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Preparation method of rare earth complex grafted luminescent titanium dioxide mesoporous microsphere

A technology of rare earth complexes and titanium dioxide, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as uneven distribution, aggregation of rare earth luminescent centers, and easy precipitation

Active Publication Date: 2014-01-29
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Mesoporous materials based on titanium dioxide have a wide range of applications in separation and purification, biomaterial catalysis, energy storage and conversion, etc. It is physically doped, which may lead to problems such as aggregation of rare earth luminescent centers, uneven distribution, and easy precipitation

Method used

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  • Preparation method of rare earth complex grafted luminescent titanium dioxide mesoporous microsphere
  • Preparation method of rare earth complex grafted luminescent titanium dioxide mesoporous microsphere
  • Preparation method of rare earth complex grafted luminescent titanium dioxide mesoporous microsphere

Examples

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Embodiment 1

[0025] This embodiment provides a preparation method of luminescent titanium dioxide mesoporous microspheres grafted with rare earth complexes, which includes the following steps:

[0026] (1) dodecylamine is dissolved in the round-bottomed flask that 200ml ethanol solvent is housed, then dropwise potassium chloride, deionized water and titanium tetraisopropoxide, dodecylamine: potassium chloride: deionized water : The molar ratio of titanium tetraisopropoxide is 0.5: (5.5×10 -3 ): (3-6): 1. After the reaction was fully stirred for 5 hours, it was allowed to stand at room temperature for 16 hours, and the obtained solid product was centrifuged, washed and dried; the dried solid product was the precursor of mesoporous titanium dioxide microspheres. Weigh 1.6g of mesoporous titania microsphere precursor, measure 20ml of ethanol, 10ml of deionized water and 0.2-0.3ml of ammonia water, place in a reaction kettle, heat at 160°C, after fully reacting, wash and dry the solid product ...

Embodiment 2

[0031] This example provides a method for preparing rare earth complex-grafted luminescent titanium dioxide mesoporous microspheres, the basic steps of which are the same as those of Example 1, except that the following specific steps are different:

[0032] (1) dodecylamine is dissolved in the round-bottomed flask that 200ml ethanol solvent is housed, then dropwise respectively potassium chloride, deionized water and titanium tetraisopropoxide, dodecylamine: potassium chloride: deionized water: The molar ratio of titanium tetraisopropoxide is 0.5: (5.5×10 -3 ): (3-6): 1. After the reaction was fully stirred for 5 hours, it was allowed to stand at room temperature for 16 hours, and the obtained solid product was centrifuged, washed and dried; the dried solid product was the precursor of mesoporous titanium dioxide microspheres. Weigh 1.6g of mesoporous titania microsphere precursor, measure 20ml of ethanol, 10ml of deionized water and 0.2-0.3ml of ammonia water, place in a rea...

Embodiment 3

[0037]The preparation method of a rare earth complex-grafted luminescent titanium dioxide mesoporous microsphere provided in this embodiment, the basic steps

[0038] Step is identical with embodiment 1, and its difference is that its following specific steps are different:

[0039] (1) dodecylamine is dissolved in the round-bottomed flask that 200ml ethanol solvent is housed, then dropwise potassium chloride, deionized water and titanium tetraisopropoxide, dodecylamine: potassium chloride: deionized water : The molar ratio of titanium tetraisopropoxide is 0.5: (5.5×10 -3 ): (3-6): 1. After the reaction was fully stirred for 5 hours, it was allowed to stand at room temperature for 16 hours, and the obtained solid product was centrifuged, washed and dried; the dried solid product was the precursor of mesoporous titanium dioxide microspheres. Weigh 1.5-2g of mesoporous titania microsphere precursor, measure 20ml of ethanol, 10ml of deionized water and 0.2-0.3ml of ammonia water...

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Abstract

The invention discloses a preparation method of a rare earth complex grafted luminescent titanium dioxide mesoporous microsphere. The preparation method mainly comprises the following steps: firstly, synthesizing a mesoporous titanium dioxide microsphere, modifying the mesoporous titanium dioxide microsphere with 2-2'-bipyridyl-4,4'-dicarboxylic acid to obtain a functionalized mesoporous titanium dioxide microsphere precursor, and then, carrying out reflux reaction on the precursor obtained in the former step and a synthesized binary rare earth complex in ethanol for hours to obtain a solid product, washing and drying the solid product to prepare a mesoporous composite material of the rare earth complex covalent grafted luminescent mesoporous titanium dioxide microsphere. According to the preparation method disclosed by the invention, a ternary rare earth complex is grafted into the mesoporous titanium dioxide microsphere through a covalent bond, and the obtained rare earth functionalized mesoporous titanium dioxide microsphere composite material can emit visible light and near-infrared light under visible light excitation, so that the composite material has a potential application prospect on the aspects of bioluminescence imaging, dye-sensitized solar cells, photocatalysis, etc.

Description

technical field [0001] The invention belongs to the technical field of preparation of luminescent nanocomposite materials, and in particular relates to a method for preparing luminescent titanium dioxide mesoporous microspheres grafted with rare earth complexes. Background technique [0002] Rare earth luminescent materials have been widely used in lighting, display, laser, medicine and other aspects. Because of the special electronic layer structure, rare earth elements have spectral properties that are incomparable to ordinary elements, but the fluorescence of direct excitation of rare earth ions is very weak, which limits their practical application. However, organic ligands have strong absorption in the ultraviolet-visible region. If rare earth ions are coordinated with ligands to obtain rare earth organic complexes, and the rare earth complexes are compounded in stable matrices such as sol-gel, mesoporous materials, and polymers, etc. In this process, rare earth organi...

Claims

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Application Information

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IPC IPC(8): C09K11/67C09K11/06
Inventor 孙丽宁施利毅王志娟仇衍楠韦族武
Owner SHANGHAI UNIV
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