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Rapid screening of zeolite acidity by thermal response measurements using InfraSORP technology
Microporous and Mesoporous Materials ( IF 5.2 ) Pub Date : 2018-03-30 , DOI: 10.1016/j.micromeso.2018.03.032
Anja Werner , Michelle Wöllner , Paul Bludovsky , Matthias Leistner , Carolin Selzer , Stefan Kaskel

Thermal response measurements using the recently developed InfraSORP technology are nowadays established as a versatile and rapid screening tool for the estimation of physicochemical properties of porous materials, such as adsorption capacity, surface area and porosity. In the present work, InfraSORP experiments are explored for fast screening of zeolite acidity especially for test samples available only in small quantity. Twelve MFI and beta type zeolite samples with varying molar Si/Al ratios were examined using ammonia as test gas (0.5% NH3 in nitrogen). Caused by the exothermic adsorption of ammonia on acidic sites of the zeolite samples, a characteristic temperature response curve (temperature vs. time) is observed. The specific peak area under the curve reflects the total NH3 amount adsorbed. In two consecutive adsorption/desorption runs the contributions of physisorbed and chemisorbed NH3 are distinguished. The difference between the first integral of the thermal response (caused by physisorption and chemisorption of NH3) and a second adsorption cycle (reflecting only weakly adsorbed NH3) correlates directly with the sample acidity determined by conventional temperature-programmed desorption of ammonia (TPD). Calibration of the signal versus established TPD techniques results in excellent correlation and renders the new technique as a promising high-throughput screening tool for zeolite acidity assessment in industrial process and product quality control requiring less than 30 min per sample.



中文翻译:

使用InfraSORP技术通过热响应测量快速筛选沸石酸度

如今,使用最近开发的InfraSORP技术进行的热响应测量已被确立为一种通用且快速的筛选工具,用于评估多孔材料的物理化学特性,例如吸附能力,表面积和孔隙率。在目前的工作中,探索了InfraSORP实验来快速筛选沸石酸度,特别是对于仅少量获得的测试样品。使用氨作为测试气体(氮气中0.5%NH 3)检查了十二份MFI和β型沸石样品,这些样品具有不同的Si / Al摩尔比。由于氨在沸石样品的酸性位置上放热吸附,导致观察到特征温度响应曲线(温度与时间的关系)。曲线下的特定峰面积反映了总NH 3吸附量。在两个连续的吸附/解吸运行中,区分了物理吸附和化学吸附的NH 3的贡献。热响应的第一个积分(由NH 3的物理吸附和化学吸附引起)与第二个吸附循环(仅反映弱吸附的NH 3)之间的差异与通过常规程序升温的氨解吸(TPD)确定的样品酸度直接相关。 )。信号与已建立的TPD技术的校准可产生出色的相关性,并使该新技术成为用于工业过程中沸石酸度评估和产品质量控制的有希望的高通量筛选工具,每个样品少于30分钟。

更新日期:2018-03-30
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