Process for producing beta-diketone functionalization rare earth mesoporous hybridisation luminescent material

A technology of luminescent materials and functionalization, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of low doping amount of rare earth complexes, uneven distribution, instability of rare earth complexes, etc., to overcome mechanical and Insufficient stability, simple process, regular and orderly microscopic appearance

Inactive Publication Date: 2009-11-11
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this way, some problems will inevitably occur, such as uneven distribution of organic components, low doping amount of rare earth complexes, unstable rare earth complexes, easy to precipitate from the matrix, etc.
Although researchers are constantly exploring new preparation technologies, so far, there is no report on the synthesis technology of β-diketone functionalized rare earth mesoporous hybrid luminescent materials.

Method used

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  • Process for producing beta-diketone functionalization rare earth mesoporous hybridisation luminescent material
  • Process for producing beta-diketone functionalization rare earth mesoporous hybridisation luminescent material
  • Process for producing beta-diketone functionalization rare earth mesoporous hybridisation luminescent material

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Experimental program
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Effect test

Embodiment 1

[0026] (1) Synthesis of Dibenzoylmethane Intermediate

[0027] Dissolve 1mmol of dibenzoylmethane in 20mL of anhydrous tetrahydrofuran and add 2mmol of NaH to the solution system. The reaction solution bubbled vigorously. After one and a half hours, add 2.2mmol of propyltriethoxysilyl group to the above reflux solution. The tetrahydrofuran solution of propyl isocyanate was reacted at 65°C for 12 hours, and the solvent was removed by rotary evaporation to obtain an abnormally viscous yellow oil drop product.

[0028] (2) Synthesis of dibenzoylmethane functionalized binary mesoporous hybrid luminescent material

[0029] First, weigh 1.0 g of Pluronic P123 surfactant, add 7.5 g of deionized water and 30 g of 2 mol / L hydrochloric acid, and heat and stir to dissolve it. At room temperature, slowly add dropwise the mixed solution of TEOS and dibenzoylmethane intermediate at a molar ratio of 0.94:0.06, and stir for 24 hours. Then it was put into a stainless steel reaction kettle lined wi...

Embodiment 2

[0031] (1) Synthesis of Dibenzoylmethane Intermediate

[0032] Dissolve 1.5mmol of dibenzoylmethane in 25mL of anhydrous tetrahydrofuran and add 3mmol of NaH to the solution system. The reaction solution bubbled vigorously. After about one and a half hours, add 3.3mmol of propyltriethoxy to the reflux solution. The tetrahydrofuran solution of silyl propyl isocyanate was reacted at 70° C. for 12 hours, and the solvent was removed by rotary evaporation to obtain an abnormally viscous yellow oil drop product.

[0033] (2) Synthesis of dibenzoylmethane functionalized ternary mesoporous hybrid luminescent material

[0034] Weigh 1.5g of PluronicPl23 surfactant, add 11g of deionized water and 45g of 2mol / L hydrochloric acid, heat and stir to dissolve it. At room temperature, slowly add dropwise the mixed solution of TEOS and dibenzoylmethane intermediate at a molar ratio of 0.96:0.04, and stir for 24 hours. Then put it into a stainless steel reaction kettle lined with polytetrafluoroeth...

Embodiment 3

[0036] (1) Synthesis of acetylacetone intermediate

[0037] Dissolve 1mmol of acetylacetone in 15mL of anhydrous pyridine and add 2mmol of NaH to the solution system. The reaction solution bubbled vigorously. After about one and a half hours, add 2.2mmol of propyltriethoxysilyl isocyanide to the above reflux solution. The tetrahydrofuran solution of propyl acid was reacted at 65°C for 12 hours, and the solvent was removed by rotary evaporation to obtain an abnormally viscous yellow oily product.

[0038] (2) Synthesis of acetylacetone functionalized mesoporous hybrid luminescent material

[0039]Weigh 1.2 g of Pluronic P123 surfactant, add 9.0 g of deionized water and 36 g of 2 mol / L hydrochloric acid, and heat and stir to dissolve it. At room temperature, slowly add the TEOS and acetylacetone intermediate mixture dropwise with a molar ratio of 0.94:0.06, and stir for 24 hours. Then it was put into a stainless steel reaction kettle lined with polytetrafluoroethylene and crystalliz...

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Abstract

The invention belongs to the technical field of preparation of nano mesoporous materials, and in particular relates to a synthesis technology of a novel β-diketone functionalized rare earth mesoporous hybrid luminescent material. In the present invention, organic ligand molecules with β-diketone structure are covalently grafted into the inorganic mesoporous main frame by the method of organic modification synthesis, and then the rare earth europium or terbium ions are introduced to obtain stable chemical and thermodynamic properties and a high degree of order. mesoporous hybrid luminescent materials. The method of the invention has mild experimental conditions, easy construction of the whole preparation system, simple and convenient operation, easy control of conditions, and stable product quality.

Description

Technical field [0001] The invention belongs to the technical field of mesoporous material preparation, and specifically relates to a preparation method of a beta-diketone functionalized rare earth mesoporous hybrid luminescent material. Background technique [0002] Nano mesoporous materials have a special mesoscopic structure and properties, ultra-high specific surface area (>2000m 2 / g), super large pore volume (~2cm 3 / g), large and uniformly adjustable pore size (2-50nm), used in high-tech fields such as microelectronics, biological protein separation and identification, drug delivery, sensors, photoelectromagnetic materials, etc., especially in petroleum cracking, catalysis, adsorption, separation, etc. It has broad application prospects. Its discovery has also injected new vitality into the research of photocatalysis, solar cells, fuel cells and other fields, and is a core technology with great market potential. The synthetic chemistry of nano mesoporous materials with ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/77
Inventor 李颖闫冰
Owner TONGJI UNIV
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