Methyltri(2,3-dichloropropoxy)silane compound and preparation method thereof
A technology of methyltrichlorosilane and dichloropropoxy, which is applied in the field of methyltrisilane compound and its preparation, can solve the problems of narrow application range and high price, and achieve no pollution, low cost, good physical and chemical properties stable effect
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Embodiment 1
[0017] Example 1 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.6mol (55.5g) of epichlorohydrin at 25°C , control the drop below 60°C within 1 hour, maintain 60°C, and continue the reaction for 28 hours. After the reaction was completed, a small amount of low-boiling matter was distilled off under reduced pressure to obtain oily liquid methyl tris(2,3-dichloropropoxy)silane with a yield of 94%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.
Embodiment 2
[0018] Example 2 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.68mol (62.9g) of epichlorohydrin at 25°C , controlled below 60°C within 1h to complete the drop, then raised the temperature to 80°C, and continued the reaction for 23h. After the reaction, excess epichlorohydrin and a small amount of low-boiling matter were distilled off under reduced pressure to obtain oily liquid methyl tris(2,3-dichloropropoxy)silane with a yield of 96%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.
Embodiment 3
[0019] Example 3 In a 150ml three-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.72mol (66.6g) of epichlorohydrin at 25°C , control the temperature below 60°C within 1h to complete the drop, raise the temperature to 100°C, and continue the reaction for 15h. After the reaction, excess epichlorohydrin and a small amount of low-boiling matter were distilled off under reduced pressure to obtain oily liquid methyl tris(2,3-dichloropropoxy)silane with a yield of 98%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.
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