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Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal

A technology of rare earth up-conversion and glycidyl ether, applied in chemical instruments and methods, luminescent materials, etc., to achieve good application prospects, easy access to raw materials, and good photostability

Inactive Publication Date: 2013-08-21
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hyperbranched glycidyl ether has excellent solubility and good biocompatibility, because it has a large number of hydroxyl groups, it can be conveniently chemically modified to give hyperbranched glycidyl ether more functions, and the polymer material has good Toughness and excellent processability have also been widely concerned by the material science community; although there have been many reports on the synthesis of rare earth upconversion luminescent nanocrystals, there are few reports on the synthesis of polymer functionalized rare earth upconversion luminescent nanocrystals. Therefore, combining the two to synthesize nanocomposites with excellent fluorescence properties and a wide range of applications has far-reaching theoretical significance and application prospects.

Method used

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  • Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal
  • Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal
  • Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) 100 mg of NaYF containing hydroxyl groups on the surface 4 : Yb / Er up-converting luminescent nanocrystals were added to 5 grams of tetrahydrofuran for ultrasonic dispersion, then 10 mg of potassium methylate was added, stirred at 50°C for 30 minutes, and then heated to 70°C to evaporate the solvent to prepare NaYF containing potassium methylate 4 : Yb / Er up-conversion luminescent nanocrystals.

[0018] (2) NaYF containing potassium methylate obtained in step (1) 4 : Yb / Er up-conversion luminescent nanocrystals are mixed with 5 grams of dioxane, and ultrasonically dispersed to obtain NaYF 4 : Yb / Er up-conversion luminescent nanocrystal dispersion liquid.

[0019] (3) to the NaYF prepared in step (2) 4 : Introduce argon gas into Yb / Er up-conversion luminescent nanocrystal dispersion liquid for 5 minutes, heat up to 95°C, then slowly add 2 grams of glycidyl alcohol dropwise through a constant pressure dropping funnel, and react for 48 hours to obtain hyperbranched ...

Embodiment 2

[0022] (1) 120 mg of NaYF containing hydroxyl groups on the surface 4 : Yb / Tm up-converting luminescent nanocrystals were added to 2 grams of tetrahydrofuran for ultrasonic dispersion, then 6 mg of potassium methylate was added, stirred at 30°C for 30 minutes, and then heated to 70°C to evaporate the solvent to obtain NaYF containing potassium methylate 4 : Yb / Tm up-conversion luminescent nanocrystals.

[0023] (2) NaYF containing potassium methylate obtained in step (1) 4 : Yb / Tm up-conversion luminescent nanocrystals are mixed with 2 grams of dioxane, and ultrasonically dispersed to obtain NaYF 4 : Yb / Tm up-conversion luminescence nanocrystal dispersion liquid.

[0024] (3) to the NaYF prepared in step (2) 4 : Introduce argon into the Yb / Tm up-conversion luminescent nanocrystal dispersion for 30 minutes, heat up to 90°C, then slowly add 2 grams of glycidyl alcohol dropwise through a constant pressure dropping funnel, and react for 24 hours to obtain a hyperbranched NaYF ...

Embodiment 3

[0026] (1) 150 mg of NaYF containing hydroxyl groups on the surface 4 : Yb / Er up-converting luminescent nanocrystals were added to 2 grams of tetrahydrofuran for ultrasonic dispersion, then 5 mg of potassium methylate was added, stirred at 45°C for 30 minutes, and then heated to 70°C to evaporate the solvent to prepare NaYF containing potassium methylate 4 : Yb / Er up-conversion luminescent nanocrystals.

[0027] (2) NaYF containing potassium methylate obtained in step (1) 4 : Yb / Er up-conversion luminescent nanocrystals are mixed with 2 grams of dioxane, and ultrasonically dispersed to obtain NaYF 4 : Yb / Er up-conversion luminescent nanocrystal dispersion liquid.

[0028] (3) to the NaYF prepared in step (2) 4 : Introduce argon gas into Yb / Er up-conversion luminescent nanocrystal dispersion liquid for 15 minutes, heat up to 120°C, then slowly add 0.2 g of glycidol dropwise through a constant pressure dropping funnel, and react for 4 hours to obtain hyperbranched NaYF graft...

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Abstract

The invention discloses a preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal. The preparation method comprises the following steps of: adding 1 part by weight of rare earth up-conversion luminescence nanocrystal into 10-100 parts by weight of tetrahydrofuran for ultrasonic dispersion, further adding potassium methoxide, stirring for 30 minutes at 30-50 DEG C, subsequently heating to be 70 DEG C so as to evaporate the solvent, further adding the components into 10-100 parts by weight of dioxane for ultrasonic dispersion, introducing argon for 5-30 minutes, raising the temperature to 90-120 DEG C, dropwise adding 1-50 parts by weight of glycidol, and reacting for 4-48 hours so as to obtain the hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal. The preparation method disclosed by the invention is simple to operate, the raw materials are easily available, the prepared nanocrystal has excellent up-conversion luminescence property and is high in luminescence intensity, good in photostability and good in solubility, and due to rich hydroxyl functional groups on the surface, the nanocrystal has good application prospects in aspects such as fluorescence labeling, biological detection and luminescent devices.

Description

technical field [0001] The invention belongs to the technical field of nanocomposite materials, and in particular relates to a preparation method of hyperbranched polyglycidyl ether-grafted rare earth up-conversion luminescent nanocrystals. Background technique [0002] Rare earth up-conversion luminescent materials refer to fluorescent materials that can emit visible light under the excitation of infrared or near-infrared light; they are widely used due to their advantages such as high fluorescence quantum yield, narrow emission peak, high light resistance and low toxicity. attention; compared with traditional luminescent markers (such as quantum dots, organic dyes), up-conversion luminescent materials have the advantages of high luminous intensity and large Stokes shift. Its excitation uses infrared light, which has a high penetration depth and can It effectively avoids the interference of autofluorescence and scattered light of biological samples, reduces the detection ba...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/85
Inventor 周立何本钊黄佳昌
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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