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One-step synthesis, characterization and catalytic performance of hierarchical Zn-ZSM-11 via facile ZnO routes

机译：简便的ZnO路径一步法合成Zn-ZSM-11的表征和催化性能

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摘要

Hierarchical Zn-ZSM-11 zeolite with an olive-shaped intergrowth morphology was synthesized via a novel and facile one-step hydrothermal method by using tetrabutylammonium bromide (TBABr) and zinc oxide (ZnO) as a difunctional template and zinc source, respectively. Structural characterizations (XRD, IR, TG-DTA, SEM, and N-2 adsorption-desorption) were conducted to analyze the textural properties of Zn-ZSM-11 samples. Compared with the Zn containing ZSM-11 samples prepared by other methods (ZnSO4 method, ZnO-impregnated-seed method and impregnation method), the Zn-ZSM-11 prepared by ZnO method exhibited enriched mesopores as well as good catalytic activity in methanol conversion. TEM images showed that Zn species were well incorporated into the zeolite framework, while the different morphology of Zn-ZSM-11 from ZSM-11 further verified that the Zn species had been involved in the formation of the ZSM-11 framework. Al-27 and Si-29 MAS NMR spectra revealed that Zn species in the zeolite framework significantly impacted the coordination of Si. The XRD pattern variation of the ZnO containing gel was also tracked to illustrate the crystallization process. It was found that the ZnO would be gradually dissolved under the severely alkaline environment and subsequently incorporated into the ZSM-11 framework in the crystallization process. This facile new synthesis strategy can also be extended to prepare other Zn containing zeolites and is potentially important for practical utilization.
机译：以四丁基溴化铵（TBABr）和氧化锌（ZnO）为双功能模板，通过新颖，简便的一步水热法合成了橄榄形共生形的层状Zn-ZSM-11分子筛。进行结构表征（XRD，IR，TG-DTA，SEM和N-2吸附-脱附）以分析Zn-ZSM-11样品的织构特性。与通过其他方法（ZnSO4方法，ZnO浸渍种子方法和浸渍方法）制备的含锌ZSM-11样品相比，通过ZnO方法制备的Zn-ZSM-11具有丰富的中孔和良好的甲醇转化催化活性。 TEM图像表明，Zn物种已很好地结合到沸石骨架中，而ZSM-11与Zn-ZSM-11的不同形态进一步证实了Zn物种已参与ZSM-11骨架的形成。 Al-27和Si-29 MAS NMR光谱表明，沸石骨架中的Zn物种显着影响Si的配位。还跟踪了含ZnO的凝胶的XRD图谱变化，以说明结晶过程。发现ZnO将在强碱性环境下逐渐溶解，随后在结晶过程中掺入ZSM-11骨架。这种简便的新合成策略也可以扩展到制备其他含锌沸石，并且对于实际应用可能具有重要意义。

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