晶态层状苯乙胺-N,N-双甲基膦酸锆的合成及层间距异常分析 |
Synthesis of Crystalline Layered Zirconium Phenylethylamino-N,N-bis Methylphosphonates and Analysis for Its Novel Interlayer Distance |
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摘要: 本文用氢氟酸络合法合成了高结晶度的苯乙胺-N,N-双甲基膦酸锆(ZBEDP),用1H NMR、31P NMR、FTIR 、TG-DSC、XRD和SEM对其进行了结构表征和形貌分析。热重研究表明该化合物具有较好的热稳定性,直到400 ℃层状结构才开始破坏。XRD和SEM结果表明ZBEDP具有典型的层状结构,其层间距(1.70 nm)比α-ZrP(0.76nm)增加了0.94 nm。有趣的是ZBEDP的层间距比少一个C原子的苄胺-N,N-双甲基膦酸锆(ZBMDP)减少了0.06 nm,与烷胺双膦酸锆的层间距线性关系相反。ZBEDP层间距反常现可能是-NCH2CH2C6H5部分在层板间的空间排列不同于ZBMDP所致。 |
关键词: 苯乙胺 苯乙胺-N,N-双甲基膦酸 苯乙胺-N,N-双甲基膦酸锆 层状化合物 层间距 |
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Abstract: Zirconium phenylethylamino-N,N-bis methylphosphonate (ZBEDP) with high crystalline was synthesized in the presence of HF in this paper, this compound was well characterized by 1H NMR, 31P NMR, FTIR, TG-DSC, XRD and SEM. The result showed that the ZBEDP possess a high thermal stability by TG-DSC analysis, the layered structure wasn′t be destroyed till 400 ℃. Meanwhile, the results showed that the ZBEDP is a typical layered compound by XRD and SEM, with the interlayer distance(1.70 nm) increasing 0.940 nm comparing to α-ZrP, however,an interesting thing is that the interlayer distance of ZBEDP decreased 0.060 0 nm comparing to Zirconium phenzylamino-N,N-bis methylphosphonate (ZBMDP), which is opposite to the linear relation of Zirconium alkylamino-N,N-bismethylphosphonate′ interlayer distance. The novel interlayer distance of ZBEDP differing from ZBMDP is likely to the difference of space arrangement for C6H5CH2CH2N-. |
Keywords: phenylethylamine phenylethylamino-N,N-bis-methylphosphonic zirconium phenylethylamino-N,N-bis methylphosphonate layered compounds interlayer distance |
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全文下载次数: 1965 |
邹晓川,傅相锴,李跃东,龚必伟,陈俊显,涂小波.晶态层状苯乙胺-N,N-双甲基膦酸锆的合成及层间距异常分析[J].无机化学学报,2009,25(2):290-295. |
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