Production of Hematite Micro- and Nanoparticles in a Fluidized Bed Process—Mechanism Study

A continuous, compact and simple process was developed to synthesize micro- and nanoparticles of iron oxide. The process combines the spraying (pulverization) of an aqueous solution of iron nitrate in a fluidized bed reactor containing coarse and hot glass beads ( T = 200 °C) for the production of solids and a transported bed reactor for calcination ( T = 490 °C). The intermediate product formed in the fluidized bed reactor is 2-line ferrihydrite, while the calcination reactor allows the production of hematite micro- and nanoparticles. These particles are characterized by a narrow size distribution, a mean size of 0.5 μm, a specific surface area of 24 m 2 g –1 and a density of 4499 kg m –3 . Particles are made up of small clusters of crystallites having an average size of 47 nm and a low internal porosity (0.12). The reaction mechanism was studied using a muffle furnace and a lab convective dryer. It was found that several steps are involved leading first to the production of iron nitrate dihydrate after the removal of the solution water, as well as two and then five molecules of water of hydration. After that, the elimination of nitrate leads to the production of ferrihydrite. Finally, ferrihydrite is transformed into hematite due to the removal of residual nitrate and water of hydroxylation.