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机构地区:[1]北京化工大学北京市新型高分子材料制备与成型加工重点实验室,北京100029
出 处:《合成橡胶工业》2009年第3期184-187,共4页China Synthetic Rubber Industry
基 金:国家自然科学基金资助项目(50573005)
摘 要:以正丁基锂(简称L i)为引发剂、四氢呋喃为调节剂、环己烷为溶剂,通过负离子聚合法合成溶聚丁苯橡胶(SSBR),在聚合后期加入六甲基环三硅氧烷(D3)和促进剂N,N-二甲基甲酰胺(DMF),合成了SSBR-聚二甲基硅氧烷共聚物,考察了DMF用量、反应温度、反应时间对D3转化率的影响,研究了丁苯大分子链末端基种类对共聚反应的影响,并用傅里叶变换红外光谱、1H-核磁共振、差示扫描量热法对共聚物进行了表征。结果表明,在DMF/L i(摩尔比)为80、反应温度为60℃、反应时间为6 h的条件下,D3转化率达到73%;当丁苯大分子活性链末端为丁二烯端基时,能更有效地引发D3共聚合。Solution polymerized butadiene-styrene rubber(SSBR) was synthesized by anionic solution copolymerization of butadiene/styrene with initiator n-BuLi( simplified as Li) , modifier tetrahydrofuran, and solvent cyclohexane. During the later stage of polymerization, monomer hexamethylcyelotrisiloxane ( D3 ) and promoter N, N-dimethylformamide (DMF) were added into the system to synthesize SSBR- polydimethylsiloxane ( PDMS ) copolymer. Effects of DMF/Li (mole ratio), reaction time, and reaction temperature on conversion of D3 were studied. Influence of types of the macromolecular living chain end groups of SSBR on copolymerization was also investigated. Microstructures of SSBR-PDMS copolymer were characterized by Fourier transform infrared spectroscopy, nuclear magnetic resonance and differential scanning calorimetry. The results showed that when DMF/Li ( mole ratio) was 80, reaction temperature was 60 ℃ and reaction time was 6 h, the conversion of D3 reached 73%. Compared with living chain ends of polystyrene, the living chain ends of polybutadiene could initiate polymerization of D3 more efficiently.
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