Method for preparing luminescent carbon dots from glycerin

A technology of glycerin and carbon dots, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., to achieve the effects of high yield, simple preparation process, and large output

Inactive Publication Date: 2014-06-04
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the use of concentrated sulfuric acid to directly dehydrate and partially carbonize glycerol to prepare a large number of glycerol-based luminescent carbon dots under conventional methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Install an electric stirrer, a thermometer and a water separation and reflux device on a 250mL three-necked flask, add 42g of glycerin, heat to 115°C under stirring, and slowly add 40ml of concentrated sulfuric acid dropwise under stirring to keep the reaction temperature not exceeding 125°C, then drop the sulfuric acid After the addition, continue to keep the system temperature at 115-125 ° C, react for 1 hour, then dilute with water, filter with suction, wash until the filtrate is neutral, dry and dehydrate the filter cake to obtain a glycerin-based solid carbon material, 12.8 g, the yield is 30.5% of the input amount of glycerin. XPS-photoelectron spectroscopy analysis shows that the carbon, oxygen and sulfur atomic ratios on the surface of the glycerol-based solid carbon material are respectively: 81.45%, 17.72% and 0.82% (CO 0.218 S 0.01 ), its carbon-to-oxygen ratio is smaller than the carbon-to-oxygen atomic ratio of acrolein.

Embodiment 2

[0016] Dissolve 0.2 g of the glycerol-based solid carbon material prepared in Example 1 in 25 mL of 0.4 mol / L sodium hydroxide aqueous solution, adjust the pH value to be close to neutral with dilute hydrochloric acid under stirring, put it into a dialysis bag, and dialyze with water for 24 hours, Sodium chloride and small molecule organic matter are removed to obtain a solution of luminescent carbon dots. According to the fluorescence spectrum analysis, the solution has wide excitation in the wavelength range of 350-470nm, has fluorescence emission in the wavelength range of 460-540nm, and has the strongest emission peak at 492nm at the excitation wavelength of 390nm. The quantum yield was 6.2%. According to XPS-photoelectron spectroscopy analysis, the atomic ratios of sodium carbonate on the solid surface of the glycerol-based luminescent carbon dots are: 80.57%, 17.09% and 2.34%. The average particle size of the carbon dots was 8.7 nm.

Embodiment 3

[0018] React 0.2g of the glycerin-based solid carbon material prepared in Example 1 with 2mL of ethanolamine at 145-185°C for 1 hour, then adjust the pH value to be close to neutral with dilute hydrochloric acid, and dialyze with water to obtain glycerol-based luminescent carbon dots. According to the fluorescence spectrum analysis, the solution has wide excitation in the wavelength range of 330-470nm, has fluorescence emission in the wavelength range of 432-520nm, and has the strongest emission peak at 456nm at the excitation wavelength of 370nm. The quantum yield was 9.7%. The average particle size of the carbon dots was 5.3 nm.

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Abstract

The invention relates to a method for preparing luminescent carbon dots from glycerin. The glycerin based carbon dots prepared by the invention can be used for biological imaging technology and analysis to determine the content of metal ions. The method for preparing luminescent carbon dots from glycerin is as below: heating the glycerol to a certain temperature, slowly dropwise adding concentrated sulfuric acid while stirring, reacting for a certain time, filtering, washing, and removing superfluous sulfuric acid to obtain a glycerin based solid carbon material; and further carrying out alkali dissolution and reaction or ethanol extraction to obtain the glycerin based luminescent carbon dot. The preparation method has the advantages of simple operation, high yield and easiness for preparation of a large amount of carbon dots, and can satisfy the requirement of using glycerin based luminescent carbon dot.

Description

technical field [0001] The invention relates to a method for preparing luminescent carbon dots from glycerin, and belongs to the technical field of preparing luminescent carbon dots. Background technique [0002] In recent years, luminescent carbon dots with a diameter of less than 10 nm have received great attention because of their inherent unique properties, including their low toxicity, biocompatibility, easy biolabeling, and high stability (Bourlinos, A.B.et.al, Chem. Mater. 2012, 24, 6; Baker, S.N. and Baker, G.A. Angew. Chem. Int. Ed. 2010, 49, 6726). So far, many preparation methods have been reported, but the main disadvantage of these methods is that it is difficult to obtain high-yield luminescent carbon dots. In particular, the method of preparing luminescent carbon dots directly from graphite has been widely reported (Sun, Y.-P.et.al.J.Am.Chem.Soc.2006, 128, 7756; Cao, L.et.al. J.Am.Chem.Soc.2007, 129.11318; Hu, S.-L.et.al.J.Mater.Chem.2009, 19, 484; Zhao, Q.-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65
Inventor 郭明林张凯悦
Owner TIANJIN POLYTECHNIC UNIV
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