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
作者单位
邹晓川 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
傅相锴 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
李跃东 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
龚必伟 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
陈俊显 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
涂小波 西南大学化学化工学院应用化学研究所重庆 400715
重庆市应用化学市级重点实验室重庆 400715 
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
基金项目: 
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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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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