Influence of solution constituents, solution conditioning and seeding on the crystalline phase of aluminium hydroxide using in situ X-ray diffraction

Abstract

Filtering, drying and aging of crystalline solids can affect crystalline phase(s) and therefore ex situ X-ray diffraction is not necessarily indicative of the in situ crystalline components. This paper examines some of the factors affecting the crystallised phase of aluminium hydroxides in highly caustic solutions. Caustic aluminate solutions were prepared using several different methodologies. Where solutions were prepared from aluminium metal, gibbsite and bayerite were observed to be the crystallisation products. Where gibbsite was used as the aluminium source in the liquors, the crystallised phase was found to be a function of solution conditioning. Solutions prepared at 100°C and at atmospheric pressure crystallised to form only gibbsite. These same solutions subsequently heated to 160°C for 16 h crystallised as gibbsite and bayerite. It has been concluded from these results that the caustic aluminate solutions made using gibbsite were not dissolved on the molecular scale (although optically clear) if the solutions were heated to only 100°C. Further heating at elevated temperatures completed the dissolution process so that the species in solution were similar to those found in solutions made from aluminium metal. Solutions seeded with either bayerite or gibbsite crystallised to form only gibbsite. Only crystallisation in the bulk solution and not on the seed surfaces was recorded. In some cases seeding altered the expected crystallisation products, i.e. from gibbsite and bayerite to only gibbsite.