Method for preparing water-soluble fluorescent carbon dots based on chitosan oligosaccharide-microwave assistance

A fluorescent carbon dot, microwave-assisted technology, applied in chemical instruments and methods, nano-carbon, nano-optics, etc., can solve the problems of uneven particle size distribution, complicated operation, poor stability, etc., and achieve stable fluorescence intensity and particle size distribution Uniform, good water solubility

Inactive Publication Date: 2017-05-10
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention is a preparation method of water-soluble fluorescent carbon dots designed for the problems of complex operation, difficult separation, low yield, uneven particle size distribution and poor stability in the existing preparation method of fluorescent carbon dots.

Method used

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  • Method for preparing water-soluble fluorescent carbon dots based on chitosan oligosaccharide-microwave assistance
  • Method for preparing water-soluble fluorescent carbon dots based on chitosan oligosaccharide-microwave assistance
  • Method for preparing water-soluble fluorescent carbon dots based on chitosan oligosaccharide-microwave assistance

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specific Embodiment approach 1

[0019] Specific embodiment 1: Dissolve 1.0 g of chitosan oligosaccharide in 15 mL of deionized water, add 0.2 mL of glacial acetic acid, and magnetically stir for 1 h to fully dissolve it. Put the above solution into a 50 mL polytetrafluoroethylene digestion tank, seal it and place it in a microwave digestion apparatus for digestion. The digestion conditions are: (1) temperature: 120°C, (2) power: 800 W, (3) Time: 6 min; after microwave reaction, cool to room temperature, take the solution for TEM characterization; see figure 1 , it can be seen from the figure that the surface layer of the obtained fluorescent carbon dots is covered with a layer of material to make them agglomerate together; the particle size of the carbon dots is uniform, and the particle size is ≤5 nm.

specific Embodiment approach 2

[0020] Specific embodiment 2: Dissolve 1.0 g of chitosan oligosaccharide in 15 mL of deionized water, add 0.2 mL of glacial acetic acid, and magnetically stir for 1 h to fully dissolve it. Put the above solution into a 50 mL polytetrafluoroethylene digestion tank, seal it and place it in a microwave digestion apparatus for digestion. The digestion conditions are: (1) temperature: 120°C, (2) power: 800 W, (3) Time: 6 min. After microwave reaction, cool down to room temperature; pour the obtained reaction solution into a 500 mL beaker, add 50 mL of ethanol for alcohol precipitation overnight, and separate by centrifugation, speed: 10000 r / min, time: 10 min; take the supernatant The liquid was characterized by transmission electron microscopy; for details, see figure 2 , the fluorescent carbon dots obtained after alcohol precipitation are evenly distributed, the particle size is less than 5 nm, and the dispersibility is good; no other substances are seen on the surface, indicat...

specific Embodiment approach 3

[0021] Specific embodiment 3: Dissolve 2.0 g of chitosan oligosaccharide in 20 mL of deionized water, add 0.4 mL of glacial acetic acid, and magnetically stir for 1 h to fully dissolve it; put the above solution into a 50 mL polytetrafluoroethylene digestion tank , sealed and placed in a microwave digestion apparatus for digestion, the digestion conditions are: (1) temperature: 120 °C, (2) power: 1000 W, (3) time: 6 min; after microwave reaction, cool to room temperature; Pour the obtained reaction solution into a 500 mL beaker, add 60 mL of ethanol for alcohol precipitation overnight, and separate by centrifugation at a speed of 10,000 r / min, time: 10 min; obtain the supernatant; : 80 ℃, drying time is 24 h, to obtain solid fluorescent carbon dot powder, stored in a brown transparent glass bottle until use. Take a small amount of prepared fluorescent carbon dot powder and irradiate it under a xenon lamp to measure its fluorescence stability. For details, see Figure 4 It can...

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Abstract

The invention relates to a method for preparing water-soluble fluorescent carbon dots based on chitosan oligosaccharide-microwave assistance, which is designed for the situation of complicated operation, difficult separation, low yield, non-uniform particle size distribution, poor stability and the like in fluorescent carbon dot preparation. In the method, chitosan oligosaccharide serves as a carbon source, water serves as a solvent and acetic acid serves as a cosolvent, and a microwave method is adopted for preparation; and the powder of fluorescent carbon dots is prepared by alcohol precipitation, separation and drying. In the invention, the prepared fluorescent carbon dots have good water solubility, stable fluorescence, uniform particle size distribution and high purity; the equipment is simple and convenient to operate and suitable for large-scale production; and the product has a good application prospect in the fields such as ion detection, bioimaging, fluorescent materials and the like.

Description

technical field [0001] The invention belongs to the fields of biomedical materials and nano-luminescent materials, and specifically designs a method for preparing water-soluble fluorescent carbon dots based on chitosan-microwave-assisted preparation. Background technique [0002] Fluorescent carbon dots are a new type of functionalized nanomaterials, whose particle size is generally less than 10 nm or close to the laser Bohr radius. Compared with semiconductor quantum dots (such as CdS quantum dots) and organic fluorescent dye molecules, its basic skeleton is carbon, which has low cell toxicity, good biocompatibility, easy solubility in water, high fluorescence intensity and good stability, and anti-toxicity. The advantages of photobleaching and easy functionalization are widely used in the fields of luminescent materials, biomarkers and imaging, optoelectronic devices, biosensors, photocatalytic composite materials, and ion analysis and detection. In recent years, the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15B82Y20/00B82Y40/00C09K11/65
CPCB82Y20/00B82Y40/00C01P2004/04C01P2004/64C01P2006/60C09K11/65
Inventor 刘鑫张玲帆姚建磊冯旭阳唐博朱杰冯岩
Owner EAST CHINA UNIV OF SCI & TECH
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