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笼形八聚(乙烯基)硅倍半氧烷的合成
Synthesis of cage octa(vinyl) silsesquioxanes.
【摘要】 以乙烯基三甲氧基硅烷为反应单体、甲醇为溶剂、四甲基氢氧化铵为催化剂,合成了正立方体的笼形八聚(乙烯基)硅倍半氧烷[(CH2CHSi O1.5)8]。讨论了反应温度、时间、碱的用量和乙烯基三甲氧基硅烷的浓度对成笼反应的影响。结果表明,较佳的工艺条件为:乙烯基三甲氧基硅烷与四甲基氢氧化铵的量之比为1∶3,乙烯基三甲氧基硅烷的浓度为0.0747g/mL,于室温下反应24h后再60℃下反应48h;此时产物的收率可达80%。产物分别用元素分析、FT-IR、1H NMR、13C NMR、29Si NMR进行了表征。
【Abstract】 The cube cage octa(vinyl)silsesquioxanes were synthesized by taking vinyltrimethoxy silane as monomer, methanol as solvent, and tetramethyl ammonium hydroxide as alkaline reagent. The effects of temperature, time, the amount of alkali and monomer concentration on the cage reaction were discussed. The result showed that under the condition of room temperature for 24 h, and 60 ℃ for 48 h, the mass ratio of vinyltrimethoxy silane and tetramethyl ammonium hydroxide was 1∶3 under hydrolysis, the consistency of silane was 0.0747 g/mL, the products had a yield of 80%. The products were characterized by means of elemental analysis, FT-IR, 1H NMR, 13C NMR and 29Si NMR.
【Key words】 cage; vinyltrimethoxy silane; tetramethyl ammonium hydroxide; octa(vinyl) silsesquioxane;
- 【文献出处】 有机硅材料 ,Silicone Material , 编辑部邮箱 ,2005年05期
- 【分类号】O634.41;
- 【被引频次】8
- 【下载频次】453