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

A luminescent material and functionalized technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of low doping amount of rare earth complexes, uneven distribution, unstable rare earth complexes, etc. Insufficient stability, simple process, regular and orderly microstructure

Inactive Publication Date: 2008-07-16
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Synthesis of dibenzoylmethane intermediate

[0027] Dissolve 1 mmol of dibenzoylmethane in 20 mL of anhydrous tetrahydrofuran and add 2 mmol of NaH to the solution system. The reaction solution bubbles violently. After one and a half hours, add 2.2 mmol of propyltriethoxysilyl 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 unusually viscous yellow oil drop product.

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

[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, heat and stir to dissolve it. At room temperature, a mixture of TEOS and dibenzoylmethane intermediate was slowly added dropwise, with a molar ratio of 0.94:0.06, and stirred for 24 hours. Then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, and ...

Embodiment 2

[0031] (1) Synthesis of dibenzoylmethane intermediate

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

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

[0034] Weigh 1.5g of PluronicP123 surfactant, add 11g of deionized water and 45g of 2mol / L hydrochloric acid, heat and stir to dissolve it. At room temperature, a mixture of TEOS and dibenzoylmethane intermediate was slowly added dropwise, with a molar ratio of 0.96:0.04, and stirred for 24 hours. Then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, and cry...

Embodiment 3

[0036] (1) Synthesis of acetylacetone intermediate

[0037] Dissolve 1mmol acetylacetone in 15mL anhydrous pyridine and add 2mmolNaH to the solution system. The reaction solution bubbles violently. After about one and a half hours, add 2.2mmol propyl triethoxysilyl isocyanate dropwise to the above reflux solution The tetrahydrofuran solution of propyl ester was reacted at 65°C for 12 hours, and the solvent was removed by rotary evaporation to obtain an unusually viscous yellow oil drop-like product.

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

[0039]Weigh 1.2g of PluronicP123 surfactant, add 9.0g of deionized water and 36g of 2mol / L hydrochloric acid, heat and stir to dissolve it. At room temperature, a mixture of TEOS and acetylacetone intermediate was slowly added dropwise, with a molar ratio of 0.94:0.06, and stirred for 24 hours. Then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, and ...

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Abstract

The invention belongs to the technical field of manufacturing nano mesoporous material, in particular to a novel synthesis technology of Beta to diketone functionalized rare earth mesoporous hybrization and luminescent material. The invention first adopts a method of organic modification and synthesis to covalently graft an organic ligand molecule with Beta to diketone structure in a main body framework of an inorganic mesoporous, then rare earth europium or terbium ion is introduced to synthesize the high ordered mesoporous hybrization and luminescent material with steady chemistry and thermodynamic performance. The method and experimenting condition of the invention are moderate, the whole manufacturing system is easy to be established, the operation is easy, and the condition is easy for controlling, so the obtained products has steady quality. .

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous materials, and in particular relates to a preparation method of a β-diketone functionalized rare earth mesoporous hybrid luminescent material. Background technique [0002] With its special mesoscopic structure and properties, nano mesoporous materials have ultra-high surface area (>2000m 2 / g), large pore volume (~2cm 3 / g), large and uniform adjustable pore size (2-50nm), in high-tech fields such as microelectronics, biological protein separation and identification, drug delivery, sensors, opto-electromagnetic materials, 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 it is a core technology with great market potential. Synthetic chemistry of nano-mesoporous materials using supramolecu...

Claims

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Application Information

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IPC IPC(8): C09K11/77
Inventor 李颖闫冰
Owner TONGJI UNIV
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