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A kind of hybrid luminescent material based on michael addition reaction and preparation method thereof

A luminescent material, addition reaction technology, applied in luminescent materials, chemical instruments and methods, organic chemistry, etc.

Active Publication Date: 2020-03-20
ZHOUKOU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of hybrid luminescent materials by Michael addition reaction has not been reported

Method used

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  • A kind of hybrid luminescent material based on michael addition reaction and preparation method thereof
  • A kind of hybrid luminescent material based on michael addition reaction and preparation method thereof
  • A kind of hybrid luminescent material based on michael addition reaction and preparation method thereof

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preparation example Construction

[0024] A method for preparing a hybrid luminescent material based on a Michael addition reaction, comprising the steps of:

[0025] Step 1. Add 4-vinylpyridine-2,6-dicarboxylic acid, mercapto-containing silica, ethanol and water into a three-necked flask with a mass ratio of (0.1-1):20:40:100, and adjust The pH value of the solution is 6-10, then stirred at room temperature for 6-24h under the protection of argon, filtered, the filter cake was washed with distilled water and absolute ethanol in turn, and vacuum-dried at 40-80°C for 4-10h, wherein the silica was MCM- 41 or SBA-15;

[0026]

[0027] Wherein, the preparation method of MCM-41 or SBA-15 mesoporous silica containing mercapto group comprises the following steps: MCM-41 or SBA-15, mercaptopropyltriethoxysilane, triethylamine, toluene according to (0.5-2 ): 2:1:40 mass ratio into a three-necked flask, heated to reflux for 12-48 h under the protection of argon, then stopped heating and naturally lowered to room temp...

Embodiment 1

[0032] A method for preparing a hybrid luminescent material based on a Michael addition reaction, comprising the steps of:

[0033] Step 1. Add 4-vinylpyridine-2,6-dicarboxylic acid, mercapto-containing MCM-41, ethanol and water into a three-necked flask at a mass ratio of 0.1:20:40:100 to adjust the pH of the solution The value is 10, then stirred at room temperature for 6 hours under the protection of argon, filtered, the filter cake was washed with distilled water and absolute ethanol in turn, and dried in vacuum at 60°C for 8 hours;

[0034] Step 2. Add terbium chloride hexahydrate, the product prepared in step 1, ethanol and water into the there-necked flask at a ratio of 0.1:5:20:100, adjust the pH value of the solution to 8, stir at room temperature for 2 hours, filter, and filter cake Wash with distilled water and absolute ethanol in turn, and dry under vacuum at 60°C for 8h.

[0035] The preparation method of the MCM-41 containing mercapto group comprises the steps: ...

Embodiment 2

[0039] A method for preparing a hybrid luminescent material based on a Michael addition reaction, comprising the steps of:

[0040] Step 1. Add 4-vinylpyridine-2,6-dicarboxylic acid, mercapto-containing MCM-41, ethanol and water into a three-necked flask at a mass ratio of 0.3:20:40:100 to adjust the pH of the solution The value is 8, then stirred at room temperature for 10 h under the protection of argon, filtered, the filter cake was washed with distilled water and absolute ethanol in turn, and dried in vacuum at 50 ° C for 9 h;

[0041] Step 2. Add europium chloride hexahydrate, the product prepared in step 1, ethanol and water into the there-necked flask at a ratio of 0.3:5:20:100, adjust the pH value of the solution to 7, stir at room temperature for 4 hours, filter, and filter cake Wash with distilled water and absolute ethanol in turn, and dry in vacuum at 50°C for 9h.

[0042] The preparation method of the MCM-41 containing mercapto group comprises the steps:

[0043...

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Abstract

The invention discloses a Michael addition reaction-based hybrid luminescent material and a preparation method thereof. The structural general formula of the hybrid luminescent material is shown in the description, and Ln in the formula is Tb<3+>, Eu<3+> or Dy<3+>. The preparation method comprises the following steps: adding 4-vinylpyridine-2,6-dicarboxylic acid, mercapto group-containing silica, ethanol and water to a three-necked flask, adjusting the pH value of the obtained solution to 6-10, carrying out room temperature under the protection of argon for 6-24 h, filtering the stirred solution, sequentially washing the obtained filter cake with distilled water and anhydrous ethanol, and carrying out vacuum drying at 40-80 DEG C for 4-10 h; and dispersing the above prepared product in a distilled water and ethanol mixed solution, adding a rare earth salt, adjusting the pH value of the obtained solution to 6-10, carrying out room temperature stirring for 2-12 h, filtering the stirred solution, sequentially washing the obtained filter cake with distilled water and anhydrous ethanol, and carrying out vacuum drying at 40-80 DEG C for 4-10 h. A luminescence center is molecularly compounded with an inorganic matrix through stable chemical bond connection between a rare earth complex and the inorganic matrix. The method is a universal method for preparing hybrid materials, and provides reference for the synthesis of other hybrid materials.

Description

technical field [0001] The invention belongs to the field of hybrid optical material preparation, and in particular relates to a Michael addition reaction-based hybrid luminescent material and a preparation method thereof. Background technique [0002] In recent years, organic / inorganic hybrid luminescent materials have shown good application prospects in ion detection, drug controlled release, catalysis, biomedicine and other fields. Among all luminescent groups, rare earth complexes have attracted increasing attention due to their advantages such as high luminous efficiency and color purity, long luminescent lifetime, and wide emission wavelength range. However, pure rare earth hybrid luminescent materials have poor thermal / light stability and are not easily machined. In order to solve these problems, researchers disperse rare earth complexes into inorganic or polymer matrices to prepare organic / inorganic hybrid materials with unique properties, which greatly expands the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/79C07D213/803C09K11/06
CPCC07D213/79C07D213/803C09K11/06C09K2211/182
Inventor 李庆锋张新磊胡彬李春阳王振领
Owner ZHOUKOU NORMAL UNIV