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Zeolite rho loaded with methylamines .1. Monomethylamine loadings

机译:载有甲胺的rho沸石1。一甲胺负载量

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Samples of two differently prepared zeolite rho loaded with different amounts of monomethylamine (MMA) were studied in their hydrated and dehydrated forms by X-ray and neutron diffraction. Both zeolites are partially dealuminated, as indicated by nonframework alumina, which is assumed to be Al2O3 or AlOOH. Series I was prepared from dry-calcined NH4-rho at 873 K, series II from steam-calcined NH4-rho at 773 K. The samples were loaded with different amounts of deuterated MMA, Rietveld refinements yielded the following results for series I (dry): (1) H-3.8(H-MMA)(5)Cs0.2Al9Si39O96.Al2O3.28H(2)O, X-ray data collection at room temperature, , a 14.9991 (2) Angstrom, R-wp = 0.095; (2) composition as in (1), anhydrous and deuterated, neutron data collected at 5 K, disproportionation into two phases in , with a = 14.8410(7) and 14.5273(11) Angstrom, R-wp 0.038; (3) (H-MMA)(8.8)C0.2Al9Si39O96.Al2O3.25H(2)O, X-ray data collection at room temperature, , a = 14.9771 (2) Angstrom, R-wp = 0.090. Series II (steam): (4) H-0.3(H- MMA)(5)Cs0.7Al6Si42O96.2.5Al(2)O(3).23H(2)O, X-ray data collected at room temperature, , a = 15.0323 (2) Angstrom, R-wp = 0.124; (5) composition as in (4), anhydrous and deuterated, neutron data collected at 5 K, disproportionation into two phases in with a = 14.9151 (2) and 14.6475 (8) Angstrom, R-wp = 0.031. In the hydrated samples MMA resides on the center axis in the alpha-cage with the N atoms pointing to the single eight-ring; upon dehydration it migrates into the double eight-rings.
机译:通过X射线和中子衍射研究了水合和脱水形式的两种不同制备的负载有不同量的单甲胺(MMA)的沸石样品。如非骨架氧化铝所示,两种沸石都被部分脱铝,假定为Al2O3或AlOOH。 I系列是由873 K的干法煅烧NH4-rho制备的,II系列是由773 K的蒸汽煅烧的NH4-rho制备的。样品中装有不同量的氘代MMA,Rietveld精制法得到了I系列的以下结果(干燥):(1)H-3.8(H-MMA)(5)Cs0.2Al9Si39O96.Al2O3.28H(2)O,室温X射线数据收集,,14.9991( 2)埃,R-wp = 0.095; (2)(1)中的成分,在5 K下收集的无水和氘化的中子数据,在上歧化成两相,a = 14.8410(7)和14.5273(11)埃,相对湿度0.038; (3)(H-MMA)(8.8)C0.2Al9Si39O96.Al2O3.25H(2)O,室温X射线数据收集,,a = 14.9771(2)埃, R-wp = 0.090。系列II(蒸汽):(4)H-0.3(H-MMA)(5)Cs0.7Al6Si42O96.2.5Al(2)O(3).23H(2)O,在室温下收集的X射线数据,<在条m>上的Im(3),a = 15.0323(2)埃,R-wp = 0.124; (5)(4)中的成分,在5 K下收集的无水和氘化的中子数据,在中歧化成两相,其中a = 14.9151(2)和14.6475(8)Angstrom,R -wp = 0.031。在水合样品中,MMA位于α-笼中的中心轴上,N个原子指向单个八环。脱水后,它迁移到双八环中。

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