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Title:: Synthesis and structure analysis of fluorosilicone copolymer raw rubber

Author(s):: ZHU Yan-yan; ZHANG Yu-lin; LI Ling-ling; ZHANG Sai; QIAO Wen-qiang; WANG Zhi-yuan; Department of Polymer Materials, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China

Keywords:: fluorosilicone copolymer raw rubber; 1; 3; 5-tris（3; 3; 3- trifluoropropyl）-1; 3; 5-trimethylcyclotrisiloxane; segment content; molecular weight

摘要:: 以1，3，5-三（3，3，3-三氟丙基）-1，3，5-三甲基环三硅氧烷（D3F）和六甲基环三硅氧烷为原料合成了高分子量的氟硅共聚生胶，研究了反应时间和反应温度对产物分子量的影响，以及单体投料比对共聚物链节含量的影响。通过红外光谱和核磁共振波谱对共聚生胶的结构进行了表征，并用乌氏黏度计测定了其分子量。结果表明，在D3F用量较高时氟硅生胶中其链节含量的占比与投料占比更为接近。随着反应温度升高和时间的延长，聚合产物的分子量均先增大后减小，而通过在反应过程中适当节点停止加热的方式可有效提高氟硅生胶的分子量。在反应温度为90 ℃、反应时间为10 min及D3F投料摩尔分数为80%时，氟硅共聚生胶的分子量最高，黏均相对分子质量可达8.2×105。

Abstract:: 1,3,5-tris（3,3,3-trifluoropyl）-1,3,5-trimethylcyclotrisiloxane （D3F） and hexamethylcyclotrisiloxane were used as raw materials to synthesize fluorosilicone copolymer with high molecular weight. The effects of reaction time and reaction temperature on molecular weight of the products and monomer ratio on chain segment content of the copolymers were studied. The structure of the copolymer was characterized by infrared spectroscopy and nuclear magnetic resonance spectroscopy, and its molecular weight was determined by Ubbelohde viscometer. The results showed that the proportion of chain segment content in fluorosilicone rubber was closer to that of feed when D3F amount was high. With increase of reaction temperature and time, molecular weight of the fluorosilicone copolymer first increased and then decreased. Molecular weight of fluorosilicone copolymer could be effectively increased by stopping heating at an approp-riate node in the reaction process. When the reaction temperature was 90 ℃, reaction time was 10 min and mole fraction of D3F was 80%, molecular weight of fluorosilicone copolymer reached the maximum, and the viscosity average molecular weight was 8.2×105.