2013
DOI: 10.1039/c3cp44343d
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The fast Z-scan method for studying working catalytic reactors with high energy X-ray diffraction: ZSM-5 in the methanol to gasoline process

Abstract: The methanol to gasoline process over the zeolite catalyst ZSM-5 in a lab-sized reactor bed (4 mm diameter) has been studied in operando with high energy synchrotron X-ray diffraction. The fast z-scan method was used, scanning the reactor repeatedly and at speed through the X-ray beam. The X-ray diffraction data were processed using high throughput parametric Rietveld refinement to obtain real structural parameters. The diffraction data show only very subtle changes during the process and this allows us to dem… Show more

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Cited by 12 publications
(16 citation statements)
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“…In a similar manner, the minor local expansion of the SOD cages around 820 K could also be a response to coke accumulation as there is no second event in the NH 3 related m/z trace ( Figure 5). During the in situ experiments, the powder took on a yellow tint between 473 and 523 K, its tone became darker as the temperature increased, then turned to black and finally white above 900 K. Coke formation leading to unit cell volume expansion has been observed for ZSM-5, SAPO-34 and SAPO-18 [29,[33][34][35][36]. It is worth noticing that the unit cell shrinkage observed in this temperature region is attributed to two different, synergetic mechanisms: the template removal that physically empties the space in the sodalite chages and the material's intrinsic negative thermal expansion.…”
Section: Discussionmentioning
confidence: 97%
“…In a similar manner, the minor local expansion of the SOD cages around 820 K could also be a response to coke accumulation as there is no second event in the NH 3 related m/z trace ( Figure 5). During the in situ experiments, the powder took on a yellow tint between 473 and 523 K, its tone became darker as the temperature increased, then turned to black and finally white above 900 K. Coke formation leading to unit cell volume expansion has been observed for ZSM-5, SAPO-34 and SAPO-18 [29,[33][34][35][36]. It is worth noticing that the unit cell shrinkage observed in this temperature region is attributed to two different, synergetic mechanisms: the template removal that physically empties the space in the sodalite chages and the material's intrinsic negative thermal expansion.…”
Section: Discussionmentioning
confidence: 97%
“…In addition one end of the basic construction of the cell can be attached to a goniometer allowing semi-rotating/swinging mode for improved statistics of the recorded pattern. The description of the experimental set-up can be found elsewhere [29].…”
Section: X-ray Powder Diffractionmentioning
confidence: 99%
“…Advances in automated XRD analysis have allowed synchrotron radiation to be used for real-time process monitoring for catalysts, 33,34 but to our knowledge this is the first report of a lab X-ray source for HT serial screening of metallic nanoparticle catalysts. Meanwhile, HT-TGA has been used for screening catalyst activity at low temperatures, 35 but this is the first report of its use for HT-TPR.…”
Section: Introductionmentioning
confidence: 99%