Homogeneity of powder blends is an important metric for industrial applications in fortified dairy foods including commercial pediatric nutrition products. Product development practices evaluating physical properties and nutrient stability performance are reliant on blending parameters that deliver a uniform powder at both the pilot and commercial scale. Quantities of individual micronutrients in finished products are particularly critical for formulated infant foods. The two preliminary phases of this study focused on developing a simple, efficient method, specifically for a pilot scale ribbon blender, in which maximum homogeneity in fortified dairy-based powder blends could be reached. In phase one, a red iron oxide pigment powder was mixed throughout a white dairy powder and color homogeneity was measured by comparing L*a*b* color values from powder samples extracted from different areas of the ribbon blender. For phase two, sixteen similar fortified dairy blends were produced with varying ribbon blade shaft rpm, fill level, and blending durations according to a response surface method (RSM). The level of homogeneity of ferrous sulfate in the dairy blend was measured in these fortified mixtures to determine optimal blender parameters. After operating parameters were determined for uniform blending, phase three was enacted using these parameters. A comparison study of nutrient stability in fortified model non-agglomerated powder infant formula (PIF) and agglomerated whey protein concentrate (WPC) powder blends was executed to evaluate the degradative effect of microencapsulated ferrous sulfate (MFS) vs. unencapsulated ferrous sulfate (UFS) in these fortified dairy blends. The nutrient degradation rates of vitamins A, E and C in both PIF and WPC base powder, fortified with either MFS or UFS, were determined and compared during an accelerated eight-week stability study. Using p = 0.05, no statistically significant differences in vitamin degradation rates were observed when comparing independent spray-dried dairy-based blends containing unencapsulated or microencapsulated ferrous sulfate (using an encapsulating composition of 60% stearic acid) during eight weeks of accelerated shelf-life storage conditions (37 °C with a 75% relative humidity, RH). Of note, the degradation rates of vitamins A and E in blends containing PIF and UFS were more rapid than the control and suggestively significantly different (p = 0.07).

Air-suspension particle coating is a process by which thin coatings are applied to powder particles. The coatings can be formulated to act as permeable barriers to increase powder shelf-life or to impart controlled release character. The ultimate objective of a coating operation is to produce individual particles, each with a well-controlled, even coating. This project was focused on the air-suspension coating of fine powders of ~100 µm in diameter for the dairy industry. Despite the widespread use of the technology in the pharmaceutical industry, its use in the food industry has been limited. Little is known about the fundamental mechanisms, and so published work to date is product and equipment specific and is statistical in the way the experimental design and analysis has been approached. This 'black box' approach is time consuming and costly. Better methods based on an understanding of the physical and chemical mechanisms are needed to deal with the numerous products and constantly changing formulations typical of the dairy industry. This thesis proposes a new approach to air-suspension particle coating research. The basis of this 'micro-level process approach', is to deconvolute the complex coating process into smaller manageable parts based on classical physical phenomena for which descriptions already exist. The thesis identifies and develops an understanding of the key micro-level processes controlling coated product quality and process performance. Four were selected for further study: drying, droplet impact and spreading, and stickiness which encompasses the two key micro-level processes of droplet impact and adherence and inter-particle agglomeration. They were studied separately to deconvolute the variable effects and interactions. Kinetic data were collected for the drying droplets containing maltodextrins, whey protein isolate and gum arabic. A mathematical model, based on 'ideal shrinkage' was developed to predict the drying kinetics of single droplets with particular interest in the development of the surface glass transition temperature. The model accurately predicted the kinetics until significant morphological changes occurred in the droplet. To better predict the kinetics late in the drying process, the droplet radius was set to be constant at a time based on the surface proximity to the surface glass transition temperature (critical X concept). This was done to arrest droplet shrinkage in line with experimental observations and to more accurately depict the drying of high molecular weight, amorphous glass forming polymers. After this point, a new flexible calculation scheme was used to better predict the variation in internal droplet structure as either a dense, 'collapsed shell' structure or a 'dense skin-porous crumb' structure. Further study should focus on the surface and internal droplet structure (porosity and mechanical integrity) development during drying, particularly the conditions leading to the arresting of the droplet radius and the subsequent rate of skin thickness progression. The critical X concept was used to make industrial-scale predictions of the optimum drying conditions that ensure maximum droplet impact and adherence efficiency and minimum inter-particle agglomeration in a Würster-style coating operation. This enabled the prediction of two key design parameters, the nozzle distance from the powder impact point and the Würster insert height. The span in design parameters showed that there is significant opportunity for design optimisation based on the critical X concept. A probe tack test was used to map the level of stickiness of droplets of different coating materials as they dried. As skin formation progressed, the stickiness passed through a maximum, in most cases to arrive at a point at which the droplet was no longer sticky at all (non-adhesive state). The maximum point of stickiness represents the ideal state to ensure successful droplet-substrate impact and adherence. The minimum point of stickiness represents the ideal state to prevent unwanted inter-particle agglomeration. The time interval between the onset of stickiness and the non-adhesive state was particularly dependent on the addition of plasticisers, but also on the formulation and the drying air conditions. Future work should look to establish a possible relationship between the surface glass transition temperature and the probe tack test stickiness measurements. The impact and spreading of droplets containing maltodextrin DE5 on to solid anhydrous milkfat was studied using a high speed video camera. It was found that the final spread diameter was able to be fixed close to the maximum spread diameter by using surfactants, thus avoiding significant recoil. Because existing literature focuses on predicting the maximum spread diameter, this work defines a need for adequate prediction methods for the final spread diameter, as this is the significant parameter in coating applications. Formulation and operating guidelines were established to independently optimise each micro-level process. These were used in a series of population based coating experiments in a pilot-scale Würster coater. This study highlighted the limited flexibility of the standard 'off-the-shelf' Würster coating apparatus for the coating of fine sized dairy powders. Because of this, the validation of the guidelines were inconclusive and optimisation could not be carried out. Further validation work is required on a custom-built apparatus for dairy powders. This work has advanced the fundamental knowledge of the coating process and is independent of material, equipment and scale. This knowledge, based on physical and chemical mechanisms, can be used to develop coating formulations and identify optimum process conditions for successful coating in less time and at less expense than is current practice. The next step is to put the guidelines into practice and craft the engineering of a continuous coating apparatus for dairy powder applications.

L'agglomération humide est une étape cruciale dans la technologie de mise en forme des poudres de par son fort impact sur la qualité finale des produits élaborés. Malgré son intérêt lors de l'élaboration de nombreux produits (aliment, pharmaceutique, génie civil,…), ainsi que les différents modes technologiques (malaxeurs horizontaux, verticaux, à faible ou fort de taux de cisaillement, lit fluidisé, …), elle reste insuffisamment maîtrisée de par la difficulté à proposer des diagrammes de fonctionnement opérationnels qui couplent les contributions croisées des procédés et des produits. Ce travail de thèse s'inscrit dans cette problématique et porte sur l'étude des mécanismes d'agglomération en lien avec les caractéristiques de la formulation et les paramètres opératoires. L'identification et la représentation du mode d'assemblage des particules au cours de l'opération de mouillage/malaxage est l'un des enjeux central de ce travail. A partir d'expériences menées avec deux types de poudres alimentaires (semoule de blé dur et poudre de lait), l'agglomération est induite soit par contacts humides en malaxeur à faible taux de cisaillement soit par des collisions entre les particules collantes en lit fluidisé. Les mécanismes d'agglomération humide de la semoule de blé dur développés dans un malaxeur à faible cisaillement sont décrits selon un processus de morphogénèse qui corrèle la taille des agglomérats à leur texture via une dimension fractale. L'influence des propriétés physicochimiques des liants liquides sur les mécanismes d'agglomération est étudiée au regard des paramètres du modèle fractal. L'étude fine des distributions des propriétés hydrotexturales et dimensionnelles des structures agglomérées a permis d'identifier leur « règle » d'agencement : association par même classe hydro-texturale et dimensionnelle. Les régimes d'agglomération en fonction du mode d'apport d'eau (débit faible, débit fort) sont étudiés en se basant sur la notion de flux d'atomisation adimensionné. En ce qui concerne l'agglomération de la poudre de lait en lit fluidisé, les mécanismes d'agglomération sont étudiés en suivant l'évolution des tailles et des teneurs en eau des échantillons prélevés durant l'opération de mouillage/séchage et par la suite l'étude de l'impact de certaines conditions opératoires et de formulation sur les propriétés des agglomérats finaux et les régimes d'agglomération. Un lien entre les procédés est discuté et ouvre sur une requalification des régimes d'écoulement granulaire ainsi que de la réactivité de surface des particules. / Wet agglomeration is a crucial step in the shaping technology of powders because of its strong impact on the final quality of the elaborated products. Despite its interest in the elaboration of many products (food, pharmaceutical, engineering,...) as well as different technological process (horizontal mixers, vertical, low or high shear rate, fluidized bed, ...), it remains insufficiently mastered due to the difficulty in establishing operating diagrams taking into account, in the same time, products and process contributions. This thesis focuses on the study of the agglomeration mechanisms related to the characteristics of the formulation and process parameters. The identification and representation of the way particles come together during the wetting / mixing operation is one of the central challenges of this work. From experiments with two different food powders (durum wheat semolina and milk powder), agglomeration is induced either by wet contacts in mixer at low shear rate or by collisions between sticky particles in a fluidized bed. Mechanisms of semolina wet agglomeration developed in a low shear mixer are described as a process of morphogenesis that correlates the agglomerates size to their texture via a fractal dimension. The influence of the liquid binder physicochemical properties on the agglomeration mechanisms is studied according to the values taken by the fractal parameters of the model. The detailed study of the distribution of size and textural properties of agglomerated structures make it possible to identify the rule that lead to their layout: the association is mainly possible between structures belonging to the same class concerning their hydro-textural and dimensional characteristics. Agglomeration regimes depending on the mode of water supply (low flow, high flow) are studied based on the notion of dimensionless spray flux. Concerning milk powder agglomeration in a fluidized bed, agglomeration mechanisms are studied by following the evolution of the size and water content of the samples taken during the operation of wetting / drying and thereafter studying the impact of some operational conditions and formulation on the properties of the final agglomerates and agglomeration regimes. A link between the processes (low shear mixer and fluidized bed) is discussed and opens onto a redefinition of granular flow regimes and the surface reactivity of particles.