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Method for preparing water-soluble rare-earth nanometer particles by super molecular self assembly

A technology of supramolecular self-assembly and nanoparticle, applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of complex process, long reaction time, destroying ligands, etc., and achieve simple process, fast reaction and easy raw materials The effect

Active Publication Date: 2012-05-23
中山泰辉生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the rare earth nanomaterials prepared by these methods are hydrophobic, and the surface is mostly oleic acid oleylamine ligands containing long alkyl chains, which are only easily soluble in non-polar organic solvents.
The currently reported surface modification method is to coat silica or polymer materials. Although it can improve water solubility and provide active groups, the process is complicated, the cost is high, and it affects the particle size control of rare earth nanoparticles.
The recently developed ligand oxidation method can effectively control the particle size of rare earth nanoparticles, but the reaction time is long, and the ligands on the surface are destroyed, and the cost is high.

Method used

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  • Method for preparing water-soluble rare-earth nanometer particles by super molecular self assembly
  • Method for preparing water-soluble rare-earth nanometer particles by super molecular self assembly
  • Method for preparing water-soluble rare-earth nanometer particles by super molecular self assembly

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Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: Preparation of water-soluble NaYF 4 nanoparticles.

[0033] Y(CF 3 COO) 3 2mmol, add 4mmol sodium trifluoroacetate and 7mmol sodium adamantane acetate, disperse in 20ml of mixed solvent composed of oleylamine and octadecene (V:V=1:7), heat up to 110°C, remove water for 1h, Then raise the temperature to 320°C, keep the temperature for 1 hour, cool to room temperature, add cyclohexane, ultrasonically disperse, centrifuge at 14000r / min for 10min, and wash with cyclohexane three times. After vacuum drying at room temperature for 12 hours, the desired oil-soluble rare earth nanoparticles with adamantaneacetic acid as a ligand can be obtained. The rare earth nanomaterials with adamantane acetate were dispersed in the mixed system of water and ethanol (V:V=1:10) at a concentration of 1 g / L, and then an equal volume of 1 mg / ml of β- Cyclodextrin aqueous solution, stirred for 2 minutes, centrifuged to separate rare earth nanomaterials, washed 3 times with water...

Embodiment 2

[0034] Embodiment 2: Preparation of water-soluble NaYF 4 : 20 mol% Yb, 2% mol Er nanoparticles.

[0035] Y(CF 3 COO) 3 0.78mmol, Yb(CF 3 COO) 3 0.2mmol, Er(CF 3 COO) 3 0.02mmol, add 2mmol of sodium trifluoroacetate and 7mmol of sodium adamantane carboxylate, disperse in 30ml of a mixed solvent composed of oleylamine and octadecene (V:V=2:7), heat up to 100°C, remove water for 2h, Then heat up to 330°C, keep the temperature for 1.5h, cool to room temperature, add cyclohexane, ultrasonically disperse, centrifuge at 12000r / min for 8min, and wash twice with cyclohexane. After vacuum drying at room temperature for 10 hours, the desired oil-soluble rare earth nanoparticles with adamantaneacetic acid as a ligand can be obtained. Disperse the rare earth nanomaterials with adamantane acetate in a mixed system of water and ethanol (V:V=10:1) at a concentration of 0.1 g / L, and then add 3 mg / ml of an equal volume of amino Functionalized β-cyclodextrin aqueous solution, stirred for...

Embodiment 3

[0036] Embodiment 3: Preparation of water-soluble NaGdF 4 : 20 mol% Yb, 1% mol Tm nanoparticles.

[0037] Gd(CF 3 COO) 3 3.18mmol, Yb (CF 3 COO) 3 0.8mmol, Tm (CF 3 COO) 3 0.04mmol, add 10mmol sodium trifluoroacetate and 14mmol sodium adamantane acetate, disperse in 40ml of a mixed solvent composed of oleylamine and octadecene (V:V=7:1), heat up to 80°C, remove water for 1.5 h, then raise the temperature to 310°C, keep the temperature for 1h, cool to room temperature, add cyclohexane, ultrasonically disperse, centrifuge at 13000r / min for 10min, and wash with cyclohexane three times. After vacuum drying at room temperature for 12 hours, the desired oil-soluble rare earth nanoparticles with adamantaneacetic acid as a ligand can be obtained. Disperse the rare earth nanomaterials with adamantane acetate in a mixed system of water and ethanol (V:V=1:10) at a concentration of 5 g / L, and then add an equal volume of 5 mg / ml carboxyl functional Melt β-cyclodextrin aqueous solut...

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Abstract

The invention belongs to the technical field of nanometer and super molecules, in particular to a method for preparing water-soluble rare-earth nanometer particles by super molecular self assembly. The method mainly comprises the following steps: firstly, synthesizing oil-soluble rare-earth nanometer particles modified by adamantine carboxylic acid; then, adding beta-cyclodextrin, and converting the beta-cyclodextrin into hydrophilic rare-earth nanometer particles through the strong super molecular effect with the adamantine; and carrying out centrifugal separation for washing away excrescentbeta-cyclodextrin. The method has the advantages of easy acquisition of raw materials, low cost, simple process and fast and convenient reaction, the obtained rare-earth nanometer particles have goodwater solubility, and can be easily connected with other molecules through the cyclodextrin, and the functionalization of the rare-earth nanometer particles is realized.

Description

technical field [0001] The invention belongs to the field of nanometer and supramolecular technology, and in particular relates to a method for preparing water-soluble rare earth nanoparticles by supramolecular self-assembly. Background technique [0002] Nanoscale rare earth materials (also known as rare earth nanomaterials) exhibit unique optical, electrical, and magnetic properties due to their unique 4f electronic structure, making them of great application value in biomarking and imaging. [0003] Typical preparation methods include hydrothermal method (Li Y D, Nature 2005, 437, 121) or pyrolysis method (Yan CH, Journal of the American Chemical Society 2005, 127, 3260) or inverse microemulsion method (Lemyre J L et al, Chemistry of Materials, 2005, 17, 3040) etc. However, the rare earth nanomaterials prepared by these methods are hydrophobic, and their surface is mostly oleic acid oleylamine ligands containing long alkyl chains, which are only easily soluble in non-pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82B3/00
Inventor 李富友刘倩
Owner 中山泰辉生物科技有限公司