Effect of operating conditions and physico–chemical properties on the wet granulation kinetics in high shear mixer

The wet granulation process is sensitive to changes in product properties and process variables. The optimal process and formulation are based on the knowledge of the granule growth mechanisms and of the effects of product properties and process variables. This paper presents the study of wet granulation of microcrystalline cellulose powder, MCC (Avicel PH101) using high-shear mixer granulator. It aims at understanding the effect of operating parameters (impeller rotational speed, liquid binder flow ate) and of physicochemical properties (viscosity, wettability) of a binder solution on solid particles surfaces, on the agglomeration kinetics. The experiments are carried out with water, aqueous solutions of sodium carboxymethylcellulose, polyvinylpyrrolidone, hydroxypropylméthylcellulose or a non ionic surfactant oxo-C10C6 at a critical micellar concentration. Concerning the process variables the experimental results show that an optimal interval of impeller speed operation exists ranging from 150 to 200 rpm for granule growth. Below, an uncontrollable agglomerate size and localised over-wetting occur, and above granule breakage occurs. Increasing the liquid binder flow rate reduces the extension of the non growth regime, but does not affect the granule mean size. The effect of the physicochemical properties is evaluated using a modified capillary viscous number, Ca′, that we define as the ratio between the viscous forces (μLU) and the work of adhesion Wa=γL(1+cosθ). For Ca′b1, the viscosity of the solution does not significantly affect the granulation process. The dominant forces in the granulation process are the interfacial forces since increasing the work of adhesion enhances the growth kinetics. For Ca′N1.6, the viscous forces predominate and control the granule growth

Biomass steam gasification in fluidized bed of inert or catalytic particles: Comparison between experimental results and thermodynamic equilibrium predictions

In order to improve the understanding of biomass gasification in a bed fluidized by steam, the thermochemical equilibrium of the reactive system was studied. The equilibrium results were compared to LGC experimental results, obtained by the gasification of oak and fir in a laboratory-scale fluidized bed of different catalysts: sand, alumina, and alumina impregnated with nickel. The research was completed by a study of the influence on the equilibrium of additional parameters such as the quantity of steam, the pressure or the kind of biomass. Those results of simulation may be used for evaluating the limits of actual reactors.The following conclusion may be drawn from all the results: The thermodynamic equilibrium state calculated is far away from the experimental results obtained on sand particles. The steam to biomass ratio, between 0.4 and 1 kgsteam/kgdry biomass, has a strong influence on the gas mixture composition. The temperature increase and the use of catalyst allow producing a gas mixture with a high content of hydrogen and carbon monoxide. The H2:CO ratio may reach values greater than 3. The use of catalyst allows the system to get closer from the equilibrium, especially for the nickel based catalyst

Wet granulation in laboratory-scale high shear mixers: Effect of chopper presence, design and impeller speed

The effect of the main means of agitation in a high shear mixer has been investigated in this study. Granulation runs have been performed on a fine cohesive microcrystalline cellulose powder (Avicel 105, d50 = 20 μm) often used as a pharmaceutical excipient in tablet formulations in two bowls of a Mi-Pro® laboratory high shearmixer with a capacity of 0.9 and 1.9 L, respectively. Torque curves recorded during granulation are found to allow good control of the process while increasing impeller speed is found to generally reduce granule size and the onset of breakage seems to occur for similar values of impeller tip speed. As a general rule, the chopper allows for better binder distribution in the Mi-Pro® and is found to be necessary for successful granulation at low to moderate impeller speeds. For high impeller speeds in excess of 4.4 m/s with or without a chopper, similar granule sizes and growth mechanisms are observed. Granule roundness was found to increase with impeller speed up to a certain speed after which granule roundness has been found to decrease with increasing impeller speed most probably because of increased breakage of the granules. Dry granule strength has been found to increase with increasing impeller speed, presenting only a slight decrease at the highest impeller speed studied

Rheology, granule growth and granule strength: Application to the wet granulation of lactose–MCC mixtures

This study aims at better understanding the wet granulation process of a binary mixture composed of microcrystalline cellulose (water insoluble) and lactose (water soluble). It investigates the effect of formulation (proportion of the different components in the mixture) on the granule growth kinetics, the evolution of granule morphology during granulation, the wet mass consistency and dry granule trength of the end product. Additionally the influence of mixer design has been studied by up scaling the process from the 1.9 L Mi-pro high shear mixer used as the reference scale to a 6 L Diosna P1-6 high shear mixer. The scale-up rules investigated were constant impeller tip speed and constant Froude number. Our results allowed us to draw the following conclusions: – The increase in MCC content is found to increase the optimum binder requirement for granulation, wet mass consistency and dry granule strength. – Granule growth takes place in three distinct stages: wetting, nucleation and growth. These stages can be identified with the help of the recorded torque values during the granulation process or by the evolution of granule size and granule morphology. – The characterization of the starting materials by moisture sorption isotherms brings more insight to the role of each component during the granulation process. – The increase of the granulation scale has little influence on the observed growth mechanism. However bi-modality of the granule size distribution is increased, wet mass consistency and dry granule strength are decreased with increasing scale of operation

Hydrodynamic and solid residence time distribution in a circulating fluidized bed: experimental and 3D computational study

Vertical profiles of local pressure, horizontal profiles of net vertical solid mass flux, and residence time distributions (RTD) of the solid phase are experimentally assessed in the riser of a small scale cold Circulating Fluidized Bed of 9 m high having a square cross section of 1111 cm. Air (density 1.2 kg/m3, dynamic viscosity 1.8×10-5 Pa.s) and typical FCC particles (density 1400 kg/m3, mean diameter 70 mm) are used. The superficial gas velocity is kept constant at 7 m/s while the solid mass flux ranges from 46 to 133 kg/m2/s. The axial dispersion of the solid phase is found to decrease when increasing the solid mass flux. Simultaneously, 3D transient CFD simulations are performed to conclude on the usability of the eulerian-eulerian approach for the prediction of the solid phase mixing in the riser. The numerical investigation of the solid mixing is deferred until later since the near-wall region where the solid phase downflow and mixing are predominant is not well predicted in spite of well-predicted vertical profiles of pressure

Wet granulation in laboratory scale high shear mixers: Effect of binder properties

The effect of binder properties on torque curves, granule growth kinetics, wet mass consistency and dry granule strength has been investigated in this study. Granulation runs have been performed on a fine cohesive microcrystalline cellulose powder (Avicel 105, d50 = 20 μm) in two types of laboratory high shear mixers: a Mi-Pro high shear mixer using a 1.9 L bowl and a 6 L Diosna high shear mixer. Binders used included ultra-pure water and solutions of varying concentrations of PVP and HPMC allowing us to cover different values for parameters like viscosity and work of adhesion. Torque curves recorded during granulation are found to allow good control of the process. Optimum liquid requirement for granulation has been found to vary with binder type and decrease with increasing viscosity while granule growth kinetics has been found to be to be related to the work of adhesion for low viscosity binders. Granule strength has been evaluated for wet granules by the means of wet mass consistency measurements on a mixer torque rheometer and for dried granules by means of uniaxial compression tests on a Texture Analyser mechanical testing machine. For low viscosity binders both wet mass consistency and dry granule strength have been found to depend on the work of adhesion. For high viscosity bindershigherwet mass consistencies but lower dry granule strengths have been observed. Granulating on the larger 6 L scale has shown that constant impeller tip speed offers good agreement in terms of mean granule size however granule size distribution seems to be scale dependan

Effect of the plasticizer on permeability, mechanical resistance and thermal behaviour of composite coating films

Thin layer deposit of a composite material on solid particle surfaces used in the food industry aims to ensure the protection of food powder against aggressive environments such as amoist atmosphere. The layer, having a thickness of a few fractions of millimetre, must have certain physico-chemical properties: it must be compatible with the product, itmust be impermeable to water and oxygen, itmust have goodmechanical strength and good adhesion to the surface of the coated powder. Furthermore the layer must fulfil the regulatory requirements for food ingredients. Film properties like continuity, permeability, and mechanical resistance depend on the choice of the excipients included in the formulation and the operating conditions which can modify the constraints generated at the interface film-powder. As a consequence, the scientific issue consists of combining the local phenomena happening at amicroscopic level on the surface of the particle with the processing technology and the process parameters. In a first step, the attention is focussed on the film and its formulation. For this step, films are prepared separately and they are dried under very smooth conditions. Test samples are taken from the formed composite films and contain hydroxypropyl methylcellulose asmatrix (67% of driedmaterial),micronised stearic acid as hydrophobic filler (20% of driedmaterial) and a plasticizer (13% of driedmaterial). The filmformation procedure and the testmethod are described in detail. The effect of the type of plasticizer (different grades of PEG) onmechanical, thermal and permeability properties of the coating film is studied. The results show that PEG with higher molecular rate provides a better plasticizing effect for the film but increases the water vapour permeability of the film

Metallic salt deposition on porous particles by dry impregnation in fluidized bed: Effect of drying conditions on metallic nanoparticles distribution

In this paper, the fluidized bed dry impregnation of coarse alumina porous particles by a metallic salt, manganese nitrate, is investigated. In this technique the penetration of each drop of metallic solution in the porous solid particle and solvent evaporation takes place at the same time, then liquid diffusion phenomenon is negligible. So, the metal loading is directly related to the operating time and liquid flow rate and concentration. It is found that the competition between two phenomena, drying and capillary flow, controls the deposit location. In order to determine the importance of the solvent evaporation process compared to the solution penetration by capillarity, an impregnation module, IM, was defined as the ratio between the drying characteristic time and a capillary penetration time. The adequate choice of the operating conditions (bed temperature, liquid and fluidization gas flow rate) allows a uniform deposition of the metallic precursor inside the porous matrix or on the support surface. The impregnation under slow drying conditions (IM ≥ 10 and solvent content in the bed atmosphere τs ≥ 0.2) leads to a homogeneous deposition inside the pores. Under fast drying conditions (IM < 5 and τs < 0.2), the deposit is located at the particle external surface.In the case of slow drying, the impregnation kinetics can be represented by a “shrinking core” model. The critical impregnation rate is controlled by the competition between dissolution and recrystallization at the elementary grain scale. The size of the metal crystallites depends on the pore mean size and size distribution and on the drying rate

3D numerical simulation of Circulating Fluidized Bed: comparison between theoretical results and experimental measurements of hydrodynamic

This work was realized in the frame of the European GAYA project supported by ADEME. This paper presents a description of the hydrodynamic into a CFB according to experimental measurements of gas pressure and solid mass flux. These experimental data are compared to three dimensional numerical simulation with an Eulerian approach. The obtained numerical results show that the applied mathematical models are able to predict the complex gas-solid behavior in the CFB and highlight the large influence of the particle wall boundary condition. Indeed, it is shown that free slip wall boundary condition gives a good prediction a solid mass flux profile in comparison with experimental measurements nevertheless a convex shape. Moreover, the numerical solid hold-up is underestimated compared to the experimental data. On the contrary, a no-slip boundary condition improves the profile shape of solid mass flux but highly overestimates its intensity and the solid hold-up. A compromise appears to be a friction particle-wall boundary condition such as Johnson and Jackson (1) but the model parameters have to be chosen very carefully especially the restitution coefficient

Close-packing transitions in clusters of Lennard-Jones spheres

The structures of clusters of spherical and homogeneous particles are investigated using a combination of global optimization methods. The pairwise potential between particles is integrated exactly from elementary Lennard-Jones interactions, and the use of reduced units allows us to get insight into the effects of the particle diameter. As the diameter increases, the potential becomes very sharp, and the cluster structure generally changes from icosahedral (small radius) to close-packed cubic (large radius), possibly through intermediate decahedral shapes. The results are interpreted in terms of the effective range of the potential