Phosphorus-nitrogen containing flame retardant modified silane coupler and preparation method thereof
A silane coupling agent and modification technology, which is applied in the field of flame retardant modified silane coupling agent and its preparation, to achieve the effect of solving the problem of flammability
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Embodiment 1
[0013] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours; the system was heated until the temperature rose to 83°C, kept at this temperature for reflux reaction for 2 hours, and dichloromethane was removed by decompression precipitation to obtain a white solid ;
[0014] Take 9.224 g of the white solid obtained above, put it in a 150 ml three-necked flask, add 50 ml of tetrahydrofuran to dissolve it, then add 5.060 g of triethylamine, pass nitrogen gas for 10 minutes, heat up to 50 ° C, and drop 10.32 g of N-(β- Aminoethyl)-γ-aminopropylmethyldimethoxysilane, kept at 50°C to continue the reaction for 5 hours after the dropwise addition. After the reaction is completed, filter, and...
Embodiment 2
[0023] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours. The temperature of the system was kept rising to 83° C. for reflux reaction for 2 hours, and the methylene chloride was removed under reduced pressure to obtain a white solid.
[0024] In a 150ml three-neck flask, take 9.224g of the above solid, dissolve it in 50ml of tetrahydrofuran, add 5.060g of triethylamine, blow nitrogen for 10 minutes, heat up to 80°C, add dropwise 9.567g of γ-aminopropylmethyldiethoxy Silane, after the dropwise addition was completed, the reaction was continued at 80° C. for 7 hours. After the reaction is completed, filter, and remove the solvent from the filtrate under reduced pressure to obtain a v...
Embodiment 3
[0034] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours. The temperature of the system was kept rising to 83° C. for reflux reaction for 2 hours, and the methylene chloride was removed under reduced pressure to obtain a white solid.
[0035] In a 150ml three-necked flask, take 9.224g of the above solid, dissolve it in 50ml of tetrahydrofuran, add 5.060g of triethylamine, blow nitrogen for 10 minutes, heat up to 60°C, add 11.34g of aminopropyltriethoxysilane dropwise, add dropwise After completion, the reaction was continued at 60° C. for 5 hours. After the reaction is completed, filter, and remove the solvent from the filtrate under reduced pressure to obtain a viscous liquid, whi...
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