端烷氧基聚甲基三氟丙基硅氧烷的合成、表征和室温交联特性
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北京化工大学

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Synthesis, characterization and room temperature crosslinking characteristics of alkoxy-terminated poly(methyltrifluoropropyl)siloxanes
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    摘要:

    以α,ω-端羟基聚甲基三氟丙基硅氧烷为初始聚合物,通过与含氢硅氧烷脱氢缩合合成了分子量、官能度和官能团各异的六种氟硅聚合物(M1~M4、M5和E1)。通过傅里叶变换红外光谱和核磁共振波谱对封端聚合物进行了表征,并通过流变学手段研究了聚合物在室温交联硫化过程中粘度(η)和模量(G′和G″)的变化,为交联反应速率提供依据。结果表明,封端聚合物在不外加交联剂时亦能发生自交联。当采用同一交联剂(M1)时,与初始聚合物(H4)相比,封端后的聚合物(M4)具有快得多的粘度上升趋势和交联反应速率,溶胶-凝胶转变点的时间由2h以上缩短为22.5min,原因在于烷氧基封端大大降低了三氟丙基侧基对活性端基的屏蔽作用,因而反应性大大提高。以M2~M4为基础聚合物制得的氟硅密封胶,具有较好的交联密度、力学性能和耐高低温性能。

    Abstract:

    Six alkoxy-terminated fluorosilicone polymers (M1 ~ M4, M5, and E1) with different molecular weight and functionality were synthesized from α,ω-hydroxyl-terminated poly(methyltrifluoropropyl)siloxanes through their dehydrogenation condensation end-capping reaction with various hydrosiloxanes. The molecular structure was confirmed by FT-IR and NMR spectroscopy, and rheological methods were utilized to determine the viscosity (η) and modulus (G′ and G″) during room temperature crosslinking process. Results show that alkoxy-terminated fluorosilicone polymers own self-crosslinking property without any crosslinking agent added. When low-molecular-weight polymer M1 was selected as crosslinking agent, M4 exhibited more rapid viscosity rise and faster crosslinking rate compared with its precursor H4, and the gel time was sharply shortened from over 2h to 22.5 min. The reason is that alkoxy-termination greatly reduced the shielding effect of bulky trifluoropropyl on the reactivity of active endgroups. Fluorosilicone sealants based on M2~M4 exhibited high crosslinking density, mechanical properties, and high-and-low temperature performance.

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  • 收稿日期:2021-09-05
  • 最后修改日期:2022-02-14
  • 录用日期:2022-03-26
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