CN109486486A - A kind of preparation method of the fluorescent carbon quantum dot based on microwave method - Google Patents
A kind of preparation method of the fluorescent carbon quantum dot based on microwave method Download PDFInfo
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- CN109486486A CN109486486A CN201811571932.6A CN201811571932A CN109486486A CN 109486486 A CN109486486 A CN 109486486A CN 201811571932 A CN201811571932 A CN 201811571932A CN 109486486 A CN109486486 A CN 109486486A
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Abstract
The invention discloses a kind of preparation methods of fluorescent carbon quantum dot based on microwave method, comprising the following steps: after Chinese medicine fritillaria freeze-day with constant temperature, pulverizes and sieves；Bulbus and distilled water are added in round-bottomed flask, is put into microwave reactor and stirs and carry out microwave heating treatment, with the extension of time, solution gradually becomes light yellow by colourless, ultimately become brown color, show that fluorescent carbon quantum dot is formed；Removal large granular impurity is filtered and is centrifuged to get brown color fluorescent carbon quantum dot dispersion liquid.Synthetic method instrument and equipment of the invention is simple, and easy control of reaction conditions is easy to operate, and one step of synthesis process is completed, and required time is short, environmentally protective, and the high-volume suitable for fluorescent carbon quantum dot synthesizes.
Description
Technical field
The invention belongs to fluorescent carbon quantum dot preparation fields, specifically, being related to a kind of fluorescence carbon amounts based on microwave method
The preparation method of son point.
Background technique
Fluorescence carbon nanomaterial has been developed in recent years a kind of zero dimension novel fluorescence functional material.As carbon nanometer material
A newcomer in material field, carbon quantum dot (Carbondots, CDs) partial size are generally less than 10nm, have fabulous fluorescence
The features such as performance, strong quantum confinement and edge effect, hypotoxicity and bio-compatibility and excellent luminescent properties.Meanwhile
The advantages that there are also raw material to be easy to get for carbon quantum dot, at low cost, and Preparation equipment is simple and preparation process is controllable, examines it in analysis
It surveys, chemical sensitisation, cell imaging, biomarker, the fields such as photocatalysis and photoelectric component have a wide range of applications.
Currently, the synthetic method of carbon quantum dot is broadly divided into (top-down) from top to bottom and from bottom to top on the whole
(bottom-up) this two major classes.Top-down synthetic method is to obtain carbon amounts using etching or the removing larger carbon material of size
The method of son point, mainly includes arc discharge method, electrochemical oxidation process and laser ablation method etc.；Synthetic method from bottom to top is
The method for obtaining carbon quantum dot using small molecule presoma mainly includes thermal decomposition method, combustion method and microwave method etc..
Summary of the invention
In view of this, the present invention provides a kind of preparation methods of fluorescent carbon quantum dot based on microwave method.
In order to solve the above-mentioned technical problem, the invention discloses a kind of preparation sides of fluorescent carbon quantum dot based on microwave method
Method, comprising the following steps:
Step 1, by after Chinese medicine fritillaria freeze-day with constant temperature, pulverize and sieve；
Bulbus and distilled water is added in step 2 in round-bottomed flask, is put into microwave reactor and stirs and carry out microwave
Heat treatment, with the extension of time, solution gradually becomes light yellow by colourless, ultimately becomes brown color, shows fluorescence carbon amounts
Son point is formed；
Step 3 is filtered and is centrifuged removal large granular impurity to get brown color fluorescent carbon quantum dot dispersion liquid.
Optionally, the freeze-day with constant temperature temperature in the step 1 is 40-50 DEG C, and grit number is 40-80 mesh.
Optionally, the mass volume ratio (g/mL) of the Bulbus in the step 2 and distilled water is 0.25:30-2.00:
30。
Optionally, the mixing time in the step 2 is 25-35min.
Optionally, the microwave heating power in the step 2 is 600-800W, microwave heating time 6-10min.
Optionally, for 0.01~0.45 μm, centrifugal rotational speed is in the aperture for the filter membrane that the filtering in the step 3 uses
8000-12000r/min, centrifugation time 20-30min, centrifugation number are 5 times, use molecular cut off for the dialysis of 3500Da
Bag dialysis 3d.
Compared with prior art, the present invention can be obtained including following technical effect:
1) synthetic method instrument and equipment of the invention is simple, and easy control of reaction conditions is easy to operate, one step of synthesis process
It completes, required time is short, and environmentally protective, the high-volume suitable for fluorescent carbon quantum dot synthesizes.
2) the fluorescent carbon quantum dot average grain diameter 5nm that the present invention is prepared, maximum excitation wavelength 310nm, emission maximum
Wavelength is located at 400nm, uv-absorption maximum wavelength 280nm.
Certainly, it implements any of the products of the present invention it is not absolutely required to while reaching all the above technical effect.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is influence of the Chinese medicine fritillaria dosage of the present invention to synthesis fluorescent carbon quantum dot；
Fig. 2 is influence of the microwave power of the present invention to synthesis fluorescent carbon quantum dot；
Fig. 3 is influence of the reaction time of the invention to synthesis fluorescent carbon quantum dot；
Fig. 4 is the morphology characterization for the fluorescent carbon quantum dot that the embodiment of the present invention 1 is prepared；
Fig. 5 is the Elemental Composition analysis characterization for the fluorescent carbon quantum dot that the embodiment of the present invention 1 is prepared；
Fig. 6 is that the fluorescent carbon quantum dot that the embodiment of the present invention 1 is prepared passes through fluorescence spectrum (A) and ultra-violet absorption spectrum
(B) test of optical property is carried out.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with embodiment, whereby to the present invention how application technology hand
Section solves technical problem and reaches the realization process of technical effect to fully understand and implement.
The invention discloses a kind of preparation methods of fluorescent carbon quantum dot based on microwave method, comprising the following steps:
Chinese medicine fritillaria after freeze-day with constant temperature, crushed 40-80 mesh at 40-50 DEG C by step 1；
Bulbus and distilled water is added in step 2 in round-bottomed flask, wherein the mass body of Bulbus and distilled water
Product is 0.25:30-2.00:30 than (g/mL), is put into microwave reactor and stirs 25-35min, under the power of 600-800W,
Microwave heating 6-10min ultimately becomes brown color with the extension of time, solution gradually becomes light yellow by colourless, shows glimmering
Light carbon quantum dot is formed；
Wherein, as shown in Figure 1, being prepared into when the amount of fritillaria is added in every 30mL distilled water between 0.25~2.00g
To carbon quantum dot fluorescence intensity gradually rise, subsequent fritillaria dosage increases, and carbon quantum dot fluorescence intensity decreases；When every
When addition fritillaria dosage is 2g in 30mL distilled water, the luminous efficiency of obtained fluorescent carbon quantum dot is maximum, fluorescence intensity highest.
As shown in Fig. 2, the carbon quantum dot fluorescence intensity being prepared is gradually when microwave power is between 600~800W
It increases, subsequent microwave power continues to increase, and carbon quantum dot fluorescence intensity reduces instead.When microwave power is 800W, obtain
The luminous efficiency of fluorescent carbon quantum dot is maximum, fluorescence intensity highest.
As shown in figure 3, between when reacted between 4~8min when, the carbon quantum dot fluorescence intensity being prepared gradually rises
Height, when reacted between when reaching 8min, the fluorescence intensity level of fluorescent carbon quantum dot reaches maximum, luminous efficiency highest, with anti-
Continuing growing between seasonable, carbon quantum dot fluorescence intensity level declines instead.
Step 3 is filtered and is centrifuged removal large granular impurity, wherein the aperture of filter membrane is 0.01~0.45 μm, centrifugation
Revolving speed is 8000-12000r/min, centrifugation time 20-30min, and centrifugation number is 5 times, uses molecular cut off for 3500Da
Bag filter dialysis 3d to get brown color fluorescent carbon quantum dot dispersion liquid.
Embodiment 1
A kind of preparation method of the fluorescent carbon quantum dot based on microwave method, comprising the following steps:
Chinese medicine fritillaria after freeze-day with constant temperature, crushed 60 meshes at 45 DEG C by step 1；
Bulbus and distilled water is added in step 2 in round-bottomed flask, wherein the mass body of Bulbus and distilled water
Product is 2.00:30 than (g/mL), is put into microwave reactor and stirs 30min, under the power of 800W, microwave heating 8min, with
The extension of time, solution gradually become light yellow by colourless, ultimately become brown color, show that fluorescent carbon quantum dot is formed；
Step 3 is filtered and is centrifuged removal large granular impurity, wherein the aperture of filter membrane is 0.23 μm, and centrifugal rotational speed is
10000r/min, centrifugation time 25min, centrifugation number are 5 times, and molecular cut off is used to dialyse for the bag filter of 3500Da
3d is to get brown color fluorescent carbon quantum dot dispersion liquid.
The fluorescent carbon quantum dot that the present embodiment 1 is prepared carries out morphology characterization by transmission electron microscope, as shown in figure 4,
The carbon quantum dot soilless sticking phenomenon it can be seen from TEM figure, particle are uniformly dispersed, to be spherical or spherical, in 10nm particle counting
Under, the partial size of fluorescent carbon quantum dot is 4~6nm, average grain diameter 5nm.
The fluorescent carbon quantum dot that the present embodiment 1 is prepared is analysed by Elemental Composition and is characterized, as shown in Figure 5.By XPS
Figure is O (1s), therefore fluorescence carbon quantum at the peak that 532.47eV occurs as can be seen that be C (1s) at the peak that 284.79eV occurs
Point mainly contains carbon and oxygen element.
The fluorescent carbon quantum dot that embodiment 1 is prepared carries out optical property by fluorescence spectrum and ultra-violet absorption spectrum
Research, as shown in Figure 6.Carbon quantum dot sweeps excitation, the maximum excitation of fluorescence nano carbon quantum dot between 290~340nm wavelength
Wavelength is 310nm, shown in Fig. 6 (A).Under the excitation wavelength of 310nm, there is maximum fluorescence at 400nm in fluorescent carbon quantum dot
Emission peak, fluorescent carbon quantum dot by uv-visible absorption spectra test, fluorescent carbon quantum dot 250~300nm section with compared with
Wide absorption band, a length of 280nm of maximum absorption wave.
Embodiment 2
A kind of preparation method of the fluorescent carbon quantum dot based on microwave method, comprising the following steps:
Chinese medicine fritillaria after freeze-day with constant temperature, crushed 80 meshes at 40 DEG C by step 1；
Bulbus and distilled water is added in step 2 in round-bottomed flask, wherein the mass body of Bulbus and distilled water
Product is 0.25:30 than (g/mL), is put into microwave reactor and stirs 35min, under the power of 600W, microwave heating 10min, with
The extension of time, solution gradually become light yellow by colourless, ultimately become brown color, show that fluorescent carbon quantum dot is formed；
Step 3 is filtered and is centrifuged removal large granular impurity, wherein the aperture of filter membrane is 0.01 μm, and centrifugal rotational speed is
12000r/min, centrifugation time 20min, centrifugation number are 5 times, and molecular cut off is used to dialyse for the bag filter of 3500Da
3d is to get brown color fluorescent carbon quantum dot dispersion liquid.
Embodiment 3
A kind of preparation method of the fluorescent carbon quantum dot based on microwave method, comprising the following steps:
Chinese medicine fritillaria after freeze-day with constant temperature, crushed 40 meshes at 50 DEG C by step 1；
Bulbus and distilled water is added in step 2 in round-bottomed flask, wherein the mass body of Bulbus and distilled water
Product is 1.00:30 than (g/mL), is put into microwave reactor and stirs 25min, under the power of 700W, microwave heating 6min, with
The extension of time, solution gradually become light yellow by colourless, ultimately become brown color, show that fluorescent carbon quantum dot is formed；
Step 3 is filtered and is centrifuged removal large granular impurity, wherein the aperture of filter membrane is 0.45 μm, and centrifugal rotational speed is
8000r/min, centrifugation time 30min, centrifugation number are 5 times, use molecular cut off for the bag filter of 3500Da dialysis 3d,
Up to brown color fluorescent carbon quantum dot dispersion liquid.
Above description has shown and described several preferred embodiments of invention, but as previously described, it should be understood that invention is not
It is confined to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification
And environment, and can be carried out within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
Change.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of invention, then it all should be in the appended power of invention
In the protection scope that benefit requires.
Claims (6)
1. a kind of preparation method of the fluorescent carbon quantum dot based on microwave method, which comprises the following steps:
Step 1, by after Chinese medicine fritillaria freeze-day with constant temperature, pulverize and sieve；
Bulbus and distilled water is added in step 2 in round-bottomed flask, is put into microwave reactor and stirs and carry out microwave heating
Processing, with the extension of time, solution gradually becomes light yellow by colourless, ultimately becomes brown color, shows fluorescent carbon quantum dot
It is formed；
Step 3 is filtered and is centrifuged removal large granular impurity to get brown color fluorescent carbon quantum dot dispersion liquid.
2. preparation method according to claim 1, which is characterized in that the freeze-day with constant temperature temperature in the step 1 is 40-50
DEG C, grit number is 40-80 mesh.
3. preparation method according to claim 1, which is characterized in that Bulbus and distilled water in the step 2
Mass volume ratio (g/mL) is 0.25:30-2.00:30.
4. preparation method according to claim 1, which is characterized in that the mixing time in the step 2 is 25-35min.
5. preparation method according to claim 1, which is characterized in that the microwave heating power in the step 2 is 600-
800W, microwave heating time 6-10min.
6. preparation method according to claim 1, which is characterized in that the hole for the filter membrane that the filtering in the step 3 uses
Diameter is 0.01~0.45 μm, centrifugal rotational speed 8000-12000r/min, centrifugation time 20-30min, and centrifugation number is 5 times,
Use molecular cut off for the bag filter of 3500Da dialysis 3d.
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Cited By (1)
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| CN115231551A (en) * | 2022-09-05 | 2022-10-25 | 云南师范大学 | Method for preparing carbon quantum dots by using dimethyl phthalate |
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