Continuous reaction crystallization of struvite from phosphate(V) solutions containing calcium ions

Continuous reaction crystallization of struvite from water solutions containing phosphate(V) (1.0 mass%) and calcium ions (from 0.01 to 0.20 mass%) was investigated. Process was carried out in temperature 298 K in continuous DT MSMPR type crystallizer with internal circulation of suspension. Influence of pH (from 9 to 11) and mean residence time of suspension in crystallizer (from 900 to 3600 s) on product crystal size distribution, mean size, population homogeneity and shape of crystals, as well as chemical composition of solid phase was tested. Within the investigated process parameter ranges struvite crystals of mean size from 18 to ca. 50 mu m were produced. With the increase in calcium ions concentration in a feed mean crystal size decreased from 34.2 to 18.4 mu m (pH 9, tau 900 s). Coexistence of struvite and hydroxyapatite crystals in the solid product was confirmed analytically (Ca content in solid product from 0.3 to 8.4 mass%). Presence of calcium ions favoured crystallization of struvite in a form of tubular crystals, characterized by lengthwise cracks and irregular edges. Co-precipitated hydroxyapatite particles showed relatively small sizes, even below 1 mu m, forming agglomerates on the surface of larger struvite crystals and individual agglomerates. (C) 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim