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Preparation and Characterization of Degradable Poly (silyl ester) and the Self-crosslinking Reaction of Poly (silyl ester) without Solvent

机译:可降解聚甲硅烷基酯的制备,表征及无溶剂条件下聚甲硅烷基酯的自交联反应

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The new poly (silyl ester) has been prepared by the polycondensation reaction of 1,5dichloro-1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane with di-tert-butyl fumarate by the elimination of tert-butyl chloride as a driving force. To investigate the self-crosslinking reaction of the unsaturated poly (silyl ester), poly (1,1,5,5tetramethyl-3,3-diphenyltrisiloxane) was selfcrosslinked in the presence of 2, 2'-azobis (isobutyronitrile) (AIBN) as a radical initiator without solvent. After the self-crosslinking, the unsaturated poly (silyl ester), which was viscous liquids, turned into solid product. The characterization of the poly (silyl ester) and the self-crosslinked product included 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Comparisons were made between the linear poly(silyl ester) and the self-crosslinked products. It was found that after crosslinking, the important resonance signal for ethenylene (C=C) of the poly (silyl ester) reduced, which show that the crosslinking reaction is carried out. The selfcrosslinked product exist the structures of linear isomer and four-membered ring isomer. The glasstransition temperatures of the self-crosslinked poly (silyl ester) was higher than that of the uncrosslinked poly (silyl ester), and the thermal stability of the self-crosslinked poly (silyl ester) was better than that of uncrosslinked poly(silyl ester).
机译:通过消除叔丁基,将1,5二氯-1,1,5,5-四甲基-3,3-二苯基三硅氧烷与富马酸二叔丁酯缩聚反应制得了新的聚(甲硅烷基酯)。氯化物为动力。为了研究不饱和聚(甲硅烷基酯)的自交联反应,在(2,2'-偶氮双(异丁腈)(AIBN)存在下,将聚(1,1,5,5四甲基-3,3-二苯基三硅氧烷)自交联作为无溶剂的自由基引发剂。自交联后,为粘性液体的不饱和聚(甲硅烷基酯)变成固体产物。聚甲硅烷基酯和自交联产物的表征包括1 H-NMR光谱,差示扫描量热法(DSC)和热重分析(TGA)。在线性聚(甲硅烷基酯)和自交联产物之间进行比较。发现在交联之后,聚(甲硅烷基酯)的对于乙炔(C = C)的重要共振信号降低,这表明进行了交联反应。自交联产物存在线性异构体和四元环异构体的结构。自交联的聚(甲硅烷基酯)的玻璃化转变温度高于未交联的聚(甲硅烷基酯),并且自交联的聚(甲硅烷基酯)的热稳定性优于未交联的聚(甲硅烷基酯) )。

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