Preparation method and application of sulfur-nitrogen codoped carbon quantum dots

A carbon quantum dot, co-doping technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc.

Active Publication Date: 2019-02-15
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In recent years, people have begun to study the optical limiting performance of carbon quantum dots, but how to prepare sulfur and nitrogen co-doped carbon quantum dots with excellent optical limiting performance, there is no such thing in the prior art. related reports

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  • Preparation method and application of sulfur-nitrogen codoped carbon quantum dots
  • Preparation method and application of sulfur-nitrogen codoped carbon quantum dots
  • Preparation method and application of sulfur-nitrogen codoped carbon quantum dots

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preparation example Construction

[0027] The invention provides a method for preparing carbon quantum dots co-doped with sulfur and nitrogen, which comprises the following steps:

[0028] Mix phenothiazine, sodium nitrite, dichloromethane and acetic acid to undergo nitration reaction to obtain 3,7-dinitrophenothiazine;

[0029] The 3,7-dinitrophenothiazine and lye are mixed, followed by hydrothermal reaction and dialysis to obtain carbon quantum dots co-doped with sulfur and nitrogen.

[0030] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0031] In the present invention, phenothiazine, sodium nitrite, dichloromethane and acetic acid are mixed to undergo nitration reaction to obtain 3,7-dinitrophenothiazine. In the present invention, the phenothiazine serves as both a nitrogen source and a sulfur source; the sodium nitrite is a nitrogen source; the methylene chloride is a solvent for phenothiazine; and the ...

Embodiment 1

[0061] Synthesis of 3,7-dinitrophenothiazine:

[0062]

[0063] Under stirring conditions, slowly add 20.00g sodium nitrite (300mmol) to a mixture of 20.00g phenothiazine (100mmol), 100mL dichloromethane and 40mL acetic acid. After stirring at room temperature for 1 hour, add 100mL dichloromethane. 40mL of acetic acid and 20.00g of sodium nitrite were reacted for 1.5h, and a large amount of solid was formed; then 120mL of acetic acid diluted solution was added to the system, and the stirring was continued for 2h, then suction filtered, washed with ethanol and water three times. Then the obtained solid was dissolved in DMF at 100°C, filtered while hot, and the filter cake was the product. The filter cake was washed with ethanol and dried to obtain purple-red 3,7-dinitrophenothiazine (yield 86%). 1 HNMR(400MHz; DMSO-d 6 ): 6.69 (d, J=4 Hz, 2H), 7.70 (s, 2H), 7.82 (d, J=4 Hz, 2H). HRMS(ESI)m / zC 12 H 8 N 3 O 4 S + (M+H) + Calculated value: 290.0230, measured value: 290.0245. Element...

Embodiment 2

[0069] Reference Example 1 for the synthesis of 3,7-dinitrophenothiazine;

[0070] Synthesis of carbon quantum dots co-doped with sulfur and nitrogen:

[0071] Under ultrasonic conditions, 0.3 g of 3,7-dinitrophenothiazine was dispersed in 60 mL of 1 mol / L ammonia solution and kept for 2 h to obtain a suspension, which was reacted at 200° C. for 12 h. After the reaction is completed, it is cooled to room temperature, and the reaction solution is filtered with a filter membrane with a pore size of 0.22 microns to remove large particles of water-insoluble carbon materials and some unreacted raw materials. After concentrating the filtrate, it is dialyzed with a dialysis bag with a molecular weight cut-off of 500-1000 to remove sodium salt and small molecules that are not carbonized, and vacuum-dried to obtain sulfur-nitrogen-doped carbon quantum dots, denoted as D-2. The morphology of D-2 is approximately spherical, the distribution range of particle size is 1.5-4nm, and the average ...

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Abstract

The invention provides a preparation method of sulfur-nitrogen codoped carbon quantum dots. The preparation method comprises the following steps: mixing phenothiazine, sodium nitrite, dichloromethaneand acetic acid, and performing a nitration reaction to obtain 3,7-dinitrophenothiazine; mixing the 3,7-dinitrophenothiazine and alkaline liquid, sequentially performing a hydrothermal reaction and dialysis to obtain sulfur-nitrogen codoped carbon quantum dots. According to the preparation method, firstly, nitrification is performed on a nitrogen source and a sulfur source, so that the nitrogen content of the carbon quantum dots can be increased; then, the 3,7-dinitrophenothiazine and the alkaline liquid are mixed, and the hydrothermal reaction is performed to obtain the sulfur-nitrogen dopedcarbon quantum dots. The carbon quantum dots have the nitrogen content of 3.45-9.69wt% and the sulfur content of 0.51-0.83wt%, show very strong nonlinear scattering performance and have very good optical limiting performance.

Description

Technical field [0001] The invention relates to the technical field of laser protective materials, in particular to a carbon quantum dot co-doped with sulfur and nitrogen, and a preparation method and application thereof. Background technique [0002] Carbon quantum dots are dispersed, spherical-like fluorescent carbon nanoparticles with a size below 10 nm. Compared with other fluorescent nanoparticles, carbon quantum dots not only have the advantages of good biocompatibility and easy functionalization of the surface, but also have many excellent photophysical characteristics: dependence on excitation wavelength, light stability, and pH dependence. Characteristic, electrochemiluminescence, strong absorption in the ultraviolet region, and up-conversion fluorescence properties. The above-mentioned excellent properties make carbon quantum dots have important application value in the fields of biological detection, biosensing, fluorescent probes, medicine, photocatalysis, etc. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65B82Y20/00B82Y30/00
CPCB82Y20/00B82Y30/00C09K11/65
Inventor 刘睿朱森强朱红军胡锦阳黎杨陆佳鹏宋广亮
Owner NANJING UNIV OF TECH
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