Methyl tri(2-chloropropyl)silane compound and preparation method thereof
A silane compound and chloropropoxy technology, applied in the field of methyltrisilane compound and its preparation, can solve the problems of high price and narrow scope of use, and achieve the effects of low cost, good symmetry characteristics and easy large-scale production
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Embodiment 1
[0017] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, add 0.2mol (29.9g) of methyltrichlorosilane ,. Then add 0.6 mol (34.8 g) of propylene oxide dropwise under the liquid surface under cooling conditions, and control the temperature not to exceed 70°C at the rate of addition, and react at 70°C for 10 hours after the drop is completed. After the reaction was completed, a small amount of low-boiling matter was distilled off under reduced pressure to obtain a colorless liquid methyltris(2-chloropropoxy)silane with a product yield of 93%. Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.
Embodiment 2
[0018] Example 2 Add 0.2 mol (29.9 g) of methyltrichlorosilane to a 100 ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser, and an extremely flexible and expandable soft seal at the top of the condenser ,. Then add 0.65 mol (37.7 g) of propylene oxide dropwise under the liquid surface under cooling conditions, and control the temperature not to exceed 70°C at the rate of addition, and react at 60°C for 8 hours after dropping. After the reaction is over, excess propylene oxide (recycled) is distilled off under normal pressure, and a small amount of low-boilers are removed by distillation under reduced pressure to obtain a colorless liquid methyl tris(2-chloropropoxy)silane with a product yield of 96%. . Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.
Embodiment 3
[0019] Example 3 Add 0.2 mol (29.9 g) of methyltrichlorosilane to a 100 ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser tube and an extremely flexible and expandable soft seal at the top of the condenser tube ,. Then add 0.7mol (40.6g) of propylene oxide dropwise under the liquid surface under cooling conditions, and control the temperature not to exceed 50°C at the rate of addition, and react at 50°C for 6 hours after the drop is completed. After the reaction is over, excess propylene oxide (recycled) is distilled off under normal pressure, and a small amount of low-boilers are removed by distillation under reduced pressure to obtain a colorless liquid methyl tris(2-chloropropoxy)silane with a product yield of 98%. . Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.
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