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Preparation and characterization of silicone rubber cured via catalyst-free aza-Michael reaction

机译：无催化剂AZA-MICHAEL反应的硅橡胶的制备与表征

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This paper proposes for the first time a strategy for preparing silicone rubber cured by aza-Michael reaction. A novel compound, γ-piperazinylpropylheptamethylcyclotetrasiloxane (D _(3) D ~(PyP) ), was synthesized to produce high-molecular-weight poly[(piperazinylpropyl)methylsiloxane- co -dimethylsiloxane] (PyP-PDMS) by a base equilibration reaction with octamethylcyclotetrasiloxane (D _(4) ). Then, silicone rubber was obtained with PyP-PDMS as the gum, oligo[(acryloxypropyl)methylsiloxane- co -dimethylsiloxane] (AP-PDMS) as the crosslinker, and silica as the filler. The crosslinking mechanism was validated by solid-state ~(13) C NMR spectroscopy. The curing process was analyzed by cure-curves performed by rheometry. The effects of various factors, such as post-cure temperature and time, crosslinker and filler amounts, molecular weight, and piperazine group content, on the mechanical properties of the novel silicone rubber were investigated in detail. Vulcanizate with tensile and tear strengths of 11.43 MPa and 30.72 kN m ~(?1) , respectively, was obtained. The cure was free of catalysts, and the cure temperature is not too high (120 °C). Our method yielded silicone rubber of high strength and stable dimension. The synthesized silicone rubber also exhibited favorable thermal stability, low temperature performance, and hydrophobic properties, as characterized by Thermogravimetric Analysis, Differential Scanning Calorimetry and static contact-angle analysis.
机译：本文提出首次制备由AZA-Michael反应固化的硅橡胶的策略。合成一种新型化合物，γ-哌嗪基丙二酰氯甲烷（D _（3）D〜（PY）），通过基础平衡反应生产高分子量多[（哌嗪基丙基）甲基硅氧烷 - 共二甲基硅​​氧烷]（PYP-PDMS）含八甲基甲基环四硅氧烷（D _（4））。然后，用PYP-PDMS作为胶，作为胶，寡核苷酸，作为交联剂的寡核苷酸，作为填料的二氧化硅，硅橡胶，作为交联剂，以及二氧化硅作为填料。通过固态〜（13）C NMR光谱验证交联机理。通过流变学进行的固化曲线分析固化过程。详细研究了各种因素，例如治愈后温度和时间，交联剂和填料，分子量和哌嗪基含量的各种因素对新型硅橡胶的机械性能进行研究。得到硫化含量，分别具有11.43MPa和30.72kN m〜（β1）的拉伸和撕裂强度。固化是没有催化剂的，固化温度不是太高（120℃）。我们的方法得到了高强度和稳定尺寸的硅橡胶。合成的硅橡胶还表现出良好的热稳定性，低温性能和疏水性质，其特征在于热重分析，差示扫描量热法和静态接触角分析。

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