端氨基聚硅氧烷的合成与表征

Synthesis and characterization of amino-terminated polysiloxane

以D4(八甲基环四硅氧烷)为活性单体、AT[1,3-双(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷]为封端剂、TMAH(四甲基氢氧化铵)为催化剂和DMSO(二甲亚砜)为促进剂,采用本体聚合法制备了端氨基聚硅氧烷(ATPS)。研究结果表明:采用单因素试验法优选出合成ATPS的最佳工艺条件是聚合温度为90℃、聚合时间为3 h、n(D4)∶n(AT)=1.2∶1.0、n(TMAH)∶n(AT)=1.5∶1.0和w(DMSO)=0.5%(相对于D4和AT总质量而言),此时ATPS的产率(95.13%)相对最大、氨值(2.1100 mmol/g)相对最低且黏度(628 mPa·s)适宜。

With D4 （octamethylcyclotetrasiloxane） as activated monomer,AT[1,3-bis（3-aminopropyl）-1,1,3,3-tetramethyldisiloxane] as end-capping agent,TMAH（tetramethylammonium hydroxide）as catalyst,and DMSO（dimethyl sulfoxide） as accelerant,so an ATPS （amino- terminated polysiloxane） was prepared by bulk polymerization process. The research results showed that the optimal process conditions of synthesizing ATPS were preferred by single-factor experiment when polymerization temperature was 90 ℃,polymerization time was 3 h,molar ratios of n（D4）∶n（AT） and n（TMAH）∶n（AT） were 1.2∶1.0 and 1.5∶1.0 respectively,and mass fraction of DMSO was 0.5% in D4 and AT. Here,the ATPS had the relatively maximal yield （95.13%）,the relatively minimal aminevalue （2.1100mmol/g）,and the appropriate viscosity （628 mPa·s）.