摘要
用无定形的二氧化硅和乙二醇在氢氧化钾的催化下低温反应,得到高反应活性的五配位硅钾化合物,再与3-溴丙烯反应,制备出乙烯基四配位硅单体。该单体与苯乙烯通过自由基聚合得到含硅共聚物。对所合成的单体和共聚物进行了红外光谱(IR)、热重分析(TGA)、差示扫描量热谱(DSC)、元素能谱分析(EDS)和凝胶渗透色谱法(GPC)等结构表征与性能测试。IR显示单体中1 649 cm-1处的C=C双键伸缩振动吸收峰在共聚物中消失;EDX表明乙烯基四配位硅的产率为99.61%;TG显示共聚物在310℃才开始失重,具有良好的热稳定性;DSC测得共聚物的玻璃化转变温度为约104℃;GPC测得共聚物数均相对分子质量Mn约64万,重均相对分子质量M_w约125万,分散系数为1.95,而且共聚物有良好的耐水和耐醇性。实验表明,该合成结果可为有机硅材料的合成提供一种低耗、简便的方法。
Organosilicon polymers have good thermal stability and corrosion resistance. Penta-coordinated silicon compound with high reactivity was prepared by the reaction of amorphous silica with ethylene glycol under the catalysis of potassium hydroxide,then reacted with allyl bromide to give a vinyl tetra-coordinate silicon（ VTS） monomer,and copolymer（ poly（ VTS-co-St）） was synthesized by VTS with styrene through the free radical solution polymerization. The VTS monomer and copolymer were characterized by FT-IR,elemental diffraction spectrum（ EDS）,thermo gravimetric analysis（ TGA）,differential scanning calorimetric（ DSC） and gel permeation chromatography（ GPC）. The IR spectrum of VTS monomer shows a absorption band for C = C at 1 649 cm- 1,but the absorption band was disappeared in the copolymers. The EDS indicates the yield of VTS was 99. 61%. TG analysis shows that the poly（ VTC-co-St） begin losing mass at 310℃ which has a good thermal stability. The glass transition temperature of poly（ VTS-co-St） is 104℃,and the GPC data show that the molecular weight of the copolymer is about 640 thousands. And the copolymer has good hydrolysis and alcohol resistance. The experimental results show that it can provide a low energy consumption and simple way to synthesize the organosilicon materials.
出处
《实验室研究与探索》
CAS
北大核心
2016年第6期42-45,共4页
Research and Exploration In Laboratory
关键词
乙烯基四配位硅
自由基聚合
苯乙烯
vinyl tetra-coordinate silicon
free radical polymerization
styrene
