CAJ | 학술논문

　　利用三步法合成了一系列具有不同臂数的线形和多臂星形端烃羧基聚二甲基硅氧烷（PDMS-MAAx ， x＝1，2，3，4）：首先，以Si-H数量不同的含氢封头剂分别与八甲基环四硅氧烷（D4）开环聚合，制得线形和多臂星形端氢基聚二甲基硅氧烷（PDMS-Hx ）；继而与甲基丙烯酸甲酯（MMA）进行硅氢加成反应，制得酯基封端的聚二甲基硅氧烷（PDMS-MMAx ）；最后将酯基在碱性条件下水解，制得PDMS-MAAx。采用FT-IR和1 H NMR对三个合成阶段的反应产物进行了跟踪分析，确认了各步产物的结构，并讨论了PDMS-MMAx 和PDMS-MAAx 的合成条件对产物结构的影响，在此基础上优化了PDMS-MAAx 的制备工艺，确定了PDMS-MMAx 的最佳合成条件为： Si-H与MMA的量之比为1.0∶1.2、反应温度70～80℃、催化剂摩尔浓度20×10-6～60×10-6、反应时间5 h； PDMS-MMAx 水解制备PDMS-MAAx的最佳条件为： NaOH水溶液中NaOH的质量分数为20％、 NaOH水溶液以及乙醇的用量分别为PDMS-MMAx 体积的3倍和1倍。
　　이용삼보법합성료일계렬구유불동비수적선형화다비성형단경최기취이갑기규양완（PDMS-MAAx ， x＝1，2，3，4）：수선，이Si-H수량불동적함경봉두제분별여팔갑기배사규양완（D4）개배취합，제득선형화다비성형단경기취이갑기규양완（PDMS-Hx ）；계이여갑기병희산갑지（MMA）진행규경가성반응，제득지기봉단적취이갑기규양완（PDMS-MMAx ）；최후장지기재감성조건하수해，제득PDMS-MAAx。채용FT-IR화1 H NMR대삼개합성계단적반응산물진행료근종분석，학인료각보산물적결구，병토론료PDMS-MMAx 화PDMS-MAAx 적합성조건대산물결구적영향，재차기출상우화료PDMS-MAAx 적제비공예，학정료PDMS-MMAx 적최가합성조건위： Si-H여MMA적량지비위1.0∶1.2、반응온도70～80℃、최화제마이농도20×10-6～60×10-6、반응시간5 h； PDMS-MMAx 수해제비PDMS-MAAx적최가조건위： NaOH수용액중NaOH적질량분수위20％、 NaOH수용액이급을순적용량분별위PDMS-MMAx 체적적3배화1배。
A three-step procedure was developed for synthesizing a series of linear and star-shaped car-boxyl-terminated polydimethylsiloxane , i.e., PDMS-MAAx (x=1, 2, 3, 4).First, the hydrogen-termina-ted PDMS with virous arms (PDMS-Hx ) were prepared based on the ring-opening polymerization of octam-ethylcyclotetrasiloxane (D4 ); then, methyl methacrylate (MMA) was reacted with PDMS-Hx to prepare es-ter terminated PDMS (PDMS-MMAx );finally, the terminal ester group was transformed to terminal carboxyl acid based on the hydrolysis reaction of ester under alkaline condition to obtain carboxyl acid terminated PDMS, i.e., PDMS-MAAx .FT-IR and 1 H NMR were employed to confirm the structure of the product in each step of reactions and the effects of synthetic conditions on the structure of the products were discussed . Also, the optimal conditions for the preparation of PDMS -MMAx were with a mole ratio of Si-H and MMA of 1.0∶1.2, and a catalyst molality of 20 ×10-6 ~60 ×10 -6 at 70~80℃for 5 hours.The optimal conditions for the preparation of PDMS-MAAx were that 20%mass fraction of NaOH in NaOH solution, and the volume of the NaOH solution and ethanol was threefold and one time of the PDMS -MMAx .