Preparation method and application of sulfur and nitrogen co-doped carbon quantum dots

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

Active Publication Date: 2020-05-08
NANJING TECH UNIV
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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 and nitrogen co-doped carbon quantum dots
  • Preparation method and application of sulfur and nitrogen co-doped carbon quantum dots
  • Preparation method and application of sulfur and nitrogen co-doped 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, comprising the following steps:

[0028] Mix phenothiazine, sodium nitrite, dichloromethane and acetic acid for 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] The invention mixes phenothiazine, sodium nitrite, dichloromethane and acetic acid for nitration reaction to obtain 3,7-dinitrophenothiazine. In the present invention, the phenothiazine is simultaneously used as a nitrogen source and a sulfur source; the sodium nitrite is a nitrogen source; the dichloromethane is a solvent for phenothiazine; and the acetic acid is a s...

Embodiment 1

[0061] Synthesis of 3,7-dinitrophenothiazine:

[0062]

[0063] Under the condition of stirring, in the mixture of 20.00g phenothiazine (100mmol), 100mL dichloromethane and 40mL acetic acid, slowly add 20.00g sodium nitrite (300mmol), after stirring at room temperature for 1h, then add 100mL dichloromethane, 40mL of acetic acid and 20.00g of sodium nitrite were reacted for 1.5h, and a large amount of solids were formed; then 120mL of dilute acetic acid solution was added to the system, and the stirring was continued for 2h, followed by suction filtration, and washing 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=4Hz, 2H), 7.70 (s, 2H), 7.82 (d, J=4Hz, 2H). HRMS(ESI)m / zC 12 h 8 N 3 o 4 S + (M+H) + Calculated: 290.0230, ...

Embodiment 2

[0069] Synthesis Reference Example 1 of 3,7-dinitrophenothiazine;

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

[0071] Under the condition of ultrasound, 0.3g of 3,7-dinitrophenothiazine was dispersed in 60mL of 1mol / L ammonia solution, kept for 2h to obtain a suspension, and reacted at 200°C for 12h. After the reaction is completed, cool to room temperature, and filter the reaction solution 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. Concentrate the filtrate and perform dialysis with a dialysis bag with a molecular weight cut-off of 500-1000 to remove sodium salts and non-carbonized small molecules, and vacuum-dry to obtain sulfur-nitrogen doped carbon quantum dots, which are designated as D-2. The shape of D-2 is approximately spherical, the particle size distribution range is 1.5-4nm, and the average particle size is 3.1nm;

[0072] Fig...

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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 protection materials, in particular to a carbon quantum dot co-doped with sulfur and nitrogen, a preparation method and application thereof. Background technique [0002] Carbon quantum dots are a kind of dispersed, spherical fluorescent carbon nanoparticles with a size below 10nm. 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 of excitation wavelength, photostability, pH value dependence, etc. Sex, 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 and so on. ...

Claims

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Application Information

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Patent Type & Authority Patents(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 TECH UNIV
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