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首先以五配位硅钾化合物与对苄氯苯乙烯反应制备出苯乙烯基四配位硅单体;然后进行自由基溶液聚合得到苯乙烯基四配住硅均聚物;最后对单体及聚合物进行红外光谱(IR)、元素分析(EA)、能谱元素分析(EDS)、热重分析(TG)、差示扫描量热谱(DSC)、凝胶渗透色谱法(GPC)等结构表征与性能测试.IR表明单体在1629.6 cm~(-1)处的C=C双键伸缩振动吸收峰在均聚物中消失;TG表明均聚物在239℃才开始失重;DSC表明均聚物的玻璃化转变温度为32.8℃;GPC分析表明均聚物的数均分子量(M)_n=67504,质均分子量(M)_W=88532,分散系数为1.31.

Double bond tetra-coordinated silicon was produced by the reaction of penta-coordinate silicon complex with 4-vinylbenzyl chloride, and homo-polymer was prepared using tetra-coordinated silicon as monomer through the free radical solution polymerization. The tetra-coordinate silicon monomer and homo-polymer were characterized by infra-red spectrum(IR), elemental analysis(EA), elemental diffraction spectrum (EDS), thermogravimetric analysis (TG), differential scanning calorimetry(DSC), gel permeation chromatography (GPC)etc. The IR spectrum of tetra-coordinate silicon monomer indicates a absorption band for C= C at 1629.6 cm~(-1), but the IR spectrum of homo-polymer exhibits no absorption band near 1629.6 cm~(-1). TG analysis shows that the homo-polymer begin losing mass at 239 ℃, ends at 600 ℃, the glass transition temperature is 32.8 ℃. GPC analysis shows that the molecular weight of the homo-polymer is about 67 thousand.

参考文献

[1] Kim SG;Choi J;Tamaki R;Laine RM .Synthesis of amino-containing oligophenylsilsesquioxanes[J].Polymer: The International Journal for the Science and Technology of Polymers,2005(12):4514-4524.
[2] 宋建华,章永化,刘安华,龚克成.双羟基四配位硅单体的合成[J].有机化学,2002(10):773-777.
[3] 宋建华,章永化,刘安华,龚克成.直接由SiO2低温合成含硅聚氨酯及其结构表征[J].高分子学报,2001(06):811-813.
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