Nitrogen, phosphorus and sulphur doping or co-doping carbon dot and batch controllable preparing method and application thereof

A technology of sulfur doping and co-doping, applied in the field of nanomaterials, can solve the problems of low yield, complicated process, and long synthesis time, and achieve the effects of good biocompatibility, simple process, and short synthesis time

Inactive Publication Date: 2015-10-21
XI AN JIAOTONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems of low yield, relatively complicated process and long synthesis time in the carbon dot synthesis method in the prior art, the present invention provides a nitrogen, phosphorus, sulfur doped or co-doped carbon dot and its batch controllable preparation method and application, the method is simple in process, can be produced in batches, and the doping amount can be precisely regulated. The product can be used for bioluminescent labeling and can be used as a probe for cell imaging

Method used

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  • Nitrogen, phosphorus and sulphur doping or co-doping carbon dot and batch controllable preparing method and application thereof
  • Nitrogen, phosphorus and sulphur doping or co-doping carbon dot and batch controllable preparing method and application thereof
  • Nitrogen, phosphorus and sulphur doping or co-doping carbon dot and batch controllable preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 Synthesis of nitrogen-doped carbon dots using amino acids as both carbon and nitrogen sources

[0034] Use 1 g of a mixture of glycine, alanine and valine as a nitrogen source and a carbon source at the same time, grind it into powder in an agate mortar and make it fully mixed, the molar ratio of C and N in the mixture is 1:0.3, and then Put the mixture into a 10mL glass test tube, put the test tube into an oil bath heated to 300°C in advance, the solid amino acid gradually begins to melt and turn yellowish brown until black, forming carbon dots, the reaction time is 10min, and then take it out of the oil bath The test tube was cooled naturally. The product was dissolved in water, filtered with a 22-micron membrane filter, and then dried in a vacuum oven at 40° C. for 12 hours. Then gradient column chromatography was performed using dichloromethane and methanol as developing solvents (4:1 volume ratio) to obtain nitrogen-doped fluorescent carbon dots.

[003...

Embodiment 2

[0036] Example 2 Preparation of nitrogen-sulfur co-doped carbon dots using cystine as carbon source, nitrogen source and sulfur source at the same time

[0037] Use 1g of cystine as nitrogen source, carbon source and sulfur source at the same time, wherein the molar ratio of C, N, and S is 1:0.333:0.333, put cystine into a 10mL glass test tube, put the test tube into the In an oil bath at 250°C, cystine gradually began to melt and turned yellowish brown until black, forming carbon dots. The reaction time was 25 minutes, and then the test tube was taken out of the oil bath to cool naturally. The product was dissolved in ethanol, filtered with a 22-micron membrane filter, and then dried in a vacuum oven at 40° C. for 12 hours. Then gradient column chromatography was carried out using dichloromethane and methanol as developing solvents (4:1 volume ratio) to obtain nitrogen-sulfur co-doped fluorescent carbon dots.

[0038] The raw material in this embodiment can also be the mixtu...

Embodiment 3

[0041] Example 3 Prepare nitrogen-doped carbon dots with tartaric acid and glycine as carbon source and nitrogen source respectively

[0042] Tartaric acid and glycine were mixed according to different mass ratios (respectively 9:1, 8:2, 7:3, 6:4, 5:5, 4:6, 3:7, 2:8, 1:9, 0:10 , that is, the molar ratio of C and N in the mixture is 1:(0.05~0.5)) mix evenly, each 1g, grind into powder in an agate mortar and mix well, then put each mixture into 10mL glass In the test tube, put the test tube into an oil bath heated to 200°C in advance, the mixture gradually begins to melt and turn yellowish brown until black, forming carbon dots, the reaction time is 3min, 5min, 8min, 15min, 22min, 30min, 37min , 45min, 52min, 60min, and then take out the test tube from the oil bath to cool naturally. The product was dissolved in water, filtered with a 22-micron membrane filter, and then dried in a vacuum oven at 40° C. for 12 hours. Then gradient column chromatography was performed to obtain n...

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Abstract

The invention provides a nitrogen, phosphorus and sulphur doping or co-doping carbon dot and a batch controllable preparing method and application thereof. The method comprises the steps that a carbon source, a nitrogen source, a phosphorus source and a sulphur source are evenly mixed, and a mixture is obtained, wherein the molar ratio of C to N to P to S in the mixture is 1 to 0-0.8 to 0-0.4 to 0-0.4, and the contents of N, P and S are prevented from being zero at the same time; in the air, the mixture is heated to be fused, the reaction is carried out for 3 min to 60 min, natural cooling is carried out till the indoor temperature is reached, a reaction product is separated by a silicagel column, raw materials which do not react are removed, and the nitrogen, phosphorus and sulphur doping or co-doping carbon dot is obtained. According to the method, the technology is simple, the compound time is short, batch producing can be achieved, the doping amount can be adjusted and controlled accurately, the fluorescence color of the prepared carbon dot ranges from blue to green, the application can be achieved on bioluminescence marking and cell imaging aspects, and the good economic benefit and the application prospect are achieved.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and in particular relates to a carbon dot doped or co-doped with nitrogen, phosphorus and sulfur, and a batch controllable preparation method and application thereof. Background technique [0002] Carbon nanomaterials (including carbon nanotubes, carbon nanorods, diamonds, fullerenes, carbon quantum dots, etc.) have excellent mechanical properties, electrical conductivity, thermal stability, special fluorescent properties and chemical stability, and have been used in optical Devices, medical diagnosis, catalysts, LED packaging materials and many other aspects. Fluorescent carbon material is a biocompatible material with nanostructure and chemical stability, which is widely used in biological imaging. Moreover, the recently popular graphene carbon dots have abundant surface functional groups, which can be modified and have broad application prospects. The photoluminescence of graphene quantum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65C01B31/02G01N21/64B82Y40/00B82Y20/00
Inventor 孟令杰陈招贾梦雪王晓驰刘天辉曹瑞军
Owner XI AN JIAOTONG UNIV
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