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A new developed extal loop airlift slurry reactor, which was integrated with gas–liquid–solid three-phase mixing, mass transfer, and liquid–solid separation simultaneously, was deemed to be a promising slurry reactor due to its prominent advantages such as achieving continuous separation of clear liquid from slurry and cyclic utilization of solid particles without any extra energy, energy-saving, and intrinsic safety design. The principal op-erating parameters, including gas separator volume, handling capacity, and superficial gas velocity, are system-atically investigated here to promote the capabilities of mixing, mass transfer, and yield in the pilot extal loop airlift slurry reactor. The influences of top clearance and throughput of the clear liquid on flow regime and gas holdup in the riser, liquid circulating velocity, and volumetric mass transfer coefficient with a typical high solid holdup and free of particles are examined experimentally. It was found that increasing the gas separa-tor volume could promote the liquid circulating velocity by about 14.0%at most. Increasing the handling capacity of the clear liquid from 0.9 m3·h?1 to 3.0 m3·h?1 not only could increase the output without any adverse con-sequences, but also could enhance the liquid circulating velocity as much as 97.3%. Typical operating conditions investigated here can provide some necessary data and guidelines for this new extal loop airlift slurry reactor to upgrade its performances.