be used also
Think any one size in 5nm, 8nm and 10nm.
In the present embodiment, molecular sieve is MCM-41 molecular sieves, and in practical applications, molecular sieve can also be SBA-15 points
Son sieve or FDU-12 molecular sieves.
In the present embodiment, the mass ratio of predecessor and MCM-41 molecular sieves is 1:2, in practical applications, predecessor with
The mass ratio of molecular sieve can also be 1:1~1:Arbitrary value in the range of 10.
In the present embodiment, the mode of heating of step 8 is direct heating water bath, in practical applications, can also be used cold
The mode of solidifying reflux is heated..
In the present embodiment, the heating temperature of step 8 is 95 DEG C, and in practical applications, the heating temperature of step 8 is 70
Arbitrary value in the range of~100 DEG C.
Fig. 1 is transmission electron microscope (TEM) spectrum of the nitrogen-doped graphene quantum dot obtained in the embodiment of the present invention
Figure.
As shown in Figure 1, the nitrogen-doped graphene quantum dot that embodiment obtains is spherical shape, average diameter of particles 3nm, grain size
It is distributed as 2~4nm.
Fig. 2 is the nitrogen-doped graphene quantum dot that in the present embodiment prepared by original nitrogen-doped graphene quantum dot and embodiment
Fluorescence spectrum.
As shown in Fig. 2, abscissa represents wavelength, ordinate represents fluorescence intensity, and the solid line in figure is prepared for embodiment
The fluorescence spectrum of nitrogen-doped graphene quantum dot, dotted line are the fluorescence spectrum of original nitrogen-doped graphene quantum dot.It can be with from Fig. 2
Find out, compared with the original nitrogen-doped graphene quantum dot prepared by hydro-thermal method of the prior art, make through this embodiment
The fluorescence intensity of standby nitrogen-doped graphene quantum dot significantly increases.
Meanwhile the quantum yield of nitrogen-doped graphene quantum dot prepared through this embodiment is up to up to 75%, and pass through
The quantum yield of original nitrogen-doped graphene quantum dot prepared by hydro-thermal method of the prior art is only 49%.
The effect of embodiment
According to it is according to the present invention using system with molecular sieve for preparing for the method for graphene quantum dot because being added in predecessor
Molecular sieve so that obtaining that graphene quantum dot is only similar to the pore size of molecular sieve after being handled by hydro-thermal method just can be into
Enter and graphene quantum dot-molecular sieve formed inside the hole of molecular sieve, so as to the graphene quantum dot with other scales in solution and
Impurity is detached.Graphene quantum dot-molecular sieve is obtained after centrifugation.Graphene in graphene quantum dot-molecular sieve
Quantum dot can be desorbed away to obtain graphene quantum dot under conditions of 70~100 DEG C inside the hole from molecular sieve.Institute
By the way that the graphene quantum dot particle diameter distribution of this method preparation is uniform, purity is high, quantum yield is high, to not only solve existing
The problem of graphene quantum dot particle diameter distribution that in technology prepared by hydro-thermal method is uneven, and impurity content is high also improves quantum production
Rate.
This method not only it is simple for process should, it is easy to operate, but also can be realized under 70~100 DEG C of cryogenic conditions de-
Attached, energy consumption is relatively low.
This method can also obtain the graphene quantum of corresponding uniform particle size by changing the pore size of molecular sieve
Point, it is possible to the graphene quantum dot of different-grain diameter is prepared according to actual needs.
This method can not only prepare graphene quantum dot, but also can prepare element doping graphene quantum dot.
Preferred case of the above embodiment for the present invention, is not intended to limit protection scope of the present invention.
Claims (6)
1. it is a kind of using system with molecular sieve for preparing for the method for graphene quantum dot, which is characterized in that include the following steps：
Predecessor and molecular sieve are mixed to get mixed solution by step 1 with certain proportion；
Step 2 is handled by hydro-thermal method the mixed solution to obtain synthetic；
The synthetic is centrifuged to obtain graphene quantum dot-molecular sieve containing graphene quantum dot by step 3；
Graphene quantum dot-the molecular sieve under conditions of 70~100 DEG C is stirred, is desorbed out graphene by step 4
Quantum dot.
2. it is according to claim 1 using system with molecular sieve for preparing for the method for graphene quantum dot, it is characterised in that：
Wherein, the pore size of the molecular sieve is any one size in 3nm, 5nm, 8nm and 10nm.
3. it is according to claim 1 using system with molecular sieve for preparing for the method for graphene quantum dot, it is characterised in that：
Wherein, the molecular sieve is any one in MCM-41 molecular sieves, SBA-15 molecular sieves and FDU-12 molecular sieves.
4. it is according to claim 1 using system with molecular sieve for preparing for the method for graphene quantum dot, it is characterised in that：
Wherein, the predecessor and the molecular sieve are using mass ratio as 1:1~1:Any one ratio mixing in the range of 10.
5. it is according to claim 1 using system with molecular sieve for preparing for the method for graphene quantum dot, it is characterised in that：
Wherein, the treatment temperature of the hydro-thermal method is 160 DEG C, processing time 15h.
6. it is according to claim 1 using system with molecular sieve for preparing for the method for graphene quantum dot, it is characterised in that：
Wherein, the mode of heating of step 4 is heated for direct heating water bath or by the way of condensing reflux.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349436A (en) * | 2018-12-24 | 2020-06-30 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN111422862A (en) * | 2020-05-12 | 2020-07-17 | 上海理工大学 | Method for separating graphene quantum dots by using molecular sieve |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104192827A (en) * | 2014-08-26 | 2014-12-10 | 上海交通大学 | Method for synthesizing carbon quantum dots on basis of organic micromolecule microwave solid-phase reaction |
| CN104774611A (en) * | 2015-03-31 | 2015-07-15 | 吉林大学 | One-pot method for preparing two carbon quantum dots different in illuminant property |
| CN107434972A (en) * | 2017-08-11 | 2017-12-05 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of molecular-sieve carbon quantum dot probe and preparation method thereof and the application in the detection of acid organic gas |
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- 2018-01-23 CN CN201810062764.1A patent/CN108249425B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104192827A (en) * | 2014-08-26 | 2014-12-10 | 上海交通大学 | Method for synthesizing carbon quantum dots on basis of organic micromolecule microwave solid-phase reaction |
| CN104774611A (en) * | 2015-03-31 | 2015-07-15 | 吉林大学 | One-pot method for preparing two carbon quantum dots different in illuminant property |
| CN107434972A (en) * | 2017-08-11 | 2017-12-05 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of molecular-sieve carbon quantum dot probe and preparation method thereof and the application in the detection of acid organic gas |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349436A (en) * | 2018-12-24 | 2020-06-30 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN111422862A (en) * | 2020-05-12 | 2020-07-17 | 上海理工大学 | Method for separating graphene quantum dots by using molecular sieve |
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