CN112852412A - Method for rapidly synthesizing high-fluorescence sulfur quantum dots - Google Patents
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Abstract
The invention provides a method for rapidly synthesizing a strong fluorescent sulfur quantum dot. The preparation method comprises the following steps: adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises protein and water; introducing oxidizing gas into the system, and stirring and reacting under a heating condition; and after the reaction is finished, cooling to room temperature, and performing purification treatment through centrifugation, filtration and dialysis to obtain the sulfur quantum dots. The method for preparing the sulfur quantum dots by oxidizing the oxidizing gas has the advantages of short reaction time, high fluorescence quantum yield, rich surface functional groups, uniform particle size distribution, good water solubility and biocompatibility, high stability and the like, and has great application potential and significance in a plurality of fields.
Description
Technical Field
The invention belongs to the technical field of nano materials, and relates to a method for synthesizing a sulfur quantum dot with strong fluorescence prepared by oxidizing gas and passivating protein.
Background
The sulfur quantum dots are dispersed sphere-like fluorescent sulfur nanoparticles with the size at the nanometer level. The sulfur quantum dots prepared from the sulfur powder and the protein show good chemiluminescence characteristics such as high fluorescence intensity, high light stability, photobleaching resistance, low toxicity and the like, and can be used in various fields such as detection, catalysis, imaging, treatment and the like.
At present, cheap and easily-obtained green and environment-friendly synthetic raw materials and a simple and rapid preparation method are adopted, and the high quantum yield and the red/near-infrared luminescent sulfur quantum dots are required to be further developed and researched. However, to date, there has been only a small amount of research on sulfur quantum dots. Currently, sulfur quantum dots are mainly synthesized by technologies such as an oil-water microemulsion technology, a cystine modified nano sulfur formula and a liquid synthesis method. Compared with the sulfur quantum dots synthesized by the prior art, the quantum yield is lower, and the operation steps of the synthetic reaction are relatively complex and tedious. In recent years, blue light sulfur quantum dots with quantum yield of 3.8% are obtained by simply placing sulfur powder in an alkaline solution for heating and stirring. Although the method can improve the quantum yield of the sulfur quantum dots, the method takes longer time, and the quantum yield still needs to be further improved to be more widely applied.
In view of the problems of low quantum yield, complex preparation and long reaction time of the existing preparation method of the sulfur quantum dots; therefore, a method for rapidly synthesizing the high-fluorescence sulfur quantum dots is urgently needed.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method and application of sulfur quantum dots, the preparation method has the advantages of easily available raw materials, low price and simple preparation method, and can solve the problems of long time consumption, complex operation steps, low fluorescence quantum yield and the like in the prior art for preparing the sulfur quantum dots; the invention has the advantages of green economy, rapid preparation, convenient operation, high fluorescence quantum yield and wide application potential.
The purpose of the invention is realized by the following technical means:
in one aspect, the invention provides a preparation method of a sulfur quantum dot, which comprises the following steps:
step one, adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises protein and water;
transferring the dispersion liquid into a round-bottom flask, introducing oxidizing gas, and reacting for a period of time under heating and stirring;
and step three, cooling to room temperature after the reaction is finished, and carrying out purification treatment through centrifugation, filtration and dialysis to obtain the sulfur quantum dots.
In the preparation method of the sulfur quantum dots, the metal sulfide and the protein are added to synergistically enhance the fluorescence intensity of the sulfur quantum dots and influence the emission wavelength, so that the complicated steps are reduced, and the reaction time is shortened; the raw materials adopted by the invention are green, safe and easily available, the reaction conditions are mild, the requirements on equipment are low, and the prepared sulfur quantum dots have good water solubility, good dispersibility, stable performance and high fluorescence quantum yield.
In the above method, preferably, the mass of the sodium sulfide is 5 to 10 g; further preferably, the mass of the sodium sulfide is 5 g.
In the above method, preferably, the sulfur includes one or more of sublimed sulfur powder, elemental sulfur, sulfur blocks, sulfur granules, and sulfur powder; further preferably, the sulfur is sublimed sulfur powder.
In the above method, the BSA has a mass of 0.05 to 0.1 g; further preferably, the BSA has a mass of 0.1 g.
In the above method, preferably, the ratio of the amounts of the sulfur powder, the sodium sulfide, the BSA, and the water is (0.05 to 1 g): (5-10 g): (0.05-0.10 g): (10-60 mL).
In the above method, preferably, the flow rate of the ozone is 1 to 100 mL/min; further preferably, the flow rate of the ozone is 50 mL/min.
In the above method, preferably, the reaction temperature is 25 to 150 ℃; further preferably, the reaction temperature is 90 ℃.
In the above method, preferably, the prepared sulfur quantum dot further comprises a purification step, specifically:
and centrifuging the sulfur quantum dots, and filtering the obtained supernatant by using a microporous filter membrane or dialyzing by using a dialysis bag to remove impurities to obtain pure sulfur quantum dots.
In the method, preferably, the rotation speed of the sulfur quantum dots for centrifugation is 100-2000 rpm, and the centrifugation time is 0.1-10 h; further preferably, the centrifuge rotation speed is 2000rpm and the centrifugation time is 30 min.
In the above method, preferably, the pore diameter of the microporous filter membrane is 0.22 to 0.45 μm; further preferably, the pore size of the microfiltration membrane is 0.22 μm.
In the method, a dialysis bag with a molecular interception amount of 500-5000 Da is preferably adopted for dialysis; the dialysis time is 24-72 h; further preferably, a dialysis bag with the molecular interception amount of 500-1000 Da is adopted for dialysis; the dialysis time was 24 h.
The invention has the beneficial effects that:
(1) in the preparation method of the sulfur quantum dot, the dispersant BSA is added and the O is introduced3The oxidation can accelerate the reaction time, synergistically enhance the fluorescence intensity of the sulfur spot and change the emission wavelength, and BSA and O are creatively added3The oxidation can synergistically promote the reaction to be carried out more efficiently, so that the complicated steps are reduced, and the reaction time is shortened; the raw materials adopted by the invention are green, safe and easily available, the reaction conditions are mild, the requirements on equipment are low, the prepared sulfur quantum dots have high yield, rich surface functional groups and small size, the particle size distribution is uniform, and water is usedGood solubility and good light stability; the fluorescent material has wide application prospect in the fields of analysis and detection, photocatalysis and disease treatment as a luminescent material.
Drawings
FIG. 1 is a schematic diagram of a transmission electron microscope for synthesizing fluorescent sulfur quantum dots.
FIG. 2 shows the emission intensity and color of sulfur quantum dots irradiated by an ultraviolet lamp at different reaction times.
FIG. 3 wavelength dependent spectral response of sulfur quantum dots at 1.5 and 5 h.
FIG. 4 wavelength dependent spectral response of the sulfur quantum dots at 7 and 10 h.
FIG. 5 xenon lamp irradiation (1W/cm)-2) And testing the light stability of the sulfur quantum dots and the fluorescein sodium.
FIG. 6 shows the sulfur quantum dots to metal ions Hg2+Titration and interference rejection diagrams.
The specific implementation mode is as follows:
the embodiment of the invention provides a method for rapidly synthesizing high-fluorescence sulfur quantum dots, which comprises the following steps:
example 1
At room temperature, 1g of sulfur powder and 5g of Na2S and 0.1g BSA,50mL H2Placing O in a round-bottom flask, and carrying out ultrasonic treatment for 10 min;
(2) setting the reaction temperature at 90 ℃ and the reaction time at 5h, and naturally cooling to room temperature after the reaction is finished.
(3) Centrifugation was performed, and the supernatant was taken. In order to obtain the pure sulfur quantum dots with uniform size distribution and without impurities such as unreacted raw materials and the like, the centrifuged supernatant is filtered for three times through a microporous filter membrane or placed in a dialysis bag for dialysis. And (3) placing the filtrate or the dialysate into a vacuum drying oven for heating, concentrating and drying, wherein the obtained solid sulfur quantum dots can be dissolved in other solvents such as water and the like so as to meet the requirements of different application aspects.
FIG. 1 is a TEM micrograph of the sulfur quantum dots prepared in example 1. As can be seen from figure 1, the sulfur quantum dots obtained by ozone oxidation have small particle size of 3nm and uniform distribution.
FIG. 2 is a graph of the emission of ozone-oxidized sulfur quantum dots under an ultraviolet lamp, as provided in example 1 of the present invention. It can be seen from the figure that the fluorescence intensity of the sulfur quantum dots is stronger and stronger, the fluorescence color is changed from blue to green, and the fluorescence is strongest at the time of 5 h.
FIGS. 3a,3b and FIGS. 4a,4b are fluorescence spectra of the ozonized sulfur quantum dots provided in example 1 of the present invention with reaction times of 1.5, 5h, 7h and 10 h. The spectrogram shows that the sulfur quantum dot has strong fluorescence intensity when the reaction time is 5 hours, the quantum yield is 25 percent, the wavelength is red-shifted, and the emission wavelength is 520 nm.
FIG. 5 is a photo-stability test of the sulfur quantum dots prepared by the invention, and the sulfur quantum dots have good photo-stability as can be seen by comparing with sodium fluorescein.
The sulfur quantum dots obtained by the preparation method and the conditions are used for analyzing and detecting heavy metal ions Hg2+As the concentration increased, fluorescence continued to be quenched and no other metal ions responded significantly, as shown in fig. 6, indicating that it can be used for Hg2+Selective and highly sensitive testing of.
Example 2
The sulfur quantum dots prepared in example 1 were subjected to surface modification treatment. The specific method comprises the following steps:
and (3) adding 100 mu L of hydrazine hydrate into 20mL of sulfur quantum dot solution at room temperature, stirring and reacting for 1h, and performing optical property characterization on the obtained surface-modified sulfur quantum dot to prove that the sulfur quantum dot has the capability of biological imaging.
The modified sulfur quantum dots are used for cell fluorescence imaging, and have high fluorescence quantum yield and good biocompatibility, so that brighter fluorescence signals are displayed in cells.
Example 3
The sulfur quantum dots prepared in example 1 were subjected to surface modification treatment. The specific method comprises the following steps:
at room temperature, 10 μ L of 0.1M glucose oxidase (GOx) was added to 20mL of the sulfur quantum dot solution, and the mixture was stirred for 1 hour to obtain sulfur quantum dots for tumor treatment.
Loaded GOx is able to consume glucose in vivo to produce H2O2To produce the effect of treating hunger.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for rapidly synthesizing strong fluorescent sulfur quantum dots comprises the following steps:
step one, adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises protein and water;
transferring the dispersion liquid into a round-bottom flask, introducing oxidizing gas, and stirring and reacting for a period of time under a heating condition;
and step three, naturally cooling to room temperature after the reaction is finished, and purifying by centrifuging, filtering and dialyzing to obtain the sulfur quantum dots.
2. The method of claim 1, the sulfur powder comprising one or more of sublimed sulfur powder, elemental sulfur, sulfur chunks, sulfur pellets, and sulfur powder; preferably, the sulfur is sublimed sulfur powder.
3. The method of claim 1, wherein the metal sulfide comprises one or more of sodium sulfide, potassium sulfide, magnesium sulfide, zinc sulfide, and the like, preferably the metal sulfide is sodium sulfide.
4. The method of claim 1, wherein the protein comprises one or more of bovine serum albumin, human serum albumin, egg protein, and the like.
5. The method of claim 1, the oxidizing gas being O2、O3、Cl2、Br2And the like.
6. The method according to claim 1, wherein the sulfur powder, the metal sulfide, the protein and the water are used in a ratio of (0.05-1 g): (0.02-0.1 g): (5-10 g): (10-60 mL).
7. The method according to claim 1, wherein the oxidizing gas is introduced at a rate of 1 to 100mL/min, the heating temperature is 25 to 150 ℃, the stirring speed is 100 to 2000rpm, and the reaction time is 0.1 to 10 hours.
8. The method according to claim 1, wherein the prepared sulfur quantum dots further comprise a purification step, in particular: and centrifuging the sulfur quantum dots, and removing impurities from the obtained supernatant by adopting microporous membrane filtration and dialysis bag dialysis to obtain pure sulfur quantum dots.
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ZHENGUANG WANG等: "Two-Step Oxidation Synthesis of Sulfur with a Red Aggregation-", 《COMMUNICATIONS》 * |
白状伟: "层状硫纳米材料的合成及光电特性研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
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