Strength and structure of granules produced in continuous granulators
KeywordREF 2014; High shear granulator; Seeded granulation; Continuous granulator; Modulomix; Nica M6; Extrudomix
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AbstractThe effect of the operating conditions of three continuous high shear granulators on the internal structure and strength of granules has been investigated and the possibility of seeded granulation has been explored. In a recently concluded programme of research on the scale-up of a high shear granulator, Cyclomix (manufactured by Hosokawa Micron B.V., The Netherlands), a novel method of granulation called seeded granulation was introduced, where each granule contained, at its core, a large particle from the upper tail end of the feed particle size distribution. Seeded granulation is particularly useful for process control of continuous granulators as there is the potential to control granulation by the flow rate of the seed particles. Hence, the performance of three different types of continuous granulators in terms of granule strength and structure has been evaluated here; these are Extrudomix, Modulomix (manufactured by Hosokawa Micron, UK and The Netherlands, respectively) and the Nica M6 Turbine continuous granulator (manufactured by GEA, UK). Calcium carbonate (Durcal 65) powder was granulated using an aqueous solution of polyethylene glycol (PEG) as binder in the same ratio as used previously in our batch granulation, to allow comparison between the continuous and batch processes. The crushing strength was characterised by quasi-static side crushing between two platens using a mechanical testing machine. The internal structure and morphology were evaluated by scanning electron microscopy and the extent of seeding quantified. Granules produced in all the three continuous granulators were significantly weaker than those of the batch granulator tested previously. Among the continuous granulators only the Modulomix granulator produced some seeded granules. It is considered that longer residence time is necessary to produce seeded granules.
CitationRahmanian, N., Ghadiri, Mojtaba (2013) Strength and structure of granules produced in continuous granulators. Powder Technology, 233, 227-233.
Link to publisher’s versionhttp://dx.doi.org/10.1016/j.powtec.2012.09.008
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Characterisation of granule structure and strength made in a high shear granulatorRahmanian, Nejat; Ghadiri, M.; Jia, X.; Stepanek, F. (2009)Results of a study of the influence of impeller speed on the strength, structure and morphology of granules produced in a type of high shear mixer granulators are reported. Calcium carbonate particles (Durcal 65) have been granulated in a Cyclomix with a capacity of 5 L. An aqueous solution of polyethylene glycol was used as the binder. The granules produced have been dried and their structure visualized using X-ray micro-tomography equipment, Nanotom, with a resolution of less than 1 μm. It is shown that the operation of the granulator at high impeller tip speeds produces granules with a higher strength and lower porosity than those produced at medium and low impeller speeds. Two different granule micro-structures and morphologies are produced at high and low impeller speeds. Structure descriptors such as phase volume fraction (as representative of porosity), chord length distribution and auto-correlation function (as indices of homogeneity of structure) are used to quantify the internal structure of granules in 3D, which in turn affects the granule strength.
Effects of process parameters on granules properties produced in a high shear granulatorRahmanian, Nejat; Naji, A.; Ghadiri, M. (2011)Results of a study on the influence of process parameters such as impeller speed, granulation time and binder viscosity on granule strength and properties are reported. A high shear granulator (Cyclomix manufactured by Hosokawa Micron B.V., The Netherlands) has been used to produce granules. Calcium carbonate (Durcal) was used as feed powder and aqueous polyethylene glycol (PEG) as the binder. The dried granules have been analysed for their strength, density and size distribution. The results show that increasing the granulation time has a great affect on granules strength, until an optimum time has been reached. The underlying cause is an increase in granule density. Granules are consolidated more at higher impeller speeds. Moreover, the granule size distribution seems not to be affected significantly by an increase in impeller speed. Granules produced with high binder viscosity have a considerably lower strength, wide strength distribution due to poor dispersion of binder on the powder bed. Binder addition methods have showed no considerable effect on granule strength or on granule size distribution.
Influence of type of granulators on formation of seeded granulesKitching, V.R.; Rahmanian, Nejat; Jamaluddin, N.H.; Kelly, Adrian L.; CCIP grant (Collaboration, Capacity and IP Develop-ment) fund from the University of Bradford. (2020-08)It has been shown that seeded granules of calcium carbonate can be produced in commercial batch high shear granulators such as the Cyclomix high-shear impact mixer. Seeded granules are attractive to the pharmaceutical industry due to their high uniformity and good mechanical properties which can assist efficient tablet manufacture. In the current study, attempts to produce seeded granules of Durcal 65 and PEG 4000 binder using hot melt granulation are reported, in response to the recent shift towards continuous pharmaceutical manufacturing. Various screw configurations and rotation speeds were investigated in a series of experiments to determine the relationship between process conditions and granule properties. Particle size analysis, strength measurement and structural characterisation were used to quantify granule properties. It was found that using a series of kneading elements arranged at a 60° staggering angle located near to the feed section of the extruder screw generated strong, spherical granules. From structural characterisation approximately 5–15% of extruded granules were found to be seeded. Twin screw melt granulation is therefore considered to be a promising technique for continuous production of seeded granules, although a more detailed investigation is required to optimise yield and quality.