Method for preparing sulfur-phosphorus co-doped carbon quantum dots by adopting buckwheat shell as carbon source

A technology of carbon quantum dots, carbon source sulfur phosphorus, applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc. Low quantum yield, unclear luminescence mechanism, etc., to achieve the effect of improved fluorescence performance, uniform size and good biocompatibility

Inactive Publication Date: 2019-11-12
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current research on fluorescent C-Dots nanomaterials is still in its infancy, and there are still some urgent scientific research problems to be solved. For example, the yield and fluorescence quantum yield (QY) of existing synthesis methods are often relatively low, and it is impossible to accurately control its lateral direction. Size and surface chemistry, unclear luminescence mechanism, narrow fluorescence spectral range, etc.

Method used

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  • Method for preparing sulfur-phosphorus co-doped carbon quantum dots by adopting buckwheat shell as carbon source
  • Method for preparing sulfur-phosphorus co-doped carbon quantum dots by adopting buckwheat shell as carbon source
  • Method for preparing sulfur-phosphorus co-doped carbon quantum dots by adopting buckwheat shell as carbon source

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Embodiment 1

[0020] (1) Buckwheat husk powder pretreatment: In the reactor, add 3.0mol / L hydrochloric acid solution: 80mL, potassium periodate: 6g, dissolve, then add buckwheat husk powder: 14g, soak at room temperature for 8h, and then boil After cooling for 30 minutes, wash with deionized water until neutral, separate solid and liquid, then wash with deionized water until neutral, and dry to obtain pretreated buckwheat husk powder;

[0021] (2) Preparation of crude sulfur-phosphorus co-doped carbon quantum dots: Add 1-ethyl-2,3-dimethylimidazolium hexafluorophosphorus salt in a reaction kettle with a polytetrafluoroethylene liner: 66g, pretreated buckwheat husk powder: 26g, thioacetamide: 8g, stir evenly, cover the airtight cover, place in a constant temperature box, keep the temperature at 120±2°C, and react for 25h to obtain a brown viscous transparent liquid, which is Crude sulfur and phosphorus co-doped carbon quantum dots;

[0022] (3) Preparation of sulfur and phosphorus co-doped ...

Embodiment 2

[0024] (1) Buckwheat husk powder pretreatment: In the reactor, add 3.0mol / L hydrochloric acid solution: 79mL, potassium periodate: 5g, dissolve, then add buckwheat husk powder: 16g, soak at room temperature for 8h, and then boil After cooling for 30 minutes, wash with deionized water until neutral, separate solid and liquid, then wash with deionized water until neutral, and dry to obtain pretreated buckwheat husk powder;

[0025] (2) Preparation of crude sulfur-phosphorus co-doped carbon quantum dots: Add 1-ethyl-2,3-dimethylimidazolium hexafluorophosphorus salt in a reaction kettle with a polytetrafluoroethylene liner: 67g, pretreated buckwheat husk powder: 27g, thioacetamide: 6g, stir evenly, cover the airtight cover, place in a constant temperature box, keep the temperature at 120±2°C, and react for 26h to obtain a brown viscous transparent liquid, which is Crude sulfur and phosphorus co-doped carbon quantum dots;

[0026] (3) Preparation of sulfur and phosphorus co-doped ...

Embodiment 3

[0028] (1) Buckwheat husk powder pretreatment: In the reactor, add 3.0mol / L hydrochloric acid solution: 78mL, potassium periodate: 7g, dissolve, then add buckwheat husk powder: 13g, soak at room temperature for 8h, and then boil After cooling for 30 minutes, wash with deionized water until neutral, separate solid and liquid, then wash with deionized water until neutral, and dry to obtain pretreated buckwheat husk powder;

[0029] (2) Preparation of crude sulfur-phosphorus co-doped carbon quantum dots: Add 1-ethyl-2,3-dimethylimidazolium hexafluorophosphorus salt in a reaction kettle with a polytetrafluoroethylene liner: 66g, pretreated buckwheat husk powder: 24g, thioacetamide: 10g, stir evenly, cover the airtight cover, place in a constant temperature box, keep the temperature at 120±2°C, and react for 24h to obtain a brown viscous transparent liquid, which is Crude sulfur and phosphorus co-doped carbon quantum dots;

[0030] (3) Preparation of sulfur and phosphorus co-doped...

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Abstract

The invention discloses a method for preparing sulfur-phosphorus co-doped carbon quantum dots by adopting buckwheat shell as a carbon source. The method is characterized in that buckwheat shell powderis pretreated with hydrochloric acid and a potassium periodate solution to obtain pretreated buckwheat shell powder; then in a reaction vessel with a polytetrafluoroethylene liner, 64-68% by mass of1-ethyl-2,3-dimethylimidazolium hexafluorophosphate, 24-28% by mass of the pretreated buckwheat shell powder and 6-10% by mass of thioamide are added and reacted at a constant temperature of 120 + / - 2DEG C for 24-28 h to obtain brown viscous transparent liquid which is a crude product of the sulfur-phosphorus co-doped carbon quantum dots; purification is performed in a dialysis manner to obtain the sulfur-phosphorus co-doped carbon quantum dots. The method is green and simple to operate, the sulfur-phosphorus co-doped carbon quantum dot composite material can have high fluorescence performance stability, small size and uniformity, good biocompatibility, and other advantages without the need of secondary modification, and the quantum yield of the sulfur-phosphorus co-doped carbon quantum dots is increased by near 88%.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano-luminescent materials, in particular to a preparation method and application of sulfur and phosphorus co-doped carbon quantum dots with buckwheat hulls as carbon source. Background technique [0002] As an emerging nanomaterial, carbon quantum dots (C-Dots) have the advantages of good biocompatibility, non-toxicity, small particle size, adjustable emission spectrum, high fluorescence stability and photobleaching resistance, and the raw materials are cheap. And the characteristics of rich sources, easy preparation and modification make its preparation and application become one of the hot research fields of analytical chemistry in recent years. However, the current research on fluorescent C-Dots nanomaterials is still in its infancy, and there are still some urgent scientific research problems to be solved. For example, the yield and fluorescence quantum yield (QY) of existing synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/70B82Y20/00B82Y30/00B82Y40/00
CPCB82Y20/00B82Y30/00B82Y40/00C09K11/701
Inventor 李慧芝魏琴杨春霞
Owner UNIV OF JINAN
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