CN107572501B - Preparation method of high-yield carbon quantum dots - Google Patents
Preparation method of high-yield carbon quantum dots Download PDFInfo
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- CN107572501B CN107572501B CN201710895607.4A CN201710895607A CN107572501B CN 107572501 B CN107572501 B CN 107572501B CN 201710895607 A CN201710895607 A CN 201710895607A CN 107572501 B CN107572501 B CN 107572501B
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Abstract
The invention discloses a preparation method of a high-yield carbon quantum dot. The method comprises the following steps: dispersing yeast powder in water, and ultrasonically mixing uniformly to obtain a yeast powder suspension; transferring the yeast powder suspension to a reaction kettle, and sealing; reacting at 120-200 ℃ for 4-36 h, naturally cooling to room temperature, filtering and collecting filtrate; and drying the filtrate to obtain the carbon quantum dots. The invention adopts filtration to further optimize and purify, effectively removes unreacted macromolecules and has simple and convenient treatment. The prepared carbon quantum dots have high yield, excellent dispersibility, water solubility and strong fluorescence, and can realize large-scale production and industrial application in the aspects of absorption, fluorescence and the like. The method adopts a hydrothermal method to prepare the carbon quantum dots, uses water as a solvent, is green and environment-friendly, has simple process, realizes the preparation of the carbon quantum dots in one step, has simple required equipment, easy operation, easy realization of process conditions, low production cost and wide application range, and is beneficial to industrial popularization.
Description
Technical field
The invention belongs to field of functional materials, in particular to a kind of preparation method of high yield carbon quantum dot.
Background technique
Carbon quantum dot not only has similar optics special as a kind of novel fluorescent material with traditional semiconductor-quantum-point
Property, also there is good biocompatibility and biological hypotoxicity, therefore in light absorption, biomedicine, sensing, photoelectric device and essence
Refining the fields such as work has huge application prospect.With the continuous deepening of research, the quantum efficiency of carbon quantum dot has reached
90% or more, however, preparing, yield is but still lower, significantly limits the industrial applications of carbon quantum dot.
At present, it has been reported that carbon dots synthetic method following two can be divided into according to synthetic method, one is from top to bottom
Synthetic method, another kind are synthetic methods from bottom to top.Synthetic method is usually by the carbon material of macromolecule (including stone from top to bottom
Ink, carbon nanotube, carbon fiber etc.) it is split or decomposes to prepare carbon quantum dot by physics or chemical means.Mainly
Including electrochemical synthesis, hydrothermal/solvent thermal synthesis method, metal-graphite graft process, arc discharge method, laser ablation method, nanometer
Photoetching technique etc..Method is usually to use the polymer of small organic molecule and small-molecular-weight as presoma from bottom to top, in high temperature item
The carbonization of part core and surface modification, to form carbon quantum dot.A variety of methods have had been established to make small organic molecule in researcher
Above-mentioned dehydrating condensation and carbonisation can be carried out simultaneously, and such method has Microwave-assisted synthesis method, hydro-thermal method, enhancing water respectively
Thermal method (microwave-hydro-thermal method and plasma-hydro-thermal method), strong acid pyrolysismethod, combustion method and microreactor auxiliary carbonization etc..This
Although a little methods are widely used in laboratory research carbon quantum dot, but the above-mentioned method being related to is due to its preparation process complexity
Generally it is lower than 30% [Zhang J, et al.Advanced Science, 2015.2 (4): p.1500002], no with yield is prepared
Meet environmentally protective and economic benefit and limits its production industrially.Exist in actual production economic benefit it is low lack
It falls into, the large-scale production of carbon quantum dot is limited, to hinder the practical application of carbon quantum dot.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the purpose of the present invention is to provide a kind of high yield carbon quantum dots
Preparation method.The preparation method directly synthesizes carbon quantum dot using yeast powder as raw material, by one step hydro thermal method.It is existing for solving
There is the problems such as carbon quantum dot preparation process complexity, expensive starting materials, low yield in technology.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of high yield carbon quantum dot, comprising the following steps:
(1) yeast powder is dispersed in water, ultrasound mixes, and obtains yeast powder suspension；
(2) yeast powder suspension described in step (1) is transferred in reaction kettle, is sealed；4 are reacted in 120~200 DEG C
~36h, cooled to room temperature, filtering and collecting filter liquid；
(3) gained filtrate in step (2) is dried to obtain carbon quantum dot.
Further, the concentration of yeast powder suspension described in step (1) is 15~100g/L；Preferably 26.7g/L.
Further, reaction kettle described in step (2) is polytetrafluoroethyllining lining reaction kettle.
Further, it is water phase filter that filtering, which uses, described in step (2).
Further, drying means described in step (3) is -40 DEG C of freeze-dryings.
Further, the yield of carbon quantum dot obtained in step (3) is 34.94%~65.80%, and quantum efficiency is
3.02%~13.68%.
A kind of carbon quantum dot is prepared by above-mentioned preparation method.
The carbon quantum dot can be applied leads in light absorption, biomedicine, sensing, photoelectric device and fine chemistry industry etc.
Domain.
The present invention has the following advantages and effects with respect to the prior art:
(1) present invention prepares carbon quantum dot using hydro-thermal method, and solvent for use is water, and method is environmentally protective.
(2) present invention advanced optimizes purification to income approach using filtering, effectively eliminates unreacted macromolecular,
And processing is easy.The carbon quantum dot of preparation has high yield, and excellent dispersibility, water-soluble and strong fluorescence is, it can be achieved that carbon
Quantum dot large-scale production and absorb in terms of industrial applications.
(3) present invention process is simple, and a step is to realize the preparation of carbon quantum dot, and required instrument and equipment is simple, is easy to grasp
Make, process conditions are easily achieved, and production cost is low, are had a wide range of application, and industrialization promotion is conducive to.
Detailed description of the invention
Fig. 1 is picture of the carbon quantum dot aqueous solution of the preparation of embodiment 1 under daylight (left side) and ultraviolet light (right side) irradiation.
Fig. 2 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment 1.
Fig. 3 is the grain size distribution of carbon quantum dot prepared by embodiment 1.
Fig. 4 is ultraviolet-visible absorption spectroscopy and the excitation, emission spectrum of carbon quantum dot prepared by embodiment 1.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Yeast powder used in embodiment is purchased from Angel Yeast Co., Ltd.
Embodiment 1
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 200 DEG C of reaction 8h, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
53.12%, quantum efficiency 10.53%.
Fig. 1 is picture of the carbon quantum dot aqueous solution of the preparation of embodiment 1 under daylight (left side) and ultraviolet light (right side) irradiation.By
As can be seen that carbon quantum dot obtained in the present embodiment shows strong blue-fluorescence under the ultraviolet light irradiation of 365nm in figure.
Fig. 2 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment 1.As can be seen from Figure, interplanar distance is
0.24nm, corresponding graphite (1120) crystal face.
Fig. 3 is the grain size distribution of carbon quantum dot prepared by embodiment 1.As can be seen from Figure, the carbon quantum dot of acquisition
Average grain diameter is about 3.6nm.
Fig. 4 is ultraviolet-visible absorption spectroscopy and the excitation, emission spectrum of carbon quantum dot prepared by embodiment 1.The result shows that
Optimal absorption wavelength is 340nm, launch wavelength 420nm.
Embodiment 2
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 120 DEG C of reaction 4h, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
34.99%, quantum efficiency 3.02%.
Embodiment 3
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 140 DEG C of reaction 6h, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
49.18%, quantum efficiency 4.04%.
Embodiment 4
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 160 DEG C of reaction 12h, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
64.58%, quantum efficiency 5.16%.
Embodiment 5
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 180 DEG C of reactions for 24 hours, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
45.29%, quantum efficiency 8.90%.
Embodiment 6
0.8g yeast powder is dispersed in 30mL deionized water, ultrasonic 5min obtains yeast powder suspension, yeast powder is hanged
Supernatant liquid is transferred in reaction kettle, is warming up to 200 DEG C of reaction 36h, cooled to room temperature.Product miillpore filter is isolated
Carbon quantum dot can be obtained after -40 DEG C of freeze-dryings in gained filtrate by brown filtrate.The yield of obtained carbon quantum dot is
34.94%, quantum efficiency 13.68%.
Above embodiments explanation, the present invention provides a kind of methods of carbon quantum dot high yield preparation.The preparation method
Using yeast powder as raw material, carbon quantum dot is directly synthesized by one step hydro thermal method.It is prepared for solving carbon quantum dot in the prior art
The problems such as complex process, expensive starting materials, low yield.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of high yield carbon quantum dot, it is characterised in that the following steps are included:
(1) yeast powder is dispersed in water, ultrasound mixes, and obtains yeast powder suspension；
(2) yeast powder suspension described in step (1) is transferred in reaction kettle, is sealed；In 120~200 DEG C reaction 4~
36h, cooled to room temperature, filtering and collecting filter liquid；
(3) gained filtrate in step (2) is dried to obtain carbon quantum dot.
2. the preparation method of high yield carbon quantum dot according to claim 1, it is characterised in that:
The concentration of yeast powder suspension described in step (1) is 15~100g/L.
3. the preparation method of high yield carbon quantum dot according to claim 1, it is characterised in that:
Reaction kettle described in step (2) is polytetrafluoroethyllining lining reaction kettle.
4. the preparation method of high yield carbon quantum dot according to claim 1, it is characterised in that:
It is water phase filter that filtering, which uses, described in step (2).
5. the preparation method of high yield carbon quantum dot according to claim 1, it is characterised in that:
Drying means described in step (3) is -40 DEG C of freeze-dryings.
6. the preparation method of high yield carbon quantum dot according to claim 1, it is characterised in that:
The yield of carbon quantum dot obtained in step (3) be 34.99%~65.80%, quantum efficiency be 3.02%~
13.68%.
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