Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth

A polysilsesquioxane and siloxane-based technology, which is applied in the field of synthesis of polyhedral oligomeric silsesquioxane-based polymer composite luminescent materials, can solve the problem of reducing emission intensity, poor light and heat stability, and limiting the scope of use and effects, etc., to achieve the effects of improving luminous performance, easy control of conditions, and overcoming insufficient mechanical properties and stability

Inactive Publication Date: 2014-12-10
UNIV OF SHANGHAI FOR SCI & TECH
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Problems solved by technology

[0002] Rare earth organic complexes emit the characteristic fluorescence of rare earth ions through the ultraviolet absorption of organic ligands and intramolecular energy transfer, but the photothermal stab

Method used

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  • Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth
  • Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth
  • Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth

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Embodiment 1

[0035] A method for synthesizing a rare earth-containing polyhedral oligomeric silsesquioxane-based polymer composite luminescent material, which is characterized in that it specifically includes the following steps:

[0036] (1) Configuration of ethanol solution of rare earth terbium nitrate

[0037] Put 1.87g of terbium oxide into a beaker, add 20ml of concentrated nitric acid and 5ml of hydrogen peroxide, until the terbium oxide is completely dissolved, then heat to 60°C for reaction for 1 hour, and evaporate the obtained reaction solution to dryness to obtain solid terbium nitrate;

[0038] The amount of terbium oxide, nitric acid and hydrogen peroxide used in the above-mentioned reaction is calculated according to the ratio of terbium oxide: concentrated nitric acid: hydrogen peroxide is 1g: 10.7ml: 2.7ml;

[0039] The obtained solid terbium nitrate was dissolved in absolute ethanol to obtain a concentration of 1 mmol / L rare earth terbium nitrate ethanol solutio...

Embodiment 2

[0055] A method for synthesizing a rare earth-containing polyhedral oligomeric silsesquioxane-based polymer composite luminescent material, specifically comprising the following steps:

[0056] (1), the configuration of rare earth terbium nitrate ethanol solution is the same as in Example 1

[0057] (2) Preparation of monoamino polyhedral oligomeric silsesquioxane precursors with cage structure modified by organic ligands

[0058] Dissolve 0.874g (1mmol) of monoamino polyhedral oligomeric silsesquioxane (POSS) with a cage structure into 15ml of N,N-dimethylformamide (DMF) solvent, and then add 20ml to a concentration of 10mg / ml silane coupling agent (0.2g, 1mmol) in tetrahydrofuran solution, then under nitrogen atmosphere, control the temperature at 65 ° C for 3h, then add 0.05g (0.5mmol) organic ligand acetylacetone (ACAC), continue the reaction for 6h, The obtained reaction solution was rotary evaporated to obtain a yellow oily liquid which was the precursor of monoamino po...

Embodiment 3

[0071] A method for synthesizing a rare earth-containing polyhedral oligomeric silsesquioxane-based polymer composite luminescent material, specifically comprising the following steps:

[0072] (1), rare earth Eu(NO 3 ) 3 Configuration of ethanol solution

[0073] Put 1.75g ​​of europium oxide into a beaker, add 10ml of nitric acid, until the europium oxide is completely dissolved, then heat to 60°C for reaction for 1 hour, and the obtained reaction solution is stirred and evaporated to dryness to obtain solid europium nitrate;

[0074] The amount of europium oxide used in the above-mentioned reaction, nitric acid is calculated by the ratio of europium oxide: nitric acid: hydrogen peroxide is 1g: 10ml;

[0075] The obtained solid europium nitrate was dissolved in absolute ethanol to obtain rare earth Eu(NO3) with a concentration of 0.1 mol / L 3 weak;

[0076] (2) Preparation of mercapto polyhedral oligomeric silsesquioxane precursors with cage structure modified by organic ...

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Abstract

The invention discloses a method for synthesizing a polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth. The method comprises the following steps: firstly, coordinating organic ligand modified polyhedron oligomerization silsesquioxane of a cage-shaped structure with a first ligand rare earth ion by using a sol-gel method according to the coordination chemistry principle, subsequently introducing polymethyl methacrylate as a second ligand which can be coordinated with the rare earth ion, and coordinating, thereby obtaining the polyhedron oligomerization silsesquioxane macromolecule composite luminescent material which is good in fluorescence property and thermal stability, contains rare earth and is of the cage-shaped structure. The synthesis method is gentle in experiment condition, the whole preparation system is easy to establish and simple and convenient to operate, the conditions are easy to control, and a product is stable in quality.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth polymer composite materials, and in particular relates to a method for synthesizing rare earth-containing polyhedral oligomeric silsesquioxane based polymer composite luminescent materials. Background technique [0002] Rare earth organic complexes emit the characteristic fluorescence of rare earth ions through the ultraviolet absorption of organic ligands and intramolecular energy transfer, but the photothermal stability of rare earth organic complexes is poor. The stretching vibration of the non-radiative multipole phonon decay will reduce its emission intensity, which greatly limits its application range and effect. Therefore, doping rare earth organic complexes into specific inorganic matrices to form organic-inorganic composite materials can improve this situation, and shows good application prospects in the fields of chemistry, biology, medicine and materials. [0003] In ...

Claims

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Application Information

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IPC IPC(8): C08F20/14C08F8/42C09K11/06
Inventor 李颖王霞李华题袁红梅刘双和朱瑞丹
Owner UNIV OF SHANGHAI FOR SCI & TECH
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