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用XRD、FTIR、IG-DTA、~(13)C魔角固体核磁共振表征了用四甲基乙基二胺(TMEDA)为结构异向剂合成的高硅沸石CF-3及ZSM-39.TMEDA不同基团的~(13)C化学位移,共振峰相对强度在交叉极化(CP)及高功率去偶(HPDEC)核磁共振谱中的变化,揭示出模板分子在尺寸不同的沸石笼中的位置、运动状态及其与骨架的相互作用.在ZSM-39沸石中的TMEDA分子,它的-C_2H_4-基团~(13)C共振峰明显窄化,向高场的异常位移以及它与-CH_3基团~(13)C共振峰相对强度在CP及HPDEC谱中的明显变化,说明为2个相邻的[5~(12)6~4]笼所共有的TMEDA分子,其-C_2H_4-基团与这2个笼所共用的六氧元环的氧原子有强烈的相互作用.
The high-silica zeolites CF-3 and ZSM-39 synthesized by tetramethylethylenediamine (TMEDA) as structural anisotropic agent were characterized by XRD, FTIR, IG-DTA and ~ (13) C magic angle solid state nuclear magnetic resonance. The chemical shifts of ~ (13) C and the relative intensities of the different groups of TMEDA in the cross-polarization (CP) and high-power decoupling (HPDEC) nuclear magnetic resonance spectra revealed that the template molecules were localized in zeolitic cages with different sizes And its interaction with the framework.The TMEDA molecule in ZSM-39 zeolite showed a sharp narrowing of the resonance peak of -C_2H_4- group ~ (13) C, anomalous shift to high field and its interaction with The obvious change of the relative intensity of -CH_3 group ~ (13) C resonance in CP and HPDEC spectra indicates TMEDA molecule shared by two adjacent [5 ~ (12) 6 ~ 4] cages, the C_2H_4 - The group has a strong interaction with the oxygen atoms of the hexacyclo oxygen ring shared by these two cages.