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A method for preparing sulfur- and nitrogen-doped carbon quantum dots through separation on a column and applications

A technology of carbon quantum dots and nitrogen doping, applied in the field of chemical analysis and detection, can solve the problems of limiting the application of carbon quantum dots, incompatibility with organic solvents to form anti-counterfeiting ink, etc., and achieves easy identification, easy anti-counterfeiting processing, high fluorescence characteristics Effect

Active Publication Date: 2017-12-15
KUNMING UNIV OF SCI & TECH
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  • Description
  • Claims
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Problems solved by technology

The carbon quantum dots prepared at present are all water-soluble, which brings inevitable shortcomings to the subsequent anti-counterfeiting applications. They cannot be compatible with organic solvents to form anti-counterfeiting inks, and the anti-counterfeiting marks dissolve when exposed to water, which limits the use of carbon quantum dots in anti-counterfeiting. field application

Method used

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  • A method for preparing sulfur- and nitrogen-doped carbon quantum dots through separation on a column and applications
  • A method for preparing sulfur- and nitrogen-doped carbon quantum dots through separation on a column and applications
  • A method for preparing sulfur- and nitrogen-doped carbon quantum dots through separation on a column and applications

Examples

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Effect test

Embodiment 1

[0027] 1. Preparation of sulfur- and nitrogen-doped carbon quantum dot solution: Weigh 10 g of poly(sodium p-styrene sulfonate) and 5 g of o-phenylenediamine, add it to 500 mL of ultrapure water, and sonicate for 10 min to form a colorless and transparent solution. It was transferred to a polytetrafluoroethylene reactor, heated at 220 °C for 10 hours, and after natural cooling, it was first filtered with a 0.22 μm filter membrane, and then dialyzed with a dialysis bag with a molecular weight cut-off of 3500 Da for 24 hours to obtain water-soluble sulfur and nitrogen doped Heterofluorescent carbon quantum dots;

[0028] 2. Separation of carbon quantum dots:

[0029] (1) Wet packing: 15g of 200-300 mesh silica gel is mixed with 75mL of ethyl acetate, ultrasonicated for 5min, and stirred continuously to remove air bubbles, and packed in a chromatographic column with an inner diameter of 24mm, and the height of the silica gel column is about 10cm;

[0030] (2) Sample loading: The...

Embodiment 2

[0036] 1. Preparation of sulfur and nitrogen doped carbon quantum dot solution: Weigh 15g of poly(sodium p-styrene sulfonate) and 8g of o-phenylenediamine, add it to 500mL of ultrapure water, and ultrasonicate for 15min to form a colorless and transparent solution. It was transferred to a polytetrafluoroethylene reaction kettle, heated at 250 °C for 10 hours, and after natural cooling, it was first filtered with a 0.22 μm filter membrane, and then dialysis treatment was carried out with a dialysis bag with a molecular weight cut-off of 3000 Da for 24 hours to obtain water-soluble sulfur and nitrogen doped Heterofluorescent carbon quantum dots;

[0037] 2. Separation of carbon quantum dots:

[0038] (1) Mix 15g of 200-300 mesh silica gel with 105mL of ethyl acetate, sonicate for 10min, and keep stirring to remove air bubbles, and pack it into a 24mm inner diameter chromatography column;

[0039] (2) Sample loading: The water-soluble sulfur and nitrogen-doped fluorescent carbon...

Embodiment 3

[0046] 1. Preparation of sulfur- and nitrogen-doped carbon quantum dot solution: Weigh 12 g of poly(sodium p-styrene sulfonate) and 10 g of o-phenylenediamine, add it to 500 mL of ultrapure water, and ultrasonicate for 12 minutes to form a colorless and transparent solution. It was transferred to a polytetrafluoroethylene reactor, heated at 230°C for 10h, and after natural cooling, filtered with a 0.22μm filter membrane, and then dialysis treatment with a dialysis bag with a molecular weight cut-off of 3200Da for 24h to obtain water-soluble sulfur, nitrogen-doped Heterofluorescent carbon quantum dots;

[0047] 2. Separation of carbon quantum dots:

[0048] (1) Mix 15g of 200-300 mesh silica gel with 150mL of ethyl acetate, sonicate for 8min, and keep stirring to remove air bubbles, and pack into a 24mm inner diameter chromatography column;

[0049] (2) Sample loading: The water-soluble sulfur- and nitrogen-doped fluorescent carbon quantum dot solution was first vacuum-dried a...

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Abstract

A method for preparing sulfur- and nitrogen-doped carbon quantum dots through separation on a column is disclosed. Poly(sodium-p-styrenesulfonate) and o-phenylenediamine are adopted as a carbon source, a nitrogen source and a sulfur source, the sulfur- and nitrogen-doped carbon quantum dots are synthesized by a hydrothermal process and are subjected to chromatographic separation by adopting a silica gel column, and fluorescent quantum dots having different polarity and different colors are collected. The fluorescent quantum dots having low polarity are used for fake prevention of paper or package materials. Through designed colorless transparent patterns such as patterns, characters, quick-response codes, and the like, specific fluoresce appears under excitation by ultraviolet light having a certain wavelength, and can be used as anti-fake marks. The method has an advantage that the prepared carbon quantum dots are insoluble in water so that a water solubility issue of the carbon quantum dots is solved, and an advantage that the carbon quantum dots obtained can show different colors under ultraviolet irradiation and have specific advantages in anti-fake mark recognition.

Description

technical field [0001] The invention relates to the technical field of chemical analysis and detection, in particular to a column separation preparation method of sulfur and nitrogen doped carbon quantum dots and its application in anti-counterfeiting marks. Background technique [0002] In today's rapidly increasing amount of information, the security and accurate identification of information has become a topic of widespread concern in the society; especially with the increasing prosperity of the commodity economy and the continuous development of science and technology, anti-counterfeiting has become a new and constantly developing field. At present, anti-counterfeiting labels are often printed on the surface of the product, that is, paper-based fluorescent anti-counterfeiting, and the printing ink used has a certain color. In order to improve the appearance of the product, the manufacturer has to choose the same color as the fluorescent substance. Packaging materials, wh...

Claims

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Application Information

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IPC IPC(8): C09K11/65G06K19/06
CPCG06K19/06037G06K19/0614C09K11/65
Inventor 杨亚玲华建豪赵纯希
Owner KUNMING UNIV OF SCI & TECH
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