合成橡胶工业 |
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六甲基环三硅氧烷改性溶聚丁苯橡胶 龙平 张兴英 摘 要:以正丁基锂(简称Li)为引发荆、四氢呋喃为调节剂、环已烷为溶剂,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(D_3)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D_3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/Li(摩尔比)为80、反应温度为60℃、反应时间为6 h的条件下,D_3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D_3共聚合. Solution polymerized butadiene-styrene rubber modified with hexamethylcyclotrisiloxane Long Ping(Key Laboratory of Beijing City on Preparation and Processing of Novel Polymer Materials,Beijing University of Chemical Technology,Beijing 100029,China) Zhang Xingying (Key Laboratory of Beijing City on Preparation and Processing of Novel Polymer Materials,Beijing University of Chemical Technology,Beijing 100029,China) Abstract: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 hexamethylcyclotrisiloxane (D_3) 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 D_3 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 D_3 reached 73%.Compared with living chain ends of polystyrene,the living chain ends of polybutadiene could initiate polymerization of D_3 more efficiently. |
基金项目:国家自然科学基金资助项目(50573005). 作者简介:龙平(1981-),男,硕士研究生. 作者单位:龙平(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) 张兴英(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) 参考文献:
[1]曹湘洪,张爱民.溶液聚合合成橡胶节能技术和节能型橡胶的开发[J].中国工程学,2001,3(7):59-63. |
收稿日期:2008年3月4日 修稿日期:2009年1月8日 出版日期:2009年5月15日 |