CN104528684B - A kind of method that under the conditions of alkalescence, carbon quantum dot is prepared in ketone carbonization - Google Patents
A kind of method that under the conditions of alkalescence, carbon quantum dot is prepared in ketone carbonization Download PDFInfo
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- CN104528684B CN104528684B CN201410756169.XA CN201410756169A CN104528684B CN 104528684 B CN104528684 B CN 104528684B CN 201410756169 A CN201410756169 A CN 201410756169A CN 104528684 B CN104528684 B CN 104528684B
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Abstract
The present invention relates to the method that carbon quantum dot is prepared in ketone carbonization under the conditions of a kind of alkalescence: according to the ratio of concentration 0.1 10mol/L by alkali and ketone mix homogeneously, at 15 100 DEG C, react 12 360h.After reaction terminates, with concentrated hydrochloric acid above-mentioned reactant pH being adjusted to neutrality, centrifugation, clean 5 times with deionized water, vacuum drying obtains carbon quantum dot pressed powder.The method, with ketone as carbon source, obtains carbon quantum dot by the method for room temperature standing and reacting or low-temperature heat, and method is simple, and raw material sources are wide, and low cost can realize large-scale production.
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
The toxicity of traditional semiconductor-quantum-point self and the hazardness to environment limit its actual application.And emerging fluorescent carbon
The performance that quantum dot is unique owing to having light resistance, excellent biocompatibility, hypotoxicity, chemical inertness, low cost etc., quilt
As a kind of general fluorescent nano material.
It has been reported that the method for preparation carbon quantum dot can be divided into from top to bottom and two big class from bottom to top.Method refers to from top to bottom
By the methods such as laser ablation, supersound process, chemistry and electrochemical oxidation smash bigger material with carbon element structure (graphite, activated carbon,
CNT etc.) to obtain undersized carbon quantum dot；From bottom to top rule refer to by Hydrothermal Synthesis, Microwave-assisted synthesis,
Little molecular precursor (saccharide, organic acid, alcohols etc.) carbonization is obtained carbon quantum dot by the means such as electrochemistry carbonization.But, this
A little method mostly processes are complicated, energy consumption is high, yield poorly.
Patent application 201310376464.8 discloses a kind of method that fluorescent carbon quantum dot is prepared in ketone electrochemistry carbonization, including such as
Lower step: with ketone as carbon source, using alkaline matter and ketone mixed solution as electrolyte, platinized platinum as working electrode with to electrode,
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 obtain carbon quantum dot alcoholic solution, by carbon
The aqueous solution of carbon quantum dot is obtained after the dialysis of quantum dot alcoholic solution.Although the method productivity is higher, but operation complexity, its electrode is wanted
Use platinized platinum, also want additional electric energy, need voltage-regulation instrument, relatively costly, there is certain 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.
Under the conditions of a kind of alkalescence of the present invention, to prepare the method for carbon quantum dot as follows in ketone carbonization: preparation alkali and the mixed liquor of ketone, stands anti-
Should or low-temperature heat reaction, generate carbon quantum dot, through hydrochloric acid neutralization, centrifugation, clean, be dried to obtain carbon quantum dot solid.
Described ketone is that carbon number is more than or equal to 3, monoketone, diketone or the polyketones less than or equal to 15.
Described ketone is preferably acetone, 2-butanone, 2 pentanone, propione, methyl-n-butyl ketone, Ketohexamethylene, 2-heptanone, cycloheptanone, 2-
Octanone, cyclooctanone, methyl n-heptyl ketone, decanone, undecyl ketone, ten diketone, ten triketones, ten tetrones, 15 ketone, 1-Phenylethanone., methyl
One or more in 1-Phenylethanone..
Described alkaline matter is one or more in Lithium hydrate, potassium hydroxide, sodium hydroxide, phosphate, carbonate.
Described alkaline matter concentration in mixed liquor is 0.1-10mol/L.
Said method reaction temperature is 15-100 DEG C, and the response time is 12-360h.Preferable reaction temperature is 25-50 DEG C, reaction
Time is 48-120h.
Centrifugation is 8000-16000r/min centrifugation.Clean with deionized water after separation.
Described carbon quantum dot is nano-scale.
Described be dried into vacuum drying, temperature is 80-150 DEG C, and drying time is 4-24h.
Under the conditions of the present invention utilizes alkalescence innovatively, ketone carbonizatin method prepares carbon quantum dot.Owing to have employed above scheme, this
Bright has the beneficial effects that: preparation method is simple, and mild condition is controlled, it is not necessary to use expensive instrument, the method is with low cost,
Less energy consumption, raw material sources are extensive, centrifugal the most separable, it is not necessary to dialysis, are expected to realize industrialized production, and prepare
Carbon quantum dot even particle size distribution.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 1；
Fig. 2 is the XRD figure of the carbon quantum dot obtained in embodiment 1；
Fig. 3 is the XPS figure of the carbon quantum dot obtained in embodiment 1；
Fig. 4 is the fluorescence spectrum of the carbon quantum dot obtained in embodiment 1；
Fig. 5 is the reactant color change photo of differential responses time in embodiment 1；
Fig. 6 is the pressed powder photo of the carbon quantum dot obtained in embodiment 1.
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
Preparation 1.5mol/L sodium hydroxide acetone mixture, room temperature (25 DEG C) standing and reacting 240h, add appropriate concentrated hydrochloric acid,
By its pH regulator to neutral, centrifugation 10min under 12000r/min rotating speed, clean 5 times, at 80 DEG C with deionized water
Lower vacuum drying 24h, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 1, and particle diameter is more uniform, about 10nm.Figure
2 is its X-ray diffraction (XRD) spectrogram, and the carbon quantum dot obtained is amorphous carbon.Fig. 3 is its photoelectron spectroscopy (XPS), 284.6
EV peak corresponds to graphitization sp2 carbon atom, and the peak of 286.4eV and 288.3eV corresponds to C-O and C=O carbon atom, carbon
Quantum dot oxygen-containing functional group.Fig. 4 is its fluorescence spectrum figure, has the change along with exciting light spectrum and the feature that changes.Fig. 5
For the photo of its differential responses time, as time went on, carbon quantum dot concentration is gradually increased, color burn.Fig. 6 is
The photo of the carbon quantum dot pressed powder arrived.
Embodiment 2
Preparation 0.5mol/L sodium hydroxide butanone mixed liquor, room temperature standing and reacting 360h, add appropriate concentrated hydrochloric acid, its pH is adjusted
Joint, to neutral, centrifugation 5min under 16000r/min rotating speed, cleans 5 times with deionized water, is vacuum dried 12 at 120 DEG C
H, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 3
Preparation 5mol/L sodium hydroxide acetylacetone,2,4-pentanedione (2,4-pentanedione) mixed liquor, standing and reacting 120h, add appropriate concentrated hydrochloric acid,
By its pH regulator to neutral, centrifugation under 8500r/min rotating speed, cleaning 5 times with deionized water, at 150 DEG C, vacuum is done
Dry 4h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 4
Preparation 0.5mol/L Lithium hydrate diacetyl mixed liquor, room temperature standing and reacting 120h, add appropriate concentrated hydrochloric acid, by its pH
Regulation, to neutral, centrifugation 15min under 8000r/min rotating speed, is cleaned 5 times with deionized water, is vacuum dried at 80 DEG C
24h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 5
Preparation 1.5mol/L potassium hydroxide, Ketohexamethylene mixed liquor, room temperature standing and reacting 240h, add appropriate concentrated hydrochloric acid, by it
PH regulator, to neutral, centrifugation 10min under 10000r/min rotating speed, cleans 5 times with deionized water, vacuum at 120 DEG C
It is dried 10h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 6
Preparation 2mol/L potassium hydroxide, decanone mixed liquor, heating in water bath, react 24h at 50 DEG C, add appropriate concentrated hydrochloric acid,
By its pH regulator to neutral, centrifugation 10min under 10000r/min rotating speed, clean 5 times, at 120 DEG C with deionized water
Lower vacuum drying 10h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 7
Preparation 10mol/L potassium hydroxide, acetone soln, room temperature standing and reacting 72h, add appropriate concentrated hydrochloric acid, its pH is adjusted
Joint, to neutral, centrifugation 10min under 10000r/min rotating speed, cleans 5 times with deionized water, is vacuum dried at 120 DEG C
10h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 8
Preparation 1mol/L sodium hydroxide, methyl n-undecyl ketone mixed liquor, heating in water bath, reacts 12h, adds appropriate at 100 DEG C
Concentrated hydrochloric acid, by its pH regulator to neutral, centrifugation 10min under 10000r/min rotating speed, cleans 5 times with deionized water,
At 120 DEG C, it is vacuum dried 10h, obtains the carbon quantum dot solid of uniform particle sizes.
Embodiment 9
The 1-Phenylethanone. mixed liquor of preparation 3mol/L potassium hydroxide, room temperature standing and reacting 120h, add appropriate concentrated hydrochloric acid, by its pH
Regulation, to neutral, centrifugation 10min under 10000r/min rotating speed, is cleaned 5 times with deionized water, and at 150 DEG C, vacuum is done
Dry 8h, obtains the carbon quantum dot solid of uniform particle sizes.
The ketone selected in the embodiment of the present invention is that carbon number is more than or equal to 3, monoketone less than or equal to 15, diketone,
Polyketones, such as acetone, methyl ethyl ketone (2-butanone), methyl propyl ketone (2 pentanone), diethyl ketone (propione), 2-
Hexanone, Ketohexamethylene, 2-heptanone, cycloheptanone, methyln-hexyl ketone, cyclooctanone, methyl n-heptyl ketone, decanone, undecyl ketone, ten diketone, ten triketones,
One or more in ten tetrones, 15 ketone, 1-Phenylethanone., methyl acetophenone；Alkali includes: Lithium hydrate, potassium hydroxide, hydrogen
Sodium oxide, phosphate, carbonate, ammonia etc..
Claims (10)
1. the method that under the conditions of an alkalescence, carbon quantum dot is prepared in ketone carbonization, it is characterised in that preparation alkali and ketone mixed
Close liquid, standing and reacting or low-temperature heat reaction, generate carbon quantum dot, through hydrochloric acid neutralization, centrifugation, cleaning,
It is dried to obtain carbon quantum dot solid.
Method the most according to claim 1, it is characterised in that described ketone is that carbon number is more than or equal to 3,
Monoketone, diketone or polyketones less than or equal to 15.
Method the most according to claim 2, it is characterised in that described ketone be acetone, 2-butanone, 2 pentanone,
Propione, methyl-n-butyl ketone, Ketohexamethylene, 2-heptanone, cycloheptanone, methyln-hexyl ketone, cyclooctanone, methyl n-heptyl ketone, decanone,
One or several in undecyl ketone, ten diketone, ten triketones, ten tetrones, 15 ketone, 1-Phenylethanone., methyl acetophenone
Kind.
Method the most according to claim 1, it is characterised in that described alkali be Lithium hydrate, potassium hydroxide,
One or more in sodium hydroxide, phosphate, carbonate.
5. according to the method described in claim 1 or 4, it is characterised in that described alkali concentration in mixed liquor
For 0.1-10mol/L.
6. according to the method described in any one of claim 1-4, it is characterised in that reaction temperature is 15-100 DEG C,
Response time is 12-360h.
Method the most according to claim 6, it is characterised in that reaction temperature is 25-50 DEG C, the response time
For 48-120h.
Method the most according to claim 1, it is characterised in that centrifugation is that 8000-16000r/min is centrifuged
Separate.
Method the most according to claim 1, it is characterised in that described carbon quantum dot is nano-scale.
Method the most according to claim 1, it is characterised in that described be dried into vacuum drying, temperature is
80-150 DEG C, drying time is 4-24h.
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| 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 |
| CN108130049A (en) * | 2018-01-03 | 2018-06-08 | 北京科技大学 | A kind of preparation method of fluorescence phase-change material |
| CN109337682B (en) * | 2018-12-26 | 2020-03-31 | 赵方浩 | Method for preparing fluorescent carbon quantum dots at room temperature |
| CN110028052B (en) * | 2019-05-07 | 2021-02-02 | 中南大学 | Method for preparing hollow structure material based on carbon quantum dot template method |
| CN112871160B (en) * | 2021-01-21 | 2023-09-12 | 中南大学深圳研究院 | Preparation method of three-dimensional porous carbon supported Rh-based catalyst, product and application thereof |
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