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Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate

A technology of ammonium carboxylate salt and fluorescent carbon dots, which is applied in the direction of fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problems of cumbersome process steps, low reaction yield, and difficulty in large-scale production and promotion, and achieve water-soluble Good performance, easy access to raw materials, and low cost

Active Publication Date: 2016-08-10
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fluorescence yield of the current preparation method is not much higher than 20%, and most of the process steps are cumbersome. Large-scale production promotion, therefore, it is necessary to develop effective, simple, cheap, large-scale production of fluorescent carbon dots

Method used

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  • Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate
  • Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate
  • Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate

Examples

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Effect test

Embodiment 1

[0033] A method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate salts is composed of the following steps:

[0034] 1) Dissolve 1g of ethylenediaminetetraacetic acid in 10ml of deionized water (the mass ratio of ethylenediaminetetraacetic acid to deionized water is 1:10), ultrasonically oscillate for 5min, pour into a vacuum volumetric flask filled with nitrogen and stir, add 0.419g of ethylenediamine (the molar ratio of ethylenediaminetetraacetic acid to ethylenediamine is 1:2), reacted at 20°C for 8h, washed three times with petroleum ether after the reaction was complete, separated the water layer, and removed the unresolved residue by rotary evaporation under reduced pressure. The ethylenediamine of reaction, obtains yellow solid;

[0035] 2) Put the yellow solid in a tube furnace, heat it to 350°C under the protection of nitrogen, the heating rate is 5°C / min, keep it warm for 1.5h and grind it for 10min to get a black powder;

[0036] 3) Dissolve ...

Embodiment 2

[0039] A method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate salts is composed of the following steps:

[0040] 1) Dissolve 1g of ethylenediaminetetraacetic acid in 10ml of deionized water (the mass ratio of ethylenediaminetetraacetic acid to deionized water is 1:10), ultrasonically oscillate for 5min, pour into a vacuum volumetric flask filled with nitrogen and stir, add 0.206g of ethylenediamine (the molar ratio of ethylenediaminetetraacetic acid to ethylenediamine is 1:1), react at 20°C for 8h, wash with petroleum ether three times after the reaction is complete, separate the water layer, and remove the unresolved residue by rotary evaporation under reduced pressure. The ethylenediamine of reaction, obtains yellow solid;

[0041] 2) Put the yellow solid in a tube furnace, heat it to 350°C under the protection of nitrogen, the heating rate is 5°C / min, keep it warm for 1.5h and grind it for 10min to get a black powder;

[0042] 3) Dissolve the bla...

Embodiment 3

[0045] A method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate salts is composed of the following steps:

[0046] 1) Dissolve 1g of ethylenediaminetetraacetic acid in 10ml of deionized water (the mass ratio of ethylenediaminetetraacetic acid to deionized water is 1:10), ultrasonically oscillate for 5min, pour into a vacuum volumetric flask filled with nitrogen and stir, add 0.617g of ethylenediamine (the molar ratio of ethylenediaminetetraacetic acid to ethylenediamine is 1:3), reacted at 20°C for 8h, washed three times with petroleum ether after the reaction was complete, separated the water layer, and removed the unresolved residue by rotary evaporation under reduced pressure. The ethylenediamine of reaction, obtains yellow solid;

[0047] 2) Put the yellow solid in a tube furnace, heat it to 350°C under the protection of nitrogen, the heating rate is 5°C / min, keep it warm for 1.5h and grind it for 10min to get a black powder;

[0048] 3) Dissolve ...

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Abstract

The invention discloses a method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate .The method includes the following steps that 1, polycarboxylic acid is dissolved in deionized water, ultrasonic oscillation is carried out, diamine is added for a reaction under nitrogen protection, a reaction product is washed with petroleum ether after the reaction is complete, an aqueous layer is separated out, reduced-pressure rotary evaporation is carried out to remove unreacted diamine, and a yellow solid is obtained; 2, the yellow solid is put into a tube furnace and heated under nitrogen protection, grinding is carried out after heat preservation, and black powder is obtained; 3, the black powder is dissolved in absolute ethyl alcohol, dialysis is carried out with a dialysis bag, a solution outside the dialysis bag is subjected to rotary evaporation, and the fluorescent carbon dots are obtained .The preparation method is easy to implement, raw materials are easy to get, cost is low, no environmental pollutant is released in the preparation process, and the preparation method is an environment-friendly preparation technology; the mean grain size of the fluorescent carbon dots prepared with the method is 11 nm, water solubility is good, fluorescence is stable, the fluorescence quantum yield reaches 22.46%, and the fluorescent carbon dots can be applied to Fe3+ detection.

Description

technical field [0001] The invention relates to a method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate salt, which belongs to the technical field of nano carbon material preparation technology. Background technique [0002] Carbon dots (CarbonDots), the core of which is carbon nanoparticles with a particle size of less than 10nm, has gradually become a research topic in the field of photoluminescence due to its good fluorescence properties, excellent biocompatibility, non-toxicity and easy surface functionalization. hotspot. However, the fluorescence yield of the current preparation method is not much higher than 20%, and most of the process steps are cumbersome. Large-scale production promotion, therefore, it is very necessary to develop effective, simple, cheap, large-scale production of fluorescent carbon dots. Contents of the invention [0003] In order to solve the above technical problems, the present invention provides a method for prepa...

Claims

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Application Information

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IPC IPC(8): C09K11/65G01N21/64C01B31/02B82Y40/00
CPCB82Y40/00C09K11/65G01N21/6428G01N2021/6432
Inventor 谌梓煦关瑞芳解俊鹏
Owner UNIV OF JINAN
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