Acidity, catalyst characterization

R530 A. Zheng, S.-J. Huang, S.-B. Liu and F. Deng, Acid Properties of Solid Acid Catalysts Characterized by Solid-State P Nuclear Magnetic Resonance of Adsorbed Phosphorus Probe Molecules , Phys. Chem. Chem. Phys., [online computer file], 2011,13, 14889. 

Catalyst characterization - Characterization of mixed metal oxides was performed by atomic emission spectroscopy with inductively coupled plasma atomisation (ICP-AES) on a CE Instraments Sorptomatic 1990. NH3-TPD was nsed for the characterization of acid site distribntion. SZ (0.3 g) was heated up to 600°C using He (30 ml min ) to remove adsorbed components. Then, the sample was cooled at room temperatnre and satnrated for 2 h with 100 ml min of 8200 ppm NH3 in He as carrier gas. Snbseqnently, the system was flashed with He at a flowrate of 30 ml min for 2 h. The temperatnre was ramped np to 600°C at a rate of 10°C min. A TCD was used to measure the NH3 desorption profile. Textural properties were established from the N2 adsorption isotherm. Snrface area was calcnlated nsing the BET equation and the pore size was calcnlated nsing the BJH method. The resnlts given in Table 33.4 are in good agreement with varions literature data. 

Catalysts Characterization Catalysts were characterized by nitrogen adsorption-desorption isotherms, XRD, XPS, TEM, and FT-IR. The concentration and the strength of the acid sites were determined using a combination of NHs-chemisorption and FTIR. Detailed procedures are given elsewhere [18, 19]. 

In summary, the Avada process is an excellent example of process intensification to achieve higher energy efficiency and reduction of waste streams due to the use of a solid acid catalyst. The successful application of supported HP As for the production of ethyl acetate paves the way for future applications of supported HP As in new green processes for the production of other chemicals, fuels and lubricants. Our results also show that application of characterization techniques enables a better understanding of the effects of process parameters on reactivity and the eventual rational design of more active catalysts. 

Another thermal analysis method available for catalyst characterization is microcalorimetiy, which is based on the measurement of the heat generated or consumed when a gas adsorbs and reacts on the surface of a solid [66-68], This information can be used, for instance, to determine the relative stability among different phases of a solid [69], Microcalorimetiy is also applicable in the measurement of the strengths and distribution of acidic or basic sites as well as for the characterization of metal-based catalysts [66-68], For instance, Figure 1.10 presents microcalorimetry data for ammonia adsorption on H-ZSM-5 and H-mordenite zeolites [70], clearly illustrating the differences in both acid strength (indicated by the different initial adsorption heats) and total number of acidic sites (measured by the total ammonia uptake) between the two catalysts. 

Catalyst characterization by the relative value of slopes, a , is most useful when parallel trends in the properties of the catalysts, measured by other probes, chemical or physical, are discovered. Examples are the estimation of acid strength of the surface sites or the estimation of energy of interaction between surface atoms on the basis of shifts in spectra. All of the quantities used for comparison must be intensive, that is, they must express some form of energy or be proportional to energy. 

Surface Acid-Base Characterization of Containing Group IIIA Catalysts by Using Adsorption Microcalorimetry... 

Measurement of the thermokinetic parameter can be used to provide a more detailed characterization of the acid properties of solid acid catalysts, for example, differentiate reversible and irreversible adsorption processes. For example, Auroux et al. [162] used volumetric, calorimetric, and thermokinetic data of ammonia adsorption to obtain a better definition of the acidity of decationated and boron-modified ZSM5 zeolites (Figure 13.7). 

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