Phenyl dimethoxyphosphine heterocyclic methyl silicate compound and preparation method thereof
A flame retardant technology of phenyldimethoxyphosphine silicate and heterocyclic methyl ester, which is applied in chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, organic chemistry, etc., to prevent melting and dripping , small mechanical properties, good dispersion effect
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Embodiment 1
[0028] Example 1 In a 150ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 16.21g (0.10mol) of cage-like phosphate, 80ml of diethylene glycol dimethyl ether Solution, 27.76g (0.14mol) phenyltrimethoxysilane and 0.49g dimethyl sulfate, heated up to 155°C, kept the temperature for 13h, then cooled to 60°C, transferred to a separatory funnel to stand for stratification, separated Add 35ml of toluene to the lower layer of feed liquid, let stand to separate the lower layer of feed liquid, and then distill under reduced pressure to remove toluene and a small amount of low-boiling matter to obtain light yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product is The rate is 89.0%, its flash point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25°C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.
Embodiment 2
[0029] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 16.21g (0.10mol) of caged phosphoric acid ester, 19.83g (0.10mol) of phenyl Trimethoxysilane and 0.32g dimethyl sulfate, heat up to 130°C, keep warm for 16h, then cool to 60°C, add 35ml of toluene to wash, stand still to separate the lower layer of material liquid, and then distill under reduced pressure to remove toluene and a small amount of low boiling point The product was obtained as a pale yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product yield was 81.4%, its flash point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25 °C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.
Embodiment 3
[0030]Example 3 In a 150ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 16.21g (0.10mol) of caged phosphate ester, 60mlDMF, 23.80g (0.12mol) Phenyltrimethoxysilane and 0.45g methyl p-toluenesulfonate, heat up to 140°C, keep warm for 14h, then cool to 60°C, transfer to a separatory funnel to stand for stratification, separate the lower layer of material liquid, and then add Wash with 35ml of toluene, let stand to separate the lower layer of feed liquid, and then distill under reduced pressure to remove toluene and a small amount of low boiling point substances to obtain light yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product yield is 86.8%. Point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25°C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.
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