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Electrochemical synthesis of poly(methylsilyne) and investigation of the effects of parameters on the synthesis

机译:聚甲基硅炔的电化学合成及参数对合成的影响

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This study aims to synthesize poly(methylsi-lyne) by electrochemical reduction of methyltrichlorosilane at a constant potential of-6 V, while investigating the effects of parameters such as the nature of the electrode, solvent and supporting electrolyte, the monomer/solvent ratio, and the reaction time on the properties of the products. The polymer was characterized by ~1H-NMR (Proton Nuclear Magnetic Resonance Spectroscopy), FTIR (Fourier Transform Infrared Spectroscopy), UV-Visible Spectroscopy, and TGA (Thermogravimetry Analysis). Copper (Cu) electrodes were used as stainless steel introduced impurities into the system. In an electrolytic media consisting of acetonitrile (AN), sodium dodecyl sulfate (SDS), and Cu electrodes, increasing the monomer/solvent ratio and the reaction time affected the system negatively based on the purity of poly (methylsilyne) in the final product. Reproducible results were only achieved in an electrolytic media containing 1,2-dimethoxyethane (DME) and tetrabutylammonium perchlo-rate (TBAP). In this system, the purity of the products was less dependent on monomer/solvent ratio and reaction time. The color and the ~1H-NMR, FTIR, and UV-Visible spectra proved that the product is poly(methylsilyne). In addition, the significantly high-average decomposition temperature obtained from TGA results revealed that the polymer is a good candidate as an additive for improving thermal stability and flame retardancy in thermoplastics.
机译:这项研究旨在通过在恒定电压为6 V的条件下通过电化学还原甲基三氯硅烷来合成聚(甲基硅烷),同时研究各种参数的影响,例如电极的性质,溶剂和支持电解质,单体/溶剂比,以及反应时间对产品性能的影响。通过〜1 H-NMR(质子核磁共振波谱),FTIR(傅立叶变换红外光谱),UV-可见光谱和TGA(热重分析)对聚合物进行表征。铜(Cu)电极用作将不锈钢引入系统的杂质。在由乙腈(AN),十二烷基硫酸钠(SDS)和Cu电极组成的电解介质中,增加单体/溶剂的比例和反应时间对最终产物中的聚(甲基硅炔)的纯度有负面影响。仅在包含1,2-二甲氧基乙烷(DME)和高氯酸四丁铵(TBAP)的电解质介质中才能获得可重现的结果。在该系统中,产物的纯度较少地依赖于单体/溶剂比和反应时间。颜色和〜1H-NMR,FTIR和UV-可见光谱证明该产物为聚(甲基硅炔)。另外,由TGA获得的明显高的平均分解温度表明,该聚合物是用于改善热塑性塑料的热稳定性和阻燃性的添加剂的良好候选者。

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