Method for preparing rare earth fluorescent silicon dioxide nanoparticles by microwave heating technology

A technology of silica and nanoparticles, applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problem of preparation methods of rare earth fluorescent silica nanoparticles, particle surface The chemical modification process takes a long time and the wide application of unfavorable markers, etc., to achieve good selective heating and high efficiency, uniform size, and shorten the reaction time

Active Publication Date: 2018-07-17
CHINA INSPECTION LAB TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(3) Emission spectral band is narrow
(4) Stokes displacement is large
However, this cyclic bonding method is cumbersome, time-consuming and labor-intensive, which is not conducive to the wide application of this marker
[0005] Chinese patent CN102504808A discloses a preparation method of rare earth fluorescent silica nanoparticles, using water-in-oil microemulsion system to synthesize blank silica nanoparticles, and fully reacting silane reagents with functional groups and rare earth ion complexes in advance Form the precursor, and then directly add the precursor to the water-in-oil microemulsion system, a large number of rare earth ion complexes can be modified to the surface of each silica nanoparticle, and then the rare earth ion is added to chelate the complex, This method is simple to prepare, with uniform particle size and high fluorescence intensity, but the process of chemical modification of the particle surface takes a long time
Moreover, the preparation method of using microwave heating technology to assist the preparation of rare earth fluorescent silica nanoparticles has not been reported yet.

Method used

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  • Method for preparing rare earth fluorescent silicon dioxide nanoparticles by microwave heating technology
  • Method for preparing rare earth fluorescent silicon dioxide nanoparticles by microwave heating technology
  • Method for preparing rare earth fluorescent silicon dioxide nanoparticles by microwave heating technology

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1: Preparation of Eu by Microwave Heating Technology 3+ -BHHCT@SiO 2 Fluorescent rare earth silica nanoparticles, research experiments on the effect of different microwave reaction times on fluorescence properties

[0040] (1) Preparation of silica nanoparticles: Take 6mL of cyclohexane, 2.13mL of Tx-100, 1.87mL of n-octanol and 0.6mL of ultrapure water into the Erlenmeyer flask, stir magnetically, and after stirring evenly, add 100 μL TEOS and 60 μL ammonia water were stirred at room temperature for 24 hours to obtain SiO 2 Nano microemulsion. .

[0041] (2) Surface amination of silica nanoparticles: Add 3 μL of 3-aminopropyltrimethoxysilane (APTMs) to the SiO obtained in (1). 2 In the nano-microemulsion, microwave heating, microwave power 700W, temperature 70°C, reaction time 10min, 20min, 30min, 40min.

[0042] (3) BHHCT-Eu 3+ Synthesis of fluorescent rare earth complexes: 5 mg of 4,4'-bis(1",1",1",2",2",3",3"-heptafluoro-4",6"-hexanedione -6"-yl)-chlo...

Embodiment 2

[0045] Example 2: Preparation of Eu by Microwave Heating Technology 3+ -BHHCT@SiO 2 Fluorescent rare earth silica nanoparticles, research experiment on the effect of different microwave reaction temperatures on fluorescent properties

[0046] (1) Preparation of silica nanoparticles: same as in Example 1.

[0047] (2) Surface amination of silica nanoparticles: Take 3 μL APTMs and add them to the SiO obtained in (1) 2 In the nano microemulsion, microwave heating, microwave power 700W, investigation temperature 70°C and 60°C, reaction time 20min.

[0048] (3) BHHCT-Eu 3+ Synthesis of Fluorescent Rare Earth Complex: Same as Example 1.

[0049] (4) BHHCT-Eu 3+ Preparation of modified silica fluorescent nanoparticles: add the fluorescent complex obtained in step (3) to the microemulsion system in (2), heat with microwave, microwave power 700W, temperature 59°C and 50°C, reaction time 20min. Add 5mL of acetone, mix well, centrifuge, then wash the particles with ethanol / water (v...

Embodiment 3

[0051] Example 3: Preparation of Eu by Microwave Heating Technology 3+ -BHHCT@SiO 2 Fluorescent rare earth silica nanoparticles, research experiments on the effect of different microwave power on fluorescent properties

[0052] (1) Preparation of silica nanoparticles: same as in Example 1.

[0053] (2) Surface amination of silica nanoparticles: Take 3 μL APTMs and add them to the SiO obtained in (1) 2 In the nano microemulsion, microwave heating, microwave power investigation 600W, 700W, 800W, 900W and 1000W, investigation temperature 70 ℃, reaction time 20min.

[0054] (3) BHHCT-Eu 3+ Synthesis of Fluorescent Rare Earth Complex: Same as Example 1.

[0055] (4) BHHCT-Eu 3+ Preparation of modified silica fluorescent nanoparticles: Add the fluorescent complex obtained in step (3) to the microemulsion system in (2), microwave heating, microwave power 600W, 700W, 800W, 900W and 1000W, temperature 59 ℃, reaction time 20min. Add 5mL of acetone, mix well, centrifuge, then wash...

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Abstract

The invention discloses a method for preparing rare earth fluorescent silicon dioxide nanoparticles by a microwave heating technology. The method comprises the following steps: preparing SiO2 nanoparticles with hydroxyl groups on the surfaces by using a water-in-oil (W/O) microemulsion dispersion system, modifying the SiO2 surfaces by a microwave heating method by using an aminosilane reagent andan Eu<3+> BHHCT complex to form a fluorescent rare earth complex, blocking a reaction system by using acetone, then washing to obtain a product, namely the covalent fluorescent rare earth silicon dioxide nanoparticles. By the method, the reaction time is effectively shortened and the fluorescence intensity is higher.

Description

technical field [0001] The invention discloses a method for preparing rare earth fluorescent silica nanoparticles by microwave heating technology, relates to the preparation of silica fluorescent nano-microspheres, in particular to a method for shortening the preparation of fluorescent silica nanoparticles by using microwave-assisted heating technology. A Temporal Approach to Silicon Nanoparticles. The invention also relates to the rare earth fluorescent silicon dioxide nanoparticles prepared by the microwave heating technology and its application. Background technique [0002] Fluorescent biomarker probes with various structures and fluorescent properties play an irreplaceable role in modern life sciences and biotechnology such as genomics, proteomics, and biochips. Progress is also largely dependent on the use of fluorescent biolabeled probes and the development and advancement of fluorescent detection methodologies. The currently developed fluorescent immunoassay marker...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06B82Y20/00B82Y30/00
CPCB82Y20/00B82Y30/00C09K11/06C09K2211/182
Inventor 邹明强齐小花赵兵洁
Owner CHINA INSPECTION LAB TECH CO LTD
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