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.
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[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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