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Method for Preparing Polyaluminocarbosilane

机译:聚铝碳硅烷的制备方法

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Polyaluminocarbosilane (PACS) was synthesized directly by the one-pot reaction of polydimethylsilane (PDMS) with aluminum acetylacetonate [Al(acac)(3)] in an autoclave. In this closed system, all the aluminum in Al(acac)(3) was converted into PACS. Therefore, the content of aluminum could be readily controlled quantitatively. On the basis of Fourier transform infrared, H-1-NMR, C-13-NMR, Si-29-NMR, and Al-27 magic-angle spinning NMR analysis, the reaction mechanism was proposed as follows: PDMS dissociated during pyrolysis to generate silicon free radicals, and then they reacted with Al(acac)(3) to yield PACS containing (Si-O)(n)Al groups (n = 4, 5, or 6). Mean while, these reactions resulted in the cleavage of O-C and/or O=C bonds in Al(acac)(3). Some of the free-radical fragments generated by this cleavage continued to react with the silicon free radicals and were incorporated into the structural units of PACS; the rest of them may have been converted into small oxygen-containing compounds, which were removed in the subsequent processing after the reactions.
机译:聚铝碳硅烷(PACS)是通过聚二甲基硅烷(PDMS)与乙酰丙酮铝[Al(acac)(3)]的一锅法直接合成的。在此封闭系统中,Al(acac)(3)中的所有铝都转化为PACS。因此,铝的含量可以容易地定量控制。根据傅立叶变换红外光谱,H-1-NMR,C-13-NMR,Si-29-NMR和Al-27幻角旋转NMR分析,提出了以下反应机理:PDMS在热解过程中解离为生成硅自由基,然后它们与Al(acac)(3)反应生成包含(Si-O)(n)Al基(n = 4、5或6)的PACS。同时,这些反应导致Al(acac)(3)中的O-C和/或O = C键断裂。由这种裂解产生的一些自由基片段继续与硅自由基反应,并被引入到PACS的结构单元中。它们的其余部分可能已转化为小的含氧化合物,在反应后的后续处理中将其除去。

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