N. Hutnik

Phosphates (V) recovery from phosphorus mineral fertilizers industry wastewater by continuous struvite reaction crystallization process.

Continuous DT MSMPR (Draft Tube Mixed Suspension Mixed Product Removal) crystallizer was provided with typical wastewater from phosphorus mineral fertilizers industry (pH < 4, 0.445 mass % of PO4(3-), inorganic impurities presence), dissolved substrates (magnesium and ammonium chlorides) and solution alkalising the environment of struvite MgNH4PO4·6H2O reaction crystallization process. Research ran in constant temperature 298 K assuming stoichiometric proportions of substrates or 20% excess of magnesium ions. Influence of pH (8.5-10) and mean residence time (900-3600 s) on product size distribution, its chemical composition, crystals shape, size-homogeneity and process kinetics was identified. Crystals of mean size ca. 25-37 μm and homogeneity CV 70-83% were produced. The largest crystals, of acceptable homogeneity, were produced using 20% excess of magnesium ions, pH 9 and mean residence time 3600 s. Under these conditions nucleation rate did not exceed 9 × 10(7) 1/(s m(3)) according to SIG (Size Independent Growth) MSMPR kinetic model. Linear crystal growth rate was 4.27 × 10(-9) m/s. Excess of magnesium ions influenced struvite reaction crystallization process yield advantageously. Concentration of phosphate(V) ions decreased from 0.445 to 9.2 × 10(-4) mass %. This can be regarded as a very good process result. In product crystals, besides main component - struvite, all impurities from wastewater were detected analytically.

Reaction crystallization of struvite in a continuous DTM type crystallizer with a compressed air driven jet pump

Reaction crystallization of struvite in a continuous DTM type crystallizer with a compressed air driven jet pump Experimental tests covering the production of struvite MgNH4PO4·6H2O from water solutions containing 1.0 mass % of phosphate(V) ions using magnesium and ammonium ions in stoichiometric proportions were carried out in a crystallizer of 1.2 dm3 working volume. The process temperature was 298 K. Struvite crystals of mean size Lm from ca. 14 to ca. 38 μm were produced depending on the process environments pH (9-11) and the mean residence time of suspension in a crystallizer, τ (900-3600 s). In such defined process conditions the linear growth rate of struvite crystals changed from 1.45·10-8 m/s (pH 9, τ 900 s) to 2.06·10-9 m/s (pH 11, τ 3600 s) while the nucleation rate from 5.1·107 to 3.2·109 1/(sm3). Crystal product of the most advantageous granular characteristics was produced at pH 9 and the mean residence time 3600 s. Within this product population the largest sizes reached above 200 μm while the number of crystals smaller than 3 mm was kept below 6%.

Struvite recovery from solution containing phosphate(V) and sulphate(VI) ions

Abstract The research results concerning the application of magnesium and ammonium ions for continuous removal of phosphate(V) ions from solution containing 1.0 or 0.20 mass% of PO43– and from 0.10 to 0.50 mass% of SO42– are presented. A continuous struvite MgNH4PO4 × 6H2O reaction crystallization process was carried out both under stoichiometric conditions and using 20% excess of magnesium ions. The research was conducted in a DT MSMPR type crystallizer with internal circulation of suspension driven by a propeller stirrer, in constant temperature 298 K. The pH varied from 9 to 11 and mean residence time of suspension in a crystallizer τ varied from 900 to 3600 s. It was concluded, that sulphate(VI) ions influenced product quality disadvantageously. Depending on process parameter combinations struvite crystals of mean size from ca. 18 to ca. 44 μm and of moderate homogeneity: CV 7–95% were produced. Presence of sulphate(VI) ions favored crystallization of struvite as prismatic crystals, but tubular forms were also identified. The best shaped struvite crystals were produced at relatively low concentration of sulphate(VI) ions, pH 9 and for mean residence time of suspension in a crystallizer elongated up to 3600 s.