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Preparation method for m-chlorophenol source hyper-fluorescent carbon dots

A technology for carbon quantum dots and m-chlorophenol, which is applied in the field of solvothermal preparation of fluorescent carbon dots, can solve the problems of high cost, long time for photocatalytic degradation of m-chlorophenol, incomplete mineralization, etc. The effect of promoting value and conditions that are easy to control

Inactive Publication Date: 2016-02-24
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a method for preparing m-chlorophenol-derived high-fluorescence carbon quantum dots to overcome the defects of long time-consuming photocatalytic degradation of m-chlorophenol, high cost and incomplete mineralization

Method used

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  • Preparation method for m-chlorophenol source hyper-fluorescent carbon dots
  • Preparation method for m-chlorophenol source hyper-fluorescent carbon dots
  • Preparation method for m-chlorophenol source hyper-fluorescent carbon dots

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Embodiment 1

[0021] Weigh 0.2g of m-chlorophenol, disperse in 20mL of methanol and water mixed solvent with a volume ratio of 3:7, and disperse evenly under stirring or ultrasonic conditions; In the reaction axe, nitrogen was passed to remove dissolved oxygen for 1 hour; heated in an oven at 170°C for 10 hours and then naturally cooled to room temperature, the reaction solution in the liner was taken out and centrifuged at 10,000 rpm for 10 minutes to remove large particles; The unreacted precursor was extracted three times with methane to obtain purified highly fluorescent carbon quantum dots.

[0022] figure 1 It is a characterization diagram of carbon quantum dots obtained in Example 1. figure 1 A is the transmission electron microscope image of carbon quantum dots, which shows that carbon quantum dots are spherical uniform monodisperse particles with uniform size distribution. figure 1 B is the infrared spectrum of carbon quantum dots. It can be seen from the figure that there are a ...

Embodiment 2

[0025] Weigh 0.3g of m-chlorophenol, disperse in 20mL of mixed solvent of methanol and water with a volume ratio of 1:1, and disperse evenly under stirring or ultrasonic conditions; transfer the solution to a 30mL polytetrafluoroethylene liner In the high-pressure reaction axe, nitrogen was passed to remove dissolved oxygen for 1 hour; heated in an oven at 190°C for 12 hours and cooled to room temperature naturally, the reaction solution in the liner was taken out, and centrifuged at 10,000 rpm for 10 minutes to remove large particles; finally, 2 times the volume of Dichloromethane extracted the unreacted precursor 4 times to obtain purified highly fluorescent carbon quantum dots.

Embodiment 3

[0027] Weigh 0.1g of m-chlorophenol, disperse in 20mL of mixed solvent of methanol and water with a volume ratio of 1:2, and disperse evenly under stirring or ultrasonic conditions; In the reaction axe, remove dissolved oxygen by blowing nitrogen for 1 hour; heat in an oven at 180°C for 11 hours; cool naturally to room temperature, take out the reaction liquid in the liner, and centrifuge at 10,000 rpm for 10 minutes to remove large particles; use 2 times the volume of dichloro Methane extracted the unreacted precursor twice to obtain purified highly fluorescent quantum carbon dots.

[0028] figure 2 For the quantum yield figure of the carbon quantum dots obtained in Examples 1, 2 and 3, taking quinoline sulfate as a standard, the quantum yields of the three carbon quantum dots are very close, as ～ 17%, indicating that the prepared carbon quantum dots have a higher quantum yield.

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Abstract

The invention discloses a preparation method for m-chlorophenol source hyper-fluorescent carbon dots. The method specifically comprises the following steps: (1), dissolving m-chlorophenol into a mixed solvent of methanol and water, stirring or enabling the mixed liquid to be subjected to ultrasound to obtain a uniform mixed solution, then transferring into an autoclave, and performing constant-temperature heating in an oven of 170 to 190 DEG C for 10 to 12 hours; (2), cooling to the room temperature in a natural way, removing large particles by centrifugation, extracting unreacted m-chlorophenol by using dichloromethane of double volumes twice to four times, so that purified hyper-fluorescent carbon dots are obtained. According to the preparation method, the toxic and harmful substance m-chlorophenol is used as a precursor for preparing the hyper-fluorescent carbon dots for the first time, the poison is successfully turned into the valuable, and a novel thought is provided for the disposal of the supervirulent m-chlorophenol and pesticide residues of this kind. Besides, the prepared carbon dots have the advantages of uniform size distribution, high quantum yield, low toxicity, good biocompatibility and good photostability. Thus, the method has relatively high promotional value.

Description

technical field [0001] The invention belongs to the technical field of fluorescent carbon dots prepared by solvothermal method, and in particular relates to a preparation method of m-chlorophenol source high fluorescent carbon quantum dots. Background technique [0002] In the field of fluorescent nanomaterials, fluorescent carbon quantum dots have attracted more and more attention because of their small particle size, low cost, adjustable emission, low toxicity, and good biocompatibility. The wide selection range of precursors and no special requirement on the purity of precursors is an important factor for the rapid development of fluorescent carbon dots research. At present, it has been reported that the precursors used for the preparation of fluorescent carbon dots are: hair, humus, carbon black, milk, carbohydrates, candle soot, fruit, etc., but there is no method for preparing fluorescent carbon quantum dots using m-chlorophenol as a precursor. reports. [0003] Halo...

Claims

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Application Information

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IPC IPC(8): C09K11/65C01B31/02B82Y20/00B82Y40/00
CPCC09K11/65C01P2002/72C01P2002/82C01P2004/04C01P2004/64C01P2006/60
Inventor 邹文生王亚琴
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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