Preparation method for water-soluble quaternary ammonium ion fluorescent carbon dot

A technology of quaternary ammonium cation and fluorescent carbon dots, which is applied in the field of carbon dot materials, can solve the problems of being unsuitable for large-scale production of quaternized ammonium salted fluorescent carbon dots and the high cost of raw materials, and achieves a technology that is favorable for popularization, simple in preparation process and effective in utilization. Effect

Inactive Publication Date: 2017-09-01
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of raw materials used in this method is relatively high, and it is not suitable for large-scale production of quaternized fluorescent carbon dots.

Method used

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  • Preparation method for water-soluble quaternary ammonium ion fluorescent carbon dot
  • Preparation method for water-soluble quaternary ammonium ion fluorescent carbon dot
  • Preparation method for water-soluble quaternary ammonium ion fluorescent carbon dot

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The preparation method of the water-soluble quaternary ammonium cationic fluorescent carbon dot of the present embodiment comprises the following steps:

[0032] 1) Add 1g of sodium carboxymethylcellulose and 1mL of 4,7,10-trioxy-1,13-tridecanediamine into 50mL of water, mix well, and perform hydrothermal reaction in a hydrothermal reactor. The reaction temperature was 200°C, and the reaction time was 12 hours. After the reaction, it was cooled to room temperature, and the reaction solution was dialyzed with a 3500Da dialysis bag to obtain an aqueous solution of carboxylated fluorescent carbon dots with a solid content of 2% on the surface rich in carboxyl groups;

[0033] 2) Add 1g of 4-dimethylaminopyridine and 6g of 3-chloro-2-hydroxypropyltrimethylammonium chloride to the aqueous solution of carboxylated fluorescent carbon dots obtained in step 1), mix well, and then add 110mL of Dimethyl sulfoxide solution of N,N'-dicyclohexylcarboximide, containing 6.6g of N,N'-di...

Embodiment 2

[0035] The preparation method of the water-soluble quaternary ammonium cationic fluorescent carbon dot of the present embodiment comprises the following steps:

[0036] 1) Add 4g of sodium carboxymethylcellulose and 6mL of 4,7,10-trioxy-1,13-tridecanediamine into 100mL of water, mix well, and perform hydrothermal reaction in a hydrothermal reactor. The reaction temperature was 150°C, and the reaction time was 24 hours. After the reaction, it was cooled to room temperature, and the reaction solution was dialyzed with a 4000Da dialysis bag to obtain an aqueous solution of carboxylated fluorescent carbon dots with a solid content of 5% on the surface rich in carboxyl groups;

[0037] 2) Add 2g of 4-dimethylaminopyridine and 3g of 3-chloro-2-hydroxypropyltrimethylammonium chloride to the aqueous solution of carboxylated fluorescent carbon dots obtained in step 1), mix well, and then add 205mL of N,N'-dicyclohexylcarbimide in dimethyl sulfoxide solution, the solution contains 11.7g...

Embodiment 3

[0039] The preparation method of the water-soluble quaternary ammonium cationic fluorescent carbon dot of the present embodiment comprises the following steps:

[0040] 1) Add 8g of sodium carboxymethyl cellulose and 10mL of 4,7,10-trioxy-1,13-tridecanediamine into 200mL of water, mix well, and carry out hydrothermal reaction in a hydrothermal reactor. The reaction temperature was 240°C, and the reaction time was 8 hours. After the reaction, it was cooled to room temperature, and the reaction solution was dialyzed with a 5000Da dialysis bag to obtain an aqueous solution of carboxylated fluorescent carbon dots with a solid content of 6% on the surface rich in carboxyl groups;

[0041]2) Add 3g of 4-dimethylaminopyridine and 8g of 3-chloro-2-hydroxypropyltrimethylammonium chloride to the carboxylated fluorescent carbon dot aqueous solution obtained in step 1), mix well, and then add 280mL of N, N'-dicyclohexyl carboximide in dimethyl sulfoxide solution, the solution contains 10g...

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Abstract

The invention relates to a preparation method for a water-soluble quaternary ammonium ion fluorescent carbon dot, and belongs to the technical field of carbon dot materials. The preparation method for the water-soluble quaternary ammonium ion fluorescent carbon dot comprises the following steps: 1) carrying out hydrothermal reaction after sodium carboxymethylcellulose and 4,7,10-3 oxygen-1,13-tridecane diamine are mixed, and carrying out dialysis after cooling to obtain carboxylation fluorescent carbon dot solution; 2) adding 3-chloro-2-hydroxypropyl-trimethylammonium chloride and catalyst into the carboxylation fluorescent carbon dot solution obtained in 1) to be subjected to esterification reaction, cooling, and carrying out centrifugation and dialysis to obtain the water-soluble quaternary ammonium ion fluorescent carbon dot. According to the preparation method for the water-soluble quaternary ammonium ion fluorescent carbon dot, the sodium carboxymethylcellulose is taken as a carbon source, so that the carbon source is environmentally-friendly, and reproducible and has wide sources and low cost, and the effective utilization of renewable resources can be realized. The preparation method provided by the invention has the advantages of simple preparation process, high yield and low cost, is very suitable for mass production and is favorable for popularization.

Description

technical field [0001] The invention relates to a preparation method of water-soluble quaternary ammonium cationic fluorescent carbon dots, belonging to the technical field of carbon dot materials. Background technique [0002] Carbon dots are a new type of nanomaterial with carbon as the skeleton structure discovered in recent years, and they are spherical nanoparticles with a size less than 10 nm. Carbon dots have excellent fluorescence properties, such as high fluorescence intensity, good stability, photobleaching resistance, and adjustable emission wavelength, etc., and also have easy surface functional group modification, low toxicity, good biocompatibility, low relative molecular weight and Particle size is extremely small and so on. [0003] At present, the synthesis methods of carbon dots mainly include laser ablation, electrochemical method, concentrated acid oxidation method, and hydrothermal method. The hydrothermal method is a commonly used method for the synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/06C09K11/06C07C213/06C07C213/10C01B32/15B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C07B2200/11C07C213/06C07C213/10C07C219/06C09K11/06
Inventor 牛庆媛高可政周立明王力臻韩莉锋
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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