氨基烷基共聚型低聚硅氧烷的制备及表征

Preparation and Characterization of Amino Alkyl Copolymerization Type Siloxane Oligomers

以氨乙基氨丙基三甲氧基硅烷、丙基三甲氧基硅烷为原料,甲醇为溶剂,通过控制去离子水的用量、调节甲醇的浓度、滴加速度及反应温度,可制得链节数为5的氨基烷基嵌段共聚型低聚硅氧烷(APLOS)。研究了去离子水的用量、去离子水的滴加速度、甲醇的用量、水解/缩合温度等工艺参数对合成氨基烷基嵌段共聚型低聚硅氧烷收率的影响。结果表明:当氨乙基氨丙基三甲氧基硅烷与丙基三甲氧基硅烷的总量为1 mol(二者量之比为0.65∶0.35),水的总用量为0.8 mol时,能得到聚合度为5的APLOS;室温条件下,甲醇(58 g)与去离子水(14.4 g)混合液(即甲醇与去离子水质量比为4∶1)滴加速度为0.16 m L/s,滴加完毕持续1 h,蒸馏出甲醇后温度升至85℃回流3 h,制得氨基烷基嵌段共聚型低聚硅氧烷,收率高于90%。

Amino alkyl based oligosiloxane （APLOS） was prepared with chain numbers of 5 with [ 3 - （2 - Aminoethyl） aminopropyl ] trimethoxysilane and n - propyhrimethoxysilane as the raw materials, methyl alco-hol as the solvent, by controlling the deionized water content, adjusting the methanol concentration, dropping speed, and reaction temperature. The effects of the amount and dropping speed of deionized water, the amount of methanol, and the temperature of hydrolysis and condensation reaction to the recovery of the amino alkyl based oligosiloxane synthesis were studied. Resuls showed that the chain number of APLOS was 5 when the molar ratio between [ 3 - （ 2 - aminoethyl） aminopropyl ] trimethoxysilane and n - propyltrimethoxysilane was 0. 65：0. 35 and the water dosage was kept at 0. 8 mol. While the weight ratio of methyl alcohol（58g） and deionized water（ 14. 4g） was adjusted to 4 ： 1 and the dropping speed was 0. 16 mL/s at room temperature, then methanol was removed and refluxing for 3 h at 85℃, the yield could up to 90%.