Vibro-assisted fluidization of cohesive micro-silica has been studied by means of X-ray imaging, pressure drop measurements, and off-line determination of the agglomerate size. Pressure drop and bed height development could be explained by observable phenomena taking place in the bed; slugging, channeling, fluidization or densification. It was observed that channeling is the main cause of poor fluidization of the micro-silica, resulting in poor gas-solid contact and little internal mixing. Improvement in fluidization upon starting the mechanical vibration was achieved by disrupting the channels. Agglomerate sizes were found to not significantly change during experiments.

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Stirred gas–solid fluidized bed reactors are commercially employed in polyolefin manufacturing, but the complex gas–solid contacting dynamics pose challenges in design, scale-up, and operation. In this study, the influence of agitation on the fluidization performance of Geldart B particles was investigated experimentally by X-ray imaging and pressure drop measurements and numerically by Computational Fluid Dynamics (CFD) - Discrete Element Method (DEM) - Immersed Boundary Method (IBM). The experimentally obtained minimum fluidization curve and time-averaged pressure drop show good qualitative agreement with the simulation results. Visual observations underscore that an increase in the angular velocity of the agitator results in reduced bubble size and improved bed homogeneity, as further evidenced by reduced pressure fluctuations. Furthermore, the simulations reveal that while the impeller enhances solids agitation, a proper design study is imperative, considering that static immersed bodies, such as the stirrer shaft, can adversely impact solids motion.@en

In this study, the impact of different vibrational modes on the fluidization characteristics of cohesive micro- and nano-silica powder was examined. Fractional pressure drop, bed expansion measurements, and X-ray imaging were utilized to characterize the fluidization quality. The densities of the emulsion phase at the top and bottom of the column were quantified and compared, providing insights into the solid distribution within the fluidized bed. In the absence of vibration, neither powder could be fluidized within the considered range of superficial gas velocities. Vertical vibration was found to initiate fluidization for both powders. In contrast, elliptical vibration failed to overcome the channelling behavior when fluidizing the micro-powder. For nano-powder, combined channelling and powder compaction occurred when the bed was subjected to elliptical vibration. For the micro-powder, it was observed that bed homogeneity was independent of vertical vibration intensity but improved with increasing superficial gas velocity. For nano-powder, intensifying vertical vibration led to segregation, likely due to agglomerate densification. Furthermore, fractional pressure drop measurements proved to be a strong tool in assessing fluidization quality, providing insights that could not be attained by conventional indicators.

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Stirring has been recognized in the literature as a promising technique for facilitating fluidization of cohesive powders, via inputting additional energy to counteract interparticle forces. However, the influence of operating conditions and stirrer configurations on flow behavior remains largely unknown, which impedes the practical implementation of stirred fluidization. Utilizing X-ray imaging, this research demonstrates that stirring enhances fluidization in cohesive micron-silica powder (Sauter mean diameter [Formula presented]) by collapsing the powder packing structure, and transitioning channeling beds into bubbling states. Comb-like configurations featuring fewer stirrers and blades, placed in the bottom region, have shown to be highly effective. Excessive stirring can lead to air pockets and a compacted phase of particles on the column walls, undermining the interaction between particles and stirrers. Additionally, the experiments show that maximizing the sweeping coverage, employing complex asymmetrical configurations, and avoiding tortuous gas pathways are preferable.

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For dry powder inhaled formulations, good flow behaviour is vital in re-dispersing the powder. However, inhaled drug powders with a particle size below 10 µm are classified as highly cohesive materials with poor flow characteristics. Here we demonstrate how to alter the flow properties of micronized budesonide powders by depositing different materials (organic, inorganic, and hybrid organic–inorganic) in the forms of nanoscale films onto the drug particles using atomic/molecular layer deposition (ALD/MLD) coatings. The angle of repose (static) and pneumatic delivery measurements were performed to access the flow characteristics. The flowability can be effectively improved with the growth of inorganic nanofilm (SiO₂, TiO₂, or Al₂O₃) via ALD and hybrid nanofilm (titanicone) via combined ALD-MLD coating. This improvement is reflected by the decrease in the angle of repose and minimum pick-up velocity (U_pu), as well as promoting the pneumatic delivery of a much larger amount of drug powders after ALD or hybrid coating. In contrast, the organic PET coated budesonide via MLD exhibits comparable poor flow characteristics as the uncoated budesonide. Rather than being transported in individual particles, the uncoated or PET-coated budesonide powders are pneumatically delivered in form of complex clusters with a size of over 500 μm, whereas the ALD budesonide is dispersed in form of small agglomerates (<100 μm). Despite the difference in agglomerate size, entraining behaviors of all samples agree well with the prediction of Kalman's pick-up Zone I correlation. The inorganic nanofilm deposited via ALD alters the surface chemistry to reduce the inter-particle forces measured by atomic force microscopy, giving rise to an improved drug delivery performance. Nanoscale surface modification of dry powder particles has good potential for inhaled drug delivery enhancement.

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Mechanical vibration has been broadly used to assist fluidization of cohesive powders, because of its capability to disrupt gas channels and agglomerates. However, the improvement reported in literature is mostly deduced from bulk response and ex-situ measurements, whereas the induced fluidization behavior and underlying physics remain largely unexplored. In this work, the fluidization behavior of micron-sized cohesive silica (Sauter mean diameter D₃₂ = 7.9 μm) has been investigated experimentally under vibration of varying conditions. X-ray imaging was carried out to directly capture the temporal evolution of system hydrodynamics, and identify in-situ powder stratification, bubbling and channel formation. The study demonstrates that vibration effectively collapses gas channels, yet facilitates powder stratification and compaction, therefore developing three distinctive flow regions inside the bed with different fluidization states. Consequently, common measurements, such as pressure drop and bed expansion, tend to overestimate the improvement. In addition, increasing frequency, from 10 Hz to 30 Hz, is observed to increase the number of bubbles by 60 %, whereas a large amplitude (e.g., 2 mm) leads to a 10 % compaction in the top flow region.

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The fluidization of cohesive powders has been extensively researched over the years. When looking at literature on the fluidization of cohesive particles, one will often find papers concerned with only micro- or only nano-sized powders. It is, however, unclear whether they should be treated differently at all. In this paper, we look at differences and similarities between cohesive powders across the size range of several nanometres to 10s of micrometres. Classification of fluidization behaviour based on particle size was found to be troublesome since cohesive powders form agglomerates and using the properties of these agglomerates introduces new problems. When looking at inter-particle forces, it is found that van der Waals forces dominate across the entire size range that is considered. Furthermore, when looking into agglomeration and modelling thereof, it was found that there is a fundamental difference between the size ranges in the way they agglomerate. Where the transition between the types of agglomeration is located is, however, unknown. Finally, how models are made and agglomerate sizes are measured is currently insufficient to accurately predict or measure their sizes consistently.

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Pressure and temperature are the most important state variables for monitoring physicochemical processes to detect deviations that might lead to explosions and to verify levels, flow rate, and solids/gas hold-up. Pressure fluctuations in multi-phase systems identify regime changes and flow anomalies. Pressure signals are the first indicator of a process upset and are tied into distributed control systems (DCS) to sound alarms when they drift to high or low and activate safety interlocks in the case of high, high-high, low, and low-low conditions. To maximize the information, it requires that pressure gauges (transducers) are installed and calibrated precisely. Pressure measuring devices include manometers, aneroid devices like bellows and Bourdon gauges, and electronic instruments—piezoresistive, piezoelectric, and capacitive. The electronic elements have the advantage of higher precision and faster response times to measure fluctuations. The Bourdon gauges are standard equipment for pressure regulators and are mounted on the exterior of vessels and pipes to facilitate visual inspections. Over 2 million articles indexed by the Web of Science Core collection mention pressure, and in 2021, chemical engineering ranks had over 7000 articles—only multidisciplinary material sciences and energy and fuels had more. A bibliometric analysis identified five research clusters: temperature, combustion, and kinetics; separation, membranes, and energy efficiency; carbon dioxide (capture and storage), water, and thermodynamics; methane, adsorption, and transport phenomena (e.g., diffusion and permeability); and modelling, optimization, and computational fluid dynamics (CFD).

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