Molybdenum-containing polyoxometallate reactive flame retardant and preparation method thereof
A technology of polyoxometalate and reactive flame retardant, which is applied in the field of molybdenum-containing polyoxometalate reactive flame retardant and its preparation, can solve the problem of low flame retardant efficiency, polyoxometalate Problems such as poor compatibility of processable substrates, to improve the flame retardant effect, avoid adverse effects, and solve the effect of poor processability
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Embodiment 1
[0032] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {MnMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.244g p-Hydroxybenzaldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75 ℃ for 5h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 12h; concentrated under pressure, precipitated in ethyl acetate, and the product after suction filtration was dissolved in 25 mL of acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid was precipitated, filtered by suction, and dried in a vacuum to obtain the molybdenum-containing polysaccharide Oxygenate reactive flame retardant, as (C 19 h 15 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:
[0033]
[0034]Weigh 5g of epoxy resin E-51, heat up to 100°C, add 0.25g of the molybdenum-containing polyoxometalate reactive flame retardant obtained in Example 1, stir and dissolve,...
Embodiment 2
[0037] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {MnMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.176g 3-hydroxybutyraldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75°C for 10h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 12h; after the reaction, cool to room temperature, Concentrate under reduced pressure, precipitate in ethyl acetate, and the product after suction filtration is dissolved in 25mL acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid is precipitated, which is filtered by suction and dried in a vacuum to obtain the molybdenum-containing Polyoxometalate reactive flame retardant, as (C 16 h 17 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:
[0038]
Embodiment 3
[0040] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {FeMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.176g 3-hydroxybutyraldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75°C for 5h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 24h; after the reaction, cool to room temperature, Concentrate under reduced pressure, precipitate in ethyl acetate, and the product after suction filtration is dissolved in 25mL acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid is precipitated, which is filtered by suction and dried in a vacuum to obtain the molybdenum-containing Polyoxometalate reactive flame retardant, as (C 16 h 17 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:
[0041]
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