U. Lohse , B. Parlitz , D. Müller , E. Schreier , R. Bertram , R. Fricke
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引用次数: 11
摘要
以环己胺(结构44和5)和四乙基氢氧化铵(结构34)为模板剂制备了含镁分子筛MgAPO-44、MgAPO-34 (CHA)和MgAPO-5 (AFI)。用微波功率系统在473 K下进行结晶。采用化学分析、热分析、吸附测定、量热法测定NH3吸附差摩尔热、程序升温解吸、红外光谱和MAS NMR等方法对样品进行表征。对于合成样品,高达7.7 wt%的MgO被纳入CHA结构的晶格位置并取代铝。合成的类恰辉石样品(MgAPO-44和MgAPO-34)的反卷积31P核磁共振信号的相对强度取决于模板分子的类型。然而,煅烧样品(723 K)显示出几乎相同的结果,可以根据不同的31P(4 n Al, n Mg)环境来解释。根据核磁共振结果推导出镁原子的随机分布。Mg的掺入产生了分离的桥接羟基。随着Mg含量的增加,结构坍塌温度降低。
MgAPO molecular sieves of CHA and AFI structure — Acidity and Mg ordering
Magnesium containing molecular sieves, viz. MgAPO-44, MgAPO-34 (CHA) and MgAPO-5 (AFI), were prepared with cyclohexylamine (structures 44 and 5) and tetraethylammonium hydroxide (structure 34) as templating agents. The crystallization was performed at 473 K by means of a microwave power system. The samples were characterized by chemical analysis, thermal analysis, adsorption measurements, calorimetric measurement of the differential molar heat of NH3 sorption, temperature-programmed NH3 desorption, infrared spectroscopy and MAS NMR spectroscopy. For the as-synthesized samples, up to 7.7 wt% of MgO is incorporated into lattice positions of the CHA structure and substitutes aluminum.
The relative intensities of the deconvoluted 31P NMR signals of the as-synthesized chabazite-like samples (MgAPO-44 and MgAPO-34) depend on the type of templating molecules. The calcined samples (723 K), however, showed nearly identical results which could be interpreted in terms of different 31P(4 n Al, n Mg) environments. A random distribution of the Mg atoms is deduced from the NMR results.
The incorporation of Mg creates isolated bridging hydroxyls. The temperature of the structure collapse decreases with increasing Mg content.