Application of CFD in vacuum dezincing process

Most lead bullion is refined by pyrometallurgical methods - this involves a serics of processes that remove the antimony (softening) silver (Parkes process), zinc (vacuum dezincing) and if need be, bismuth (Betterton-Kroll process). The first step, softening, removes the antimony, arsenic and tin by air oxidation in a furnace or by the Harris process. Next, in the Parkes process, zinc is added to the melt to remove the silver and gold. Insoluble zinc, silver and gold compounds are skimmed off from the melt surface. Excess zinc added during desilvering is removed from lead bullion using one of ghree methods: * Vacuum dezincing; * Chlorine dezincing; or * Harris dezincing. The present study concentrates on the Vacuum dezincing process for lead refining. The main aims of the research are to develop mathematical model(s), using Computational Fluid Dyanmics (CFD) a Surface Averaged Model (SAM), to predict the process behaviour under various operating conditions, thus providing detailed information of the process - insight into its reaction to changes of key operating parameters. Finally, the model will be used to optimise the process in terms of initial feed concentration, temperature, vacuum height cooling rate, etc.

Assessment of the origin and stability of Nifedipine polymorph IV by differential scanning calorimetry (DSC)

Purpose. To examine the thermal transition(s) between different polymorphic forms of Nifedipine and to define experimental conditions that lead to the generation of polymorph IV. Methods. Experiments were performed using a DSC 823e (Mettler Toledo). Nifedipine exists in four polymorphic forms, as well as an amorphous state. Examination of Nifedipine was conducted using the following method(s): cycle 1: 25ºC to 190ºC, 190ºC to 25ºC (formation of amorphous Nifedipine); cycle 2: 25ºC to X (60,70,80...150ºC), X to 25ºC; cycle 3: 25ºC to 190ºC and holding isothermally for 5 min between cycles (heating/cooling rate of 10ºC/min). Results. The amorphous state Nifedipine can sustain heating up to 90ºC without significant changes in its composition. Cycle 2 of amorphous material heated up to 90ºC shows only the glass transition at ~44ºC. In cycle 3 of the same material, a glass transition has been recorded at ~44ºC, followed by two exotherms (~100 and ~115ºC (crystallisation of polymorph III and II, respectively) and an endotherm (169ºC (melting of polymorphs I/II)). Samples that have been heated to temperatures between 100ºC and 120ºC in the second cycle showed a glass transition at ~44ºC and an additional exotherm at ~95ºC (crystallisation of polymorph III) on cooling a exotherm was observed at ~40ºC (crystallisation of polymorph IV). The same material showed no glass transition in cycle 3 but an endotherm at around 62ºC (melting of polymorph IV) an exotherm (~98ºC) and an endotherm (169ºC) melting of polymorph I/II. Heating the sample to a temperatures greater than 130ºC in cycle two results in a glass transition at ~44ºC, and two exotherms at ~102 and 125ºC (crystallisation of polymorphs III and I, respectively). Conclusions. DSC data suggests that polymorph IV can only be produced from amorphous or polymorph III samples. The presence of polymorph I or II drives the conversion of the less stable polymorphic form IV into the most stable form, I. Although form IV of Nifedipine can easily be created, following defined experimental conditions, it may only coexist with amorphous or polymorph III states. When polymorphs I and II are present in the sample polymorph IV cannot be etected.