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A preparation method and application of fluorescent sulfur-doped nitrogen dots

A technology of sulfur doping and fluorescence, which is applied in the field of preparation of fluorescent sulfur-doped nitrogen dots, can solve the problems of increasing the formation mechanism of carbon dots and the difficulty of active sites, inability to effectively control the reaction process, and insufficient reaction raw materials. The effect of changing optoelectronic properties, narrow particle size distribution, and strong photostability

Active Publication Date: 2019-09-10
SUN YAT SEN UNIV
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Problems solved by technology

Heteroatom-doped carbon dots exhibit excellent photoelectric properties and broad application prospects, but their synthesis generally requires high temperature or strong acid treatment, harsh synthesis conditions, and troublesome post-processing; and the precursor components for preparing carbon dots are complex and the reaction raw materials are insufficient. Single, unable to effectively control the reaction process; in addition, the content of heteroatoms such as nitrogen and sulfur in these carbon dots is not high, and it is mainly heteroatom modification on the surface of carbon dots. difficulty

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  • A preparation method and application of fluorescent sulfur-doped nitrogen dots
  • A preparation method and application of fluorescent sulfur-doped nitrogen dots
  • A preparation method and application of fluorescent sulfur-doped nitrogen dots

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preparation example Construction

[0035] The invention discloses a preparation method and application of fluorescent sulfur-doped nitrogen dots. The preparation method comprises the following steps:

[0036] S1: Preparation of 2-azidothiazole, the synthetic route is as follows:

[0037]

[0038] S2: dissolving the 2-azidothiazole prepared in step S1 in methanol or ammonia water, performing a microwave heating reaction, and removing the solvent by rotary evaporation after the reaction, to obtain a dry crude product;

[0039] S3: Disperse the dry crude product obtained in step S2 in ultrapure water, centrifuge at a speed of 10,000r / min for 20min, discard the large particles in the lower layer, collect the supernatant, and pass the supernatant through a 0.2μm filter membrane , to obtain the filtrate;

[0040] S4: Concentrate the filtrate prepared in step S3, and freeze-dry to obtain fluorescent sulfur-doped nitrogen dots in the shape of fleshy floss solid.

Embodiment 1

[0042] see figure 1 , which is a schematic diagram of the synthesis of fluorescent sulfur-doped nitrogen dots of the present invention. The preparation method of fluorescent sulfur-doped nitrogen dots of the present invention comprises the following steps:

[0043] Step S1: Preparation of 2-azidothiazole: Weigh 4.09 g of 2-aminothiazole into a reaction flask, add 32 mL of hydrochloric acid with a concentration of 5.0 mol / L, and stir and add 48 mL of sodium nitrite aqueous solution in an ice-water bath, The mass of sodium nitrite is 2.77g; add 16.3mL sodium azide aqueous solution, wherein the mass of sodium azide is 2.66g; react at room temperature for 2h. After the reaction, extract with water and saturated sodium chloride, collect the organic layer, then dry the organic layer with anhydrous sodium sulfate, and rotary evaporate under reduced pressure to obtain 2-azidothiazole.

[0044] Step S2: Weigh 1.0 g of the 2-azidothiazole prepared in step S1 and dissolve it in 100 mL ...

Embodiment 2

[0048] This example is roughly the same as Example 1, except that the reagents used to synthesize fluorescent sulfur-doped nitrogen dots are different. The method for preparing fluorescent sulfur-doped nitrogen dots described in this example includes the following steps:

[0049] Step S1: Preparation of 2-azidothiazole: Weigh 4.09 g of 2-aminothiazole into a reaction flask, add 32 mL of hydrochloric acid with a concentration of 5.0 mol / L, and stir and add 48 mL of sodium nitrite aqueous solution in an ice-water bath, The mass of sodium nitrite is 2.77g; add 16.3mL sodium azide aqueous solution, wherein the mass of sodium azide is 2.66g; react at room temperature for 2h. After the reaction, extract with water and saturated sodium chloride, collect the organic layer, then dry the organic layer with anhydrous sodium sulfate, and rotary evaporate under reduced pressure to obtain 2-azidothiazole. .

[0050] Step S2: Weigh 1.0 g of the 2-azidothiazole prepared in step S1 and dissol...

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Abstract

The invention relates to a preparation method and an application of fluorescence sulfur doped nitrogen dots. The preparation method of the fluorescence sulfur doped nitrogen dots comprises the following steps: 1, preparing 2-azidothiazole; 2, dissolving the 2-azidothiazole prepared in step 1 in a solvent, carrying out a microwave heating reaction, and removing the solvent after the reaction ends to obtain a crude dried product; 3, dispersing the crude dried product prepared in step 2 in water, centrifuging the obtained solution, collecting the obtained supernatant, and allowing the supernatant to go through a filter membrane in order to obtain a filtrate; and 4, concentrating the filtrate obtained in step 3, and carrying out freeze drying to obtain the fluorescence sulfur doped nitrogen dots. The fluorescence sulfur doped nitrogen dots, prepared by adopting the 2-azidothiazole as a precursor through the preparation method of the fluorescence sulfur doped nitrogen dots, has the advantages of rich nitrogen content and high doped sulfur content. The method is simple and has good reappearance.

Description

technical field [0001] The invention relates to the field of preparation and application of quantum dots, in particular to a preparation method and application of fluorescent sulfur-doped nitrogen dots. Background technique [0002] Fluorescent materials have always been widely concerned in the fields of materials science, chemistry and life sciences, and their application research in luminous bodies and analysis and detection has made great progress. Efficiently preparing fluorescent materials and studying their optical properties and applications is one of the main development directions of analytical chemistry and material science. [0003] The emergence of carbon dots has further promoted the development of fluorescent materials and expanded the application range of carbon-based materials in the fields of chemistry, materials, and life. However, the currently synthesized carbon dots still have problems such as low fluorescence quantum yield, few active sites, and poor s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/56B82Y20/00B82Y40/00G01N21/64
Inventor 李攻科唐志姣胡玉玲
Owner SUN YAT SEN UNIV
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