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Microwave synthesis method for green fluorescent biomass carbon dots and application

A technology of biomass carbon and green fluorescence, applied in chemical instruments and methods, nano-carbon, luminescent materials, etc., can solve the problem of high-value conversion and utilization of unfavorable biomass carbon points, difficulty in achieving relative quantum yield, and limitation of biomass carbon points Application and other issues, to achieve the effect of shortening the synthesis time, improving the luminous performance, and fast heating speed

Active Publication Date: 2019-03-22
NANJING FORESTRY UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still many problems in related research. For example, the optimal emission wavelength of synthetic biomass carbon dots is mainly between 430 and 500 nm, which is mainly manifested as blue fluorescence emission, which greatly limits the application of biomass carbon dots in color display devices. , anti-counterfeiting printing and other fields of application
In addition, biomass carbon dots often need to be synthesized by hydrothermal method, and the preparation time of hydrothermal method is as long as several hours, which increases the energy consumption in the synthesis process of biomass carbon dots, and the synthetic biomass carbon dots The relative quantum yield of dots is difficult to reach 20%, and the lower quantum yield often leads to a decrease in luminous efficiency, which is not conducive to the high-value conversion and utilization of biomass carbon dots

Method used

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  • Microwave synthesis method for green fluorescent biomass carbon dots and application
  • Microwave synthesis method for green fluorescent biomass carbon dots and application
  • Microwave synthesis method for green fluorescent biomass carbon dots and application

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Experimental program
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Effect test

Embodiment 1

[0034] Accurately weigh 0.1 g xylose and 0.2 g m-phenylenediamine, fully dissolve in 10 mL, 2% phosphoric acid aqueous solution to form the starting material, then transfer the starting material to the reaction tube and place it in the microwave cavity, Biomass carbon dots were synthesized under the conditions of temperature 220°C, time 10 min, and input power 200 W. After the reaction was completed and cooled to room temperature, a black biomass carbon dot solution was obtained, which was filtered using a 0.22 μm syringe Purify the obtained solution, then transfer it to a clean plastic petri dish and place it in a freeze dryer, and freeze-dry it at -50°C for 48 hours to obtain a pure biomass carbon dot solid, which was measured by relative method The fluorescence quantum yield is 73.6%.

[0035] Take 20 μL of the purified biomass carbon dot solution and dilute it to 10 mL, and use a fluorescence spectrometer for emission spectrum testing. The optimal excitation wavelength is ...

Embodiment 2

[0037] Accurately weigh 0.1 g xylose and 0.2 g m-phenylenediamine, fully dissolve in 10 mL, 2% phosphoric acid aqueous solution to form the starting material, then transfer the starting material to the reaction tube and place it in the microwave cavity, Biomass carbon dots were synthesized under the conditions of temperature 180°C, time 10 min, and input power 200 W. After the reaction was completed and cooled to room temperature, a black biomass carbon dot solution was obtained, which was filtered using a syringe with a specification of 0.22 μm. The obtained solution was purified by a device, then transferred to a clean plastic petri dish and placed in a freeze dryer, and freeze-dried at -50 °C for 48 h to obtain pure biomass carbon dot solids. Figure 4 The high-resolution transmission electron microscope image of the green fluorescent carbon dots was obtained for this embodiment, and the fluorescence quantum yield was measured to be 40.9% by the relative method.

Embodiment 3

[0039] Accurately weigh 0.1 g of xylose and 0.2 g of m-phenylenediamine, fully dissolve in 10 mL of 2% nitric acid aqueous solution to form the starting material, then transfer the starting material to the reaction tube and place it in the microwave cavity, Biomass carbon dots were synthesized under the conditions of temperature 220°C, time 10 min, and input power 200 W. After the reaction was completed and cooled to room temperature, a black biomass carbon dot solution was obtained, which was filtered using a 0.22 μm syringe The obtained solution was purified by a device, then transferred to a clean plastic petri dish and placed in a freeze dryer, and freeze-dried at -50 °C for 48 h to obtain pure biomass carbon dot solids. Figure 5 The high-resolution transmission electron microscope image of the green fluorescent carbon dots was obtained for this embodiment, and the fluorescence quantum yield was measured to be 65.3% by the relative method.

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Abstract

The invention discloses a microwave synthesis method for green fluorescent biomass carbon dots. The method comprises the following steps: (1) fully dissolving xylose into a dilute acid solution or deionized water, adding a nitrogen doping agent m-phenylenediamine, and uniformly mixing to obtain an initial matter; (2) transferring the initial matter obtained in the step (1) into a reaction tube, and placing the reaction tube in a closed reaction chamber of a ring focusing single-mode microwave synthesis reactor for performing microwave treatment; (3) purifying the product to obtain an aqueous solution of biomass carbon dots after the reaction is ended and the product is cooled to a room temperature; (4) performing freeze drying on the aqueous solution of biomass carbon dots until the wateris completely lost, so as to finally obtain the pure solid biomass carbon dots. The invention further discloses application of the microwave synthesized green fluorescent biomass carbon dots, appliedto the field of anti-counterfeit printing. The microwave treatment heating speed is high, the synthetic efficiency is high, the synthesis time of the biomass carbon dots can be obviously shortened, and the relative fluorescence quantum yield of the obtained carbon dots reaches 73.6%.

Description

technical field [0001] The invention relates to a microwave synthesis method and application of green fluorescent biomass carbon dots, belonging to the technical field of fluorescent carbon dot preparation. Background technique [0002] As a new zero-dimensional carbon material, carbon dots are widely used in fluorescence detection, photocatalysis, cell It has potential application value in the fields of imaging, luminescence conversion layer and information encryption. With the deepening of research on carbon dots, biomass materials have been proved to be a cheaper and greener carbon source. In recent years, the research on biomass-based carbon dots has made many important progresses, which not only realizes the high-value conversion and utilization of biomass resources, but also provides the possibility for the further development and utilization of fluorescent carbon dots. However, there are still many problems in related research. For example, the optimal emission wave...

Claims

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Application Information

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IPC IPC(8): C01B32/15B82Y40/00C09K11/65
CPCB82Y40/00C01B32/15C09K11/65
Inventor 周晓燕杨培陈敏智朱子琪陈卫民张涛张伟
Owner NANJING FORESTRY UNIV
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