Preparation method for dual-emitting fluorescence carbon spot

A technology of dual emission fluorescence and carbon dots, which is applied in the direction of luminescent materials, fluorescence/phosphorescence, chemical instruments and methods, etc., can solve the problems of rare reports of dual emission wavelength fluorescent carbon dots, etc. The effect of mild conditions

Inactive Publication Date: 2018-01-12
SOUTHWEST UNIVERSITY
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Problems solved by technology

[0003] In recent years, great progress has been made in the synthesis of fluorescent carbon dots. At the same time, a variety of new fluorescent carbon dots have aroused the interest of scholars at home and abroad, such as doped fluorescent carbon dots, magnetic fluorescent carbon dots, and long-wavelength fluorescent carbon dots Carbon dots have been reported one after another, but the synthesis of dual emission wavelength fluorescent carbon dots is rarely reported

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  • Preparation method for dual-emitting fluorescence carbon spot
  • Preparation method for dual-emitting fluorescence carbon spot
  • Preparation method for dual-emitting fluorescence carbon spot

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The influence of embodiment 1 raw material ratio on carbon point

[0033] 0.2mmol of 1-(2-pyridylazo)-2-naphthol and corresponding 0, 0.1mmol, 0.2mmol, 0.3mmol, 0.4mmol, 0.5mmol, 0.6mmol, 1.2mmol of copper chloride dihydrate Dissolve in eight centrifuge tubes filled with 10mL of absolute ethanol and sonicate for 20min; then, transfer the mixture to eight 25mL polytetrafluoroethylene reactors, and heat at 180°C for 4h; Cool naturally to room temperature and purify the product through a silica gel column. The eluent is a mixed solution of dichloromethane and methanol at a volume ratio of 40:1. The solvent is evaporated and dried in vacuo to obtain a carbon dot solid.

[0034] The obtained carbon dots were diluted with absolute ethanol to form a carbon dot mother solution with a concentration of 1 mg / mL, 200 μL was taken, and the volume was adjusted to 2 mL with water, and the fluorescence spectrum was measured with an F-7000 fluorescence spectrophotometer. When the excita...

Embodiment 2

[0035] The influence of embodiment 2 solvent on carbon point

[0036] Accurately weigh 0.2mmol of 1-(2-pyridylazo)-2-naphthol and 0.4mmol of copper chloride dihydrate in seven parts respectively, and fill them with 10mL of absolute ethanol, 8mL of absolute ethanol and 2mL of ultrapure Mixed solution of water, mixed solution of 6mL absolute ethanol and 4mL ultrapure water, mixed solution of 5mL absolute ethanol and 5mL ultrapure water, mixed solution of 4mL absolute ethanol and 6mL ultrapure water, 2mL absolute ethanol and 8mL Dissolve the mixed solution of ultrapure water and a centrifuge tube of 10mL ultrapure water and sonicate for 20min; then, transfer the mixed solution to seven 25mL polytetrafluoroethylene reactors respectively, and heat at 180°C for 4h; after the reaction is completed, wait for the reaction The kettle was naturally cooled to room temperature, and the product was purified through a silica gel column. The eluent was a mixed solution of dichloromethane and ...

Embodiment 3

[0038] The influence of embodiment 3 temperature of reaction on carbon point

[0039] In three centrifuge tubes, accurately weigh 0.2mmol of 1-(2-pyridylazo)-2-naphthol and 0.4mmol of copper chloride dihydrate dissolved in 10mL of absolute ethanol and sonicate for 20min; then, the mixed The solution was transferred to three 25mL polytetrafluoroethylene reaction kettles, and heated and reacted at 170°C, 180°C, and 190°C for 4 hours respectively; after the reaction was completed, the reaction kettles were naturally cooled to room temperature, and the product was purified through a silica gel column. It is a mixed solution of dichloromethane and methanol with a volume ratio of 40:1. The solvent is evaporated and vacuum-dried to obtain a carbon dot solid.

[0040] Adopt the method identical with embodiment 1 to obtain its fluorescence spectrogram ( image 3 ), the carbon dots produced at 180°C had the strongest fluorescence peak at 488nm wavelength, and a small amount of product ...

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Abstract

The invention discloses a method for quickly and conveniently preparing a dual-emitting carbon spot. The method comprises the following steps: step (1) weighing 1-(2-pyridine azo)-2-naphthol and copper chloride dihydrate in the mole ratio of 1:(1-3), adding absolute ethyl alcohol and water in the volume ratio of (10-0):(0-10) and ultrasonically dissolving, thereby acquiring a mixed solution; step(2) transferring the mixed solution into an airtight reactor for heating and reacting, wherein the reaction temperature is 170 DEG C-190 DEG C and the reaction time is 3-5h; and step (3) naturally cooling the reaction system to room temperature, performing silicagel column chromatography, removing a solvent and performing vacuum drying, thereby acquiring the carbon spot. The carbon spot prepared by the method has fluorescence emission at 426nm and 488nm wavelength under the excitation of 350nm light; the carbon spot is capable of detecting Fe<3+> according to specific dual signals of fluorescence peaks at the two wavelengths; the method is wide in linear range and low in limit of detection.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing double-emission fluorescent carbon dots. Background technique [0002] Compared with traditional fluorescent dyes, carbon dots, a fluorescent carbon nanomaterial discovered in recent years, have special fluorescent properties, such as adjustable excitation and emission wavelengths, good photostability, and no light flickering phenomenon. Because of the advantages of low toxicity, good biocompatibility and simple preparation, carbon dots are favored by many scholars. and other fields have shown great advantages. [0003] In recent years, the synthesis method of fluorescent carbon dots has made great progress. At the same time, a variety of new fluorescent carbon dots have attracted the interest of scholars at home and abroad. New types of fluorescent carbon dots such as doped fluorescent carbon dots, magnetic fluorescent carbon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65G01N21/64C01B32/15
Inventor 谭克俊朱盼盼
Owner SOUTHWEST UNIVERSITY
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