摘要
以二苯基二氯硅烷与二甲基二氯硅烷为原料,二甲苯与丙酮为混合溶剂,采用逆水解法同时水解二苯基二氯硅烷与二甲基二氯硅烷。以三甲基一氯硅烷为封端剂,四甲基氢氧化铵催化缩合合成二甲基二苯基硅油。考察了原料配比、水解时间、封端剂用量、缩聚时间等因素对二甲基二苯基硅油性能的影响。采用红外光谱、高效凝胶渗透色谱以及阿贝折射仪对样品进行了表征。结果表明：以二甲苯与丙酮为混合溶剂,采用逆水解法,在n（Ph）∶n（R）=（0.1~0.5）∶1的较宽范围内,可得到结构稳定的二甲基二苯基硅油。在n（Ph）∶n（R）=0.3∶1,水解温度30℃,水解时间5h,缩聚温度100℃,缩聚时间3h,x（三甲基一氯硅烷）=2.5%,w（四甲基氢氧化铵）=0.05%时,合成的二甲基二苯基硅油重均相对分子质量为1 513.9,数均相对分子质量为1 195.5。
Dimethyldiphenylsilicone oils were synthesized using dimethyldiehlorosilane and diphenyldichlorosilane as raw materialsby the contrary hydrolysis method in a mixed solvent of xylene and acetone, followed by the condensation process with tetra-methyl ammonium hydroxide as catalyst and trimethylchlorosilane as capping agent. The effects of raw material ratio, hydrolysis time, capping agent and condensation time on the properties of dimethyldiphenylsilicone oils were investigated. The obtained samples were characterized by FT-IR, HPGPC and Abbe refractometer. The experimental re- sults showed that stable dimethyldiphenylsilicone oils were synthesized by the contrary hydrolysis method in a mixed solvent of xylene and acetone in a wide range of n（Ph） ： n（R） mole ratios of 0.1 ：0.5. The weight-and number-average molecular weights of the as-synthesized dimethyldiphenylsilicone oil could reach 1 513.9 and 1 195.5, respectively when the synthesis was carried out under the experimental conditions, n（Ph） ： n（R） of 0.3, hydrolysis at 30 ℃ for 5 h, condensation at 100 ℃ for 3 h, trimethylchlorosilane mole percentage of 2.5%, tetramethyl ammonium hydroxide weight per- centage of 0.05 %.
出处
《精细石油化工》
CAS
CSCD
北大核心
2014年第5期14-19,共6页
Speciality Petrochemicals
基金
国家科技部--100t/a耐高低温硅树脂(2011DFR50080)
