氯化含硅芳炔树脂的合成

以二氯硫酰为氯化剂,在0℃下将含硅芳炔(SA)树脂结构中的硅氢基团转化为硅氯基团,合成了氯化含硅芳炔(Cl-SA)树脂,采用傅里叶变换红外光谱和核磁共振技术对Cl-SA树脂的结构进行表征。表征结果显示,硅氢基团的转化率达到90%,炔基活性基团未发生变化。以Cl-SA树脂和三甲基硅醇为原料、三乙胺为催化剂,制备了三甲基硅氧基含硅芳炔(SiO-SA)树脂;以Cl-SA树脂和二甲胺为原料,制备了二甲胺基含硅芳炔(N-SA)树脂;采用傅里叶变换红外光谱和核磁共振技术对N-SA和SiO-SA树脂的结构进行了表征。凝胶渗透色谱表征结果显示,与SA树脂相比,N-SA和SiO-SA树脂的相对分子质量增大,相对分子质量分布基本不变。

Synthesis of Chlorinated Silicon-Containing Aryne Resin

Chlorinated silicon-containing aryne(Cl-SA) resin was synthesized by chlorination of silicon-containing aryne(SA) resin at 0 ℃ using SO2Cl2 as chlorinating agent.The SA and Cl-SA resins were characterized by means of FTIR and 1H NMR.In chlorination,conversion of Si—H groups reaches 90% and active groups,such as ethynyl,keep unchanged.On the basis of Cl-SA,a series of SA derivative resin were prepared.SA resin containing trimethyl siloxy groups(SiO-SA) was synthesized from Cl-SA and trimethyl silanol with triethylamine as catalyst.Another SA resin containing dimethylamino groups(N-SA) was prepared from Cl-SA and dimethylamine at room temperature.Both SiO-SA and N-SA resins were characterized by means of FTIR and 1H NMR.Their relative molecular masses and relative moleculat masses distributions were determined by means of GPC analyses.Comparing with mother SA resin,relative molecular masses of both SiO-SA and N-SA resins increase,and their distributions remain unchanged.