CN109095452A - A kind of preparation method of carbon quantum dot - Google Patents
A kind of preparation method of carbon quantum dot Download PDFInfo
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- CN109095452A CN109095452A CN201811248324.1A CN201811248324A CN109095452A CN 109095452 A CN109095452 A CN 109095452A CN 201811248324 A CN201811248324 A CN 201811248324A CN 109095452 A CN109095452 A CN 109095452A
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- C01B32/15—Nano-sized carbon materials
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention provides a kind of preparation methods of carbon quantum dot, belong to technical field of nanometer material preparation.The present invention uses polyethyleneimine as raw material, and carbonization treatment is directly carried out on heating platform, can be obtained the carbon quantum dot with visible spectral range fluorescent emission after natural cooling dialysis.Carbon quantum dot preparation method disclosed by the invention has synthesis technology simple, efficiently quick advantage, and polyethyleneimine is used as forming core carbon source and surface-functionalized group simultaneously, other solvent impurities are not introduced in synthesis process, carbon quantum dot purity is high, the yield of synthesis are big, have good monodispersity in aqueous solvent.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of preparation method of carbon quantum dot.
Background technique
Carbon quantum dot (also referred to as carbon dots, CDots) is different from two-dimensional graphene and one-dimensional carbon nanotube, is a kind of tool
There is the zero dimension carbon nanomaterial of special performance.Carbon quantum dot is generally defined as the carbon nano-particle with passivated surface, and right
Its most effective passivation mode is to carry out surface-functionalized processing according to application demand using organic or polymer molecule.Carbon quantum
The synthetic method of point is broadly divided into chemical fine functionalization synthetic method and " one pot " carbonizatin method.Chemical fine functionalization method is carbon amounts
Son puts initial synthetic method, using carbon nano-particle as carbon core template, using organic or polymer molecule by chemical method to it
Carry out surface-functionalized, had excellent performance and structure definition clearly carbon quantum dot, but this method is complicated for operation, cost compared with
It is high." one pot " carbonizatin method is different from the fine functionalization synthetic method of chemistry, and carbon core is formed in carbonisation, remaining after reaction
For polymer molecule by as surface-functionalized group, the advantages of this method is that reaction is convenient and adaptable.Wherein, polyethylene
Imines is the common carbon source synthetic material of " one pot " carbonizatin method, and the carbon quantum dot of synthesis is in bioluminescence imaging, catalysis energy
The application fields such as conversion and opto-electronic device are excellent in.However, existing carbonization method is mainly solvent heat carbonization, height is needed
It presses closed environment and reaction process takes a long time, such as: Chinese patent CN104974750A discloses a kind of based on polyethyleneimine
The carbon quantum dot preparation method of decomposition, the patent preparation process is complicated, needs for polyethyleneimine to be dispersed in alcohol solvent, make
The reaction up to 20h is carried out with reaction kettle, is unfavorable for the industrialization and business application of carbon quantum dot.
Chinese patent CN 107934936A discloses a kind of fast preparation method of carbon quantum dot, and this method divides carbon source
Alkali source is dissipated in solvent and is added, continuous heating prepares carbon quantum dot after mixing, although this method shortens preparation time
To 2h~5h, but the preparation process is introduced such as alkali source and solvent, is increased production cost and is made complex for operation stepization.
Therefore it provides a kind of simple process, the carbon quantum dot for not introducing impurity rapidly and efficiently, and being easy to be mass produced
Preparation method becomes this field urgent problem to be solved.
Summary of the invention
The present invention proposes a kind of preparation method of carbon quantum dot for defect present in background technique.The present invention makes
It uses polyethyleneimine (PEI) as raw material, carbonization treatment is carried out on heating platform, can be obtained tool after natural cooling dialysis
There is the carbon quantum dot of visible spectral range fluorescent emission.Carbon quantum dot preparation method disclosed by the invention has synthesis technology letter
Single, efficiently quick advantage, and polyethyleneimine is used as forming core carbon source and surface-functionalized group simultaneously, in synthesis process not
Other solvent impurities are introduced, carbon quantum dot purity is high, the yield of synthesis are big, have good monodispersity in aqueous solvent.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of carbon quantum dot, comprising the following steps:
Step 1: polyethyleneimine being placed in glass sample bottle, heating platform temperature is set, platform temperature to be heated reaches
When to 400 DEG C~425 DEG C, the glass sample bottle equipped with polyethyleneimine is placed on heating platform and carries out carbonization treatment, located
Glass sample bottle is removed from heating platform after reason, cooled to room temperature；
Step 2: deionized water is added into step 1 treated glass sample bottle, is ultrasonically treated, makes carbon quantum dot
Dispersion in deionized water, forms carbon quantum dot dispersion liquid；
Step 3: the carbon quantum dot dispersion liquid in step 2 being fitted into bag filter and is dialysed, reaction is not participated in removing
Polyethyleneimine；
Step 4: the carbon quantum dot dispersion liquid after dialysis treatment in step 3 being freeze-dried, carbon quantum can be obtained
Point.
Further, every 1g polyethyleneimine described in step 1 carries out the carbonization treatment of 40min~50min.
Further, the amount of deionized water described in step 2 be every 1g polyethyleneimine be added 10mL~15mL go from
Sub- water.
Further, sonication treatment time described in step 2 is 30min~40min.
Further, the molecular cut off of bag filter described in step 3 is 3500~10000.
The present invention also provides application of the carbon quantum dot of above method preparation in lithium-sulfur cell.
Compared with prior art, the invention has the benefit that
(1) carbon quantum dot preparation method disclosed by the invention has synthesis technology simple, efficiently quick advantage.The present invention
Preparation process because real reaction temperature it is higher, so carbonisation faster, significantly shortens preparation time, so that in industry
Time cost can be greatly reduced when upper application, it is only necessary to which a quarter of other preparation methods even 1/10th improves system
Standby efficiency；Autoclave is not necessarily in preparation process of the present invention, and purification process reduces preparation condition door only with dialysis
Sill, the advantage further expansion in terms of practical application.
(2) carbon quantum dot preparation method disclosed by the invention uses polyethyleneimine simultaneously as forming core carbon source and function of surface
To change group, be not necessarily to add solvent in synthesis process, does not introduce other solvent impurities, carbon quantum dot purity is high, the yield of synthesis are big,
There is good monodispersity in aqueous solvent.
Detailed description of the invention
Fig. 1 is carbon quantum dot transmission electron microscope picture prepared by embodiment 1.
Fig. 2 be embodiment 1 react before polyethyleneimine with react after carbon quantum dot FTIR spectrum figure.
Fig. 3 is fluorescence emission spectrum of the carbon quantum dot of the preparation of embodiment 1 under different excitation wavelengths.
Specific embodiment
The present invention is further detailed with reference to the accompanying drawings and examples, but protection scope of the present invention and not only
It is limited to this.
Embodiment 1:
Step 1: 1g polyethyleneimine is placed in the glass sample bottle of 20mL volume, heating platform temperature is set, it is to be added
When hot platform temperature reaches 400 DEG C, the glass sample bottle equipped with polyethyleneimine is placed on heating platform and is carried out at carbonization
50min is managed, after treatment removes glass sample bottle from heating platform, cooled to room temperature；
Step 2: the deionized water of 10mL being added into step 1 treated glass sample bottle, is ultrasonically treated
30min makes carbon quantum dot dispersion in deionized water, forms carbon quantum dot dispersion liquid；
Step 3: the carbon quantum dot dispersion liquid in step 2 being fitted into the bag filter that molecular cut off is 3500 and is carried out thoroughly
Analysis removes the polyethyleneimine for not participating in reaction；
Step 4: the carbon quantum dot dispersion liquid after dialysis treatment in step 3 being freeze-dried, it is dry that 77mg can be obtained
Dry carbon quantum dot.
Embodiment 2
Carbon quantum dot is prepared according to the step of embodiment 1, the platform heating temperature in step 1 is only adjusted to 425 DEG C,
His step is constant, which is prepared the dry carbon quantum dot of 70mg.
Embodiment 3
Step 1: 2g polyethyleneimine is placed in the glass sample bottle of 40mL volume, heating platform temperature is set, it is to be added
When hot platform temperature reaches 400 DEG C, the glass sample bottle equipped with polyethyleneimine is placed on heating platform and is carried out at carbonization
90min is managed, after treatment removes glass sample bottle from heating platform, cooled to room temperature；
Step 2: the deionized water of 30mL being added into step 1 treated glass sample bottle, is ultrasonically treated
30min makes carbon quantum dot dispersion in deionized water, forms carbon quantum dot dispersion liquid；
Step 3: the carbon quantum dot dispersion liquid in step 2 being fitted into the bag filter that molecular cut off is 3500 and is carried out thoroughly
Analysis removes the polyethyleneimine for not participating in reaction；
Step 4: the carbon quantum dot dispersion liquid after dialysis treatment in step 3 being freeze-dried, it is dry that 165mg can be obtained
Dry carbon quantum dot.
Fig. 1 show the transmission electron microscope picture of carbon quantum dot prepared by embodiment 1, from figure 1 it appears that carbon quantum dot
Average-size be about 27.9nm, and quantum dot size is more uniform.
Fig. 2 be embodiment 1 react before polyethyleneimine with react after carbon quantum dot FTIR spectrum figure, from figure
As can be seen that carbon quantum dot saves N-H, C-H and the C-N characteristic peak for reacting preceding polyethyleneimine after reaction in 2, show residue
It is not carbonized polyethyleneimine as surface functional group and is stored in carbon quantum dot surface.
Fig. 3 is fluorescence emission spectrum of the carbon quantum dot under different excitation wavelengths prepared by embodiment 1, can be with from Fig. 3
Find out, fluorescence emission peak red shift of the excitation wavelength to long wave direction carbon quantum dot when mobile, it was demonstrated that the substance of preparation is really carbon amounts
Sub- point.
Claims (6)
1. a kind of preparation method of carbon quantum dot, which comprises the following steps:
Step 1: polyethyleneimine being placed in glass sample bottle, heating platform temperature is set, platform temperature to be heated reaches 400
DEG C~425 DEG C when, the glass sample bottle equipped with polyethyleneimine is placed on heating platform and carries out carbonization treatment, processing terminate
Glass sample bottle is removed from heating platform afterwards, cooled to room temperature；
Step 2: deionized water is added into step 1 treated glass sample bottle, is ultrasonically treated, disperses carbon quantum dot
In deionized water, carbon quantum dot dispersion liquid is formed；
Step 3: the carbon quantum dot dispersion liquid in step 2 being fitted into bag filter and is dialysed, the poly- second for not participating in reaction is removed
Alkene imines；
Step 4: the carbon quantum dot dispersion liquid after dialysis treatment in step 3 being freeze-dried, carbon quantum dot can be obtained.
2. the preparation method of carbon quantum dot according to claim 1, which is characterized in that every poly- second of 1g described in step 1
The carbonization treatment of alkene imines progress 40min~50min.
3. the preparation method of carbon quantum dot according to claim 1, which is characterized in that deionized water described in step 2
Amount be every 1g polyethyleneimine be added 10mL~15mL deionized water.
4. the preparation method of carbon quantum dot according to claim 1, which is characterized in that ultrasonic treatment described in step 2
Time is 30min~40min.
5. the preparation method of carbon quantum dot according to claim 1, which is characterized in that bag filter described in step 3
Molecular cut off is 3500~10000.
6. the carbon quantum dot of any one the method preparation is applied in lithium-sulfur cell according to claim 1~5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115025620A (en) * | 2022-07-07 | 2022-09-09 | 安徽智泓净化科技股份有限公司 | Nanofiltration membrane for extracting lithium from salt lake and production process thereof |
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| WO2014093388A1 (en) * | 2012-12-13 | 2014-06-19 | Pacific Light Technologies Corp. | Composition having dispersion of nano-particles therein and methods of fabricating same |
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| CN108359452A (en) * | 2018-01-24 | 2018-08-03 | 天津师范大学 | A kind of water solubility class graphene quantum dot and the preparation method and application thereof |
| CN108408700A (en) * | 2018-04-04 | 2018-08-17 | 南京工业大学 | Method for large-scale preparation of blue fluorescent carbon nitrogen nanosheet through non-solvent in-situ carbonization |
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| CN115025620A (en) * | 2022-07-07 | 2022-09-09 | 安徽智泓净化科技股份有限公司 | Nanofiltration membrane for extracting lithium from salt lake and production process thereof |
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