CN104386666B - Method for preparing carbon quantum dots through alcohol decomposition - Google Patents
Method for preparing carbon quantum dots through alcohol decomposition Download PDFInfo
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- CN104386666B CN104386666B CN201410566040.2A CN201410566040A CN104386666B CN 104386666 B CN104386666 B CN 104386666B CN 201410566040 A CN201410566040 A CN 201410566040A CN 104386666 B CN104386666 B CN 104386666B
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Abstract
The invention relates to a method for preparing carbon quantum dots through alcohol decomposition. The method comprises the following steps: preparing an alkaline matter alcoholic solution of which the concentration is 0.1 to 10 mol/L to obtain a dispersing liquid containing carbon quantum dots, wherein the temperature is 15 to 200 DEG C, and the carbonization time is 2 to 360 h; conducting dialyzing and vacuum drying on the dispersing liquid to obtain solid carbon quantum dots. The method takes alcohol as a carbon source, and adopts a room temperature standing or heating manner to obtain the carbon quantum dots, thereby being simple, wide in raw material source, low in cost and high in mass production possibility.
Description
Technical field
The invention belongs to the preparing technical field of carbon quantum dot, be specifically related to the preparation method of a kind of carbon quantum dot.
Background technology
Carbon quantum dot (CQDs), due to the performance of its uniqueness, is caused extensively pass as a kind of general fluorescent nano material
Note.Compared with traditional semiconductor-quantum-point, carbon quantum dot have low optical flare, low photofading, hypotoxicity, high quantum production rate,
The advantages such as excellent Photophysical Behaviors, good biocompatibility.
It has been reported that the method for preparation carbon quantum dot have: laser ablation, plasma treatment, electrochemical synthesis, Hydrothermal Synthesis,
The synthesis of chemical oxidation, microwave, ultrasonic synthesis etc..But prepared by these methods carbon quantum dot mostly process is complicated, energy consumption is high, product
Measure low.
Patent application CN201310378455.2 discloses a kind of method that fluorescent carbon quantum dot is prepared in alcohol electrochemistry carbonization, bag
Including following steps: with alcohol as carbon source, using alkaline matter and mixed alkoxide solution as electrolyte, platinized platinum is as working electrode with to electricity
Pole,
Calomel, as reference electrode, is electrolysed, and collects reaction solution, and in reaction solution, addition acid neutralization alkaline matter is to neutral,
Stand and salt is precipitated, take supernatant, supernatant adds alcohol, will salt out further, and again take supernatant, obtain carbon quantum
Point alcoholic solution the method has obtained carbon quantum dot, and carbon quantum dot alcoholic solution evaporates to obtain solid, by the solid that obtains in water ultrasonic
Dispersion, and by the aqueous solution obtaining carbon quantum dot after bag filter dialysis of the liquid after dispersion.Although the method productivity is higher, but behaviour
Make complexity, its electrode platinized platinum to be used, also want additional electric energy, need voltage-regulation instrument, relatively costly, there is limitation.
Summary of the invention
The method that it is an object of the invention to provide the preparation carbon quantum dot that a kind of method is simple, low cost, energy consumption are low, productivity is high.
The method that a kind of alcohol of the present invention decomposes preparation carbon quantum dot is as follows: the alcoholic solution of preparation alkaline matter, standing and reacting,
To the dispersion liquid of carbon containing quantum dot, by purified for this dispersion liquid, be dried to obtain carbon quantum dot solid.
Described alcohol is that carbon number is more than or equal to 2, monohydric alcohol, dihydroxylic alcohols or the polyhydric alcohol less than or equal to 30.
Described alcohol be preferably ethanol, propanol, butanol, amylalcohol, hexanol, enanthol, capryl alcohol, nonyl alcohol, decanol, lauryl alcohol,
Tridecanol, tetradecyl alchohol, pentadecanol, hexadecanol, Heptadecyl alcohol, octadecanol, nonadecanol, eicosanol, docosanol, 24
One in alcohol, hexacosyl alcohol, octacosanol, melissyl alcohol, ethylene glycol, glycerol, 1-propenol-3, benzyl alcohol, phenethanol or
Several.
Described alkaline matter is one or more in Lithium hydrate, potassium hydroxide, sodium hydroxide, phosphate, carbonate.
Described alkaline matter concentration in alcoholic solution is 0.1-10mol/L.
The above-mentioned response time is 2-360h；Reaction temperature is 15-200 DEG C.The preferably response time is 48-120h；Preferably react
Temperature is 25-120 DEG C.
Described way of purification is dialysis.Described dialysis uses molecular cut off to be the bag filter of 500-5000；Dialysis time is
10-120h.Described carbon quantum dot is smaller in size than 5nm.
Described be dried into vacuum drying, temperature is 80-150 DEG C；Drying time is 4-24h.
Described vacuum drying temperature is 80-150 DEG C.
The described vacuum drying time is 4-24h.
The present invention utilizes alcohol chemical decomposition method to prepare carbon quantum dot innovatively.Owing to have employed above scheme, the present invention has
Benefit effect is: preparation method is simple, and mild condition is controlled, it is not necessary to using expensive instrument, the method is with low cost, less energy consumption,
Raw material sources are extensive, are expected to realize industrialized production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 1；
Fig. 2 is the fluorescence spectrum of the carbon quantum dot obtained in embodiment 1；
Fig. 3 is the XRD figure of the carbon quantum dot obtained in embodiment 1；
Fig. 4 is the XPS figure of the carbon quantum dot obtained in embodiment 1；
Fig. 5 is the reaction solution color change photo of differential responses time in embodiment 1；
Fig. 6 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 2；
Fig. 7 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 3；
Fig. 8 is the carbon quantum dot solid photo obtained in embodiment 3.
Detailed description of the invention
Following example are in order to the present invention is explained in greater detail, and these embodiments do not constitute any restriction, the present invention to the present invention
Can the either type as described in summary of the invention implement.
Embodiment 1
The ethanol solution of preparation 0.5mol/L sodium hydroxide, room temperature (25 DEG C) standing and reacting 360h, take out supernatant and obtain carbon
The dispersion liquid of quantum dot；Dialyse 60h by the carbon quantum dot dispersion liquid bag filter that molecule is 2000 through damming, vacuum at 80 DEG C
It is dried 24h, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 1, and particle diameter is more uniform, less than 5nm.Fig. 2 is it
Fluorescence spectrum figure, has the change along with exciting light spectrum and the feature that changes, and its optimal fluorescence emission peak is 440nm, corresponding
Excitation wavelength be 340nm.Fig. 3 is its X-ray diffraction (XRD) spectrogram, and the carbon quantum dot obtained is amorphous carbon.Fig. 4
For its photoelectron spectroscopy (XPS), 284.7eV peak corresponds to graphitization sp2 carbon atom, and the peak of 286.3eV and 287.8eV corresponds to
C-O and C=O carbon atom, carbon quantum dot oxygen-containing functional group.Fig. 5 is the photo of its differential responses time, as time went on,
Quantum dot concentration is gradually increased, color burn.
Embodiment 2
The butanol solution of preparation 1.5mol/L sodium hydroxide, room temperature standing and reacting 120h, take out supernatant and obtain carbon quantum dot
Dispersion liquid；Dialyse 60h by the carbon quantum dot dispersion liquid bag filter that molecular weight is 2000 through damming, and is vacuum dried at 120 DEG C
12h, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 6, and particle diameter is more uniform, less than 5nm.
Embodiment 3
The ethylene glycol solution of preparation 5mol/L sodium hydroxide, oil bath is heated, and reacts 2h at 200 DEG C, takes out supernatant and obtains carbon
The dispersion liquid of quantum dot；Dialyse 120h by the carbon quantum dot dispersion liquid bag filter that molecular weight is 2000 through damming, at 150 DEG C
Vacuum drying 4h, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 7, and particle diameter is more uniform, less than 5nm, Fig. 8 is
Obtain carbon quantum dot solid photo.
Embodiment 4
The ethanol solution of preparation 0.5mol/L Lithium hydrate, room temperature (25 DEG C) standing and reacting 360h, take out supernatant and obtain carbon
The dispersion liquid of quantum dot；Dialyse 10h by the carbon quantum dot dispersion liquid bag filter that molecular weight is 500 through damming, vacuum at 80 DEG C
It is dried 24h, obtains carbon quantum dot solid.
Embodiment 5
The butanol solution of preparation 1.5mol/L potassium hydroxide, room temperature standing and reacting 240h, take out supernatant and obtain carbon quantum dot
Dispersion liquid；Dialyse 120h by the carbon quantum dot dispersion liquid bag filter that molecular weight is 5000 through damming, and at 120 DEG C, vacuum is done
Dry 10h, obtains carbon quantum dot solid.
Embodiment 6
The ethylene glycol solution of preparation 2mol/L potassium hydroxide, oil bath is heated, and reacts 4h at 120 DEG C, takes out supernatant and obtains carbon
The dispersion liquid of quantum dot；Dialyse 120h by the carbon quantum dot dispersion liquid bag filter that molecular weight is 5000 through damming, at 120 DEG C
Vacuum drying 10h, obtains carbon quantum dot solid.
Embodiment 7
The ethanol solution of preparation 10mol/L potassium hydroxide, room temperature standing and reacting 48h, take out supernatant and obtain dividing of carbon quantum dot
Dissipate liquid；By carbon quantum dot dispersion liquid through the bag filter dialysis 120h of molecular cut off 2000, at 120 DEG C, it is vacuum dried 10h,
Obtain carbon quantum dot solid.
Embodiment 8
The decanol solution of preparation 2mol/L sodium hydroxide, room temperature standing and reacting 120h, take out supernatant and obtain dividing of carbon quantum dot
Dissipate liquid；By carbon quantum dot dispersion liquid through the bag filter dialysis 120h of molecular cut off 2000, at 100 DEG C, it is vacuum dried 12h,
Obtain carbon quantum dot solid.
Embodiment 9
The octadecanol solution of preparation 1mol/L sodium hydroxide, oil bath is heated, and reacts 8h at 100 DEG C, take out supernatant and obtain
The dispersion liquid of carbon quantum dot；By carbon quantum dot dispersion liquid through molecular cut off 2000 bag filter dialyse 120h, at 120 DEG C
Vacuum drying 10h, obtains carbon quantum dot solid.
Embodiment 10
The benzyl alcohol solution of preparation 3mol/L potassium hydroxide, room temperature standing and reacting 100h, take out supernatant and obtain carbon quantum dot
Dispersion liquid；By carbon quantum dot dispersion liquid through the bag filter dialysis 96h of molecular cut off 3000, at 150 DEG C, it is vacuum dried 8h,
Obtain carbon quantum dot solid.
The alcohol selected in the embodiment of the present invention is that carbon number is more than or equal to 2, monohydric alcohol less than or equal to 30, dihydroxylic alcohols,
Polyhydric alcohol, as ethanol, propanol, butanol, amylalcohol, hexanol, enanthol, capryl alcohol, nonyl alcohol, decanol, lauryl alcohol (lauryl alcohol),
Tridecanol, tetradecyl alchohol (myristyl alcohol), pentadecanol, hexadecanol (palmityl alcohol), Heptadecyl alcohol, octadecanol (stearyl alcohol), 19
Alcohol, eicosanol (arachidic alcohol), docosanol (behenyl alcohol), tetracosanol (wood burnt alcohol), hexacosyl alcohol (ceryl alcohol), 20
One or more in eight alcohol, melissyl alcohol (melissyl alcohol), ethylene glycol, glycerol, 1-propenol-3, benzyl alcohol, phenethanol；Alkali bag
Include: Lithium hydrate, potassium hydroxide, sodium hydroxide, phosphate, carbonate, ammonia etc..
Claims (10)
1. the method that an alcohol decomposes preparation carbon quantum dot, it is characterised in that the alcoholic solution of preparation alkaline matter, quiet
Put reaction, obtain the dispersion liquid of carbon containing quantum dot, by purified for this dispersion liquid, be dried to obtain carbon quantum dot solid.
Method the most according to claim 1, it is characterised in that described alcohol is that carbon number is more than or equal to 2,
Monohydric alcohol less than or equal to 30, polyhydric alcohol.
Method the most according to claim 2, it is characterised in that described alcohol be ethanol, propanol, butanol, penta
Alcohol, hexanol, enanthol, capryl alcohol, nonyl alcohol, decanol, lauryl alcohol, tridecanol, tetradecyl alchohol, pentadecanol, 16
Alcohol, Heptadecyl alcohol, octadecanol, nonadecanol, eicosanol, docosanol, tetracosanol, hexacosyl alcohol, 20
One or more in eight alcohol, melissyl alcohol, ethylene glycol, glycerol, 1-propenol-3, benzyl alcohol, phenethanol.
Method the most according to claim 1, it is characterised in that described alkaline matter is Lithium hydrate, hydrogen-oxygen
Change one or more in potassium, sodium hydroxide, phosphate, carbonate.
5. according to the method described in claim 1 or 4, it is characterised in that described alkaline matter is in alcoholic solution
Concentration be 0.1-10mol/L.
6. according to the method described in any one of claim 1-4, it is characterised in that the response time is 2-360h；Instead
Temperature is answered to be 15-200 DEG C.
Method the most according to claim 6, it is characterised in that the response time is 48-120h；Reaction temperature is
25-120℃。
Method the most according to claim 1, it is characterised in that described way of purification is dialysis.
Method the most according to claim 1, it is characterised in that described carbon quantum dot is smaller in size than 5nm.
Method the most according to claim 1, it is characterised in that described be dried into vacuum drying, temperature is
80-150℃；Drying time is 4-24h.
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| CN104927848B (en) * | 2015-06-16 | 2017-03-29 | 复旦大学 | Material of bio-imaging probe and oxygen reduction catalyst and preparation method thereof |
| CN105129764B (en) * | 2015-07-14 | 2017-04-26 | 中南大学 | Method of quickly preparing carbon quantum dots at high yield through aldehyde compound |
| CN109337682B (en) * | 2018-12-26 | 2020-03-31 | 赵方浩 | Method for preparing fluorescent carbon quantum dots at room temperature |
| CN110257060B (en) * | 2019-07-09 | 2020-08-28 | 西南大学 | Method for preparing carbon dots by using resveratrol, product and application |
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| CN103449404B (en) * | 2013-08-27 | 2016-04-27 | 湖南师范大学 | The method of fluorescent carbon point is prepared in the carbonization of a kind of alcohol electrochemistry |
| CN103482598A (en) * | 2013-08-30 | 2014-01-01 | 吉林大学 | Preparation method for monophosphate-adjuvant water-soluble fluorescent carbon quantum dot solid powder |
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