An Investigation of Milk Powders Produced by a Laboratory-Scale Spray Dryer

ABSTRACT

A mini spray dryer has been used to investigate morphological changes that occur to milk particles during the spray drying process. We have found that the mini spray dryer is ideal for such investigations, because phenomena such as skin and vacuole formation in particles can be analyzed without the added complication of particle agglomeration, which only occurs in much larger spray dryers where particle number concentrations are higher. We have confirmed observations made by various researchers that the bulk density of spray-dried milk powder is greatly affected by the drying temperature, due to the strong influence of the latter on the porosity of the particles. In addition, we have attempted to explain observations made by various workers that fat accumulates preferentially at the surface of a particle during drying by postulating that fluid fat is transported towards the surface, via a network of cracks and pores, by the development of a vacuole overpressure which is also responsible for the inflation of the particle. Finally, we have shown that milk powders can be spray dried a second time, by reconstitution with water, with no change to the thermodynamic characteristics of the resultant powder. Thus, milk concentrates for spray drying research can be prepared from already-spray-dried milk powders rather than using the more arduous evaporation method to concentrate unprocessed milk.     

An Investigation and Quantitative Assessment of Particle Shape in Milk Powders from a Laboratory-Scale Spray Dryer

Seven samples of spray-dried milk were prepared using a miniature-scale Buchi Mini Spray Dryer B-290 (diameter 0.5 m, height 1.1 m). For each run, all inlet conditions were held constant except for feed type, inlet solids concentration, and inlet temperature. Skim milk at a solids concentration of 8.8% and whole milk at a solids concentration of 11% were dried at two inlet temperatures, 120 and 200°C. Lactose-free skim milk (8.8% solids concentration) and skim milk at a solids concentration of 41.2% were also dried at an inlet temperature of 200°C to assess the effects of milk feed type and inlet concentration, respectively. Equilibrium between the outlet product moisture content and the outlet gas conditions in the miniature spray dryer was not reached, unlike previous results for pilot-scale and larger dryers, so it appears that, in small (miniature-scale) dryers, the outlet moisture content is limited by kinetics and not by equilibrium. Calculated yields ranged from 10.4 to 82.7%, with whole milk giving significantly lower yields than skim milk, due to the sticky nature of fat found in whole milk. Lactose-free skim milk produced lower yields than skim milk dried at the same conditions, indicating that the lower glass-transition temperatures of the converted lactose sugars make these powders stickier. This sugar effect was not as large as that of the fat content. Comparisons between the SEM images, fractal dimensions, particle size distributions, and bulk densities showed that lower inlet temperatures produced particles of a more collapsed nature with a higher bulk density and lower fractal dimension than milk particles dried at higher temperatures. Also, feed solids concentration heavily influenced the shape of the particles, with high concentrations producing more spherical, less broken or shriveled particles with higher fractal dimensions, as the shell walls are thicker under these conditions. The fractal dimensions appeared to give generally consistent results for quantifying the average particle shapes.     

An Investigation and Quantitative Assessment of Particle Shape in Milk Powders from a Laboratory-Scale Spray Dryer

Seven samples of spray-dried milk were prepared using a miniature-scale Buchi Mini Spray Dryer B-290 (diameter 0.5 m, height 1.1 m). For each run, all inlet conditions were held constant except for feed type, inlet solids concentration, and inlet temperature. Skim milk at a solids concentration of 8.8% and whole milk at a solids concentration of 11% were dried at two inlet temperatures, 120 and 200°C. Lactose-free skim milk (8.8% solids concentration) and skim milk at a solids concentration of 41.2% were also dried at an inlet temperature of 200°C to assess the effects of milk feed type and inlet concentration, respectively. Equilibrium between the outlet product moisture content and the outlet gas conditions in the miniature spray dryer was not reached, unlike previous results for pilot-scale and larger dryers, so it appears that, in small (miniature-scale) dryers, the outlet moisture content is limited by kinetics and not by equilibrium. Calculated yields ranged from 10.4 to 82.7%, with whole milk giving significantly lower yields than skim milk, due to the sticky nature of fat found in whole milk. Lactose-free skim milk produced lower yields than skim milk dried at the same conditions, indicating that the lower glass-transition temperatures of the converted lactose sugars make these powders stickier. This sugar effect was not as large as that of the fat content. Comparisons between the SEM images, fractal dimensions, particle size distributions, and bulk densities showed that lower inlet temperatures produced particles of a more collapsed nature with a higher bulk density and lower fractal dimension than milk particles dried at higher temperatures. Also, feed solids concentration heavily influenced the shape of the particles, with high concentrations producing more spherical, less broken or shriveled particles with higher fractal dimensions, as the shell walls are thicker under these conditions. The fractal dimensions appeared to give generally consistent results for quantifying the average particle shapes.     

Characteristics of Milk Powders Produced by Spray Freeze Drying

Skim and whole milk powders were manufactured at lab scale by spray freeze drying (SFD), using liquid nitrogen as the cryogen. The polydispersity of droplet/particle sizes was limited using an encapsulator nozzle to atomize the feed. Particle morphology was examined using a scanning electron microscope. Samples were compared with equivalent spray-dried powders in tests of wettability and dissolution in water. The spray freeze-dried powders were found to be highly porous, with a uniform structure of pores throughout the entire particles. When tested in water, SFD skim milk powders wetted roughly three times as fast as industrially spray-dried agglomerated skim milk powders and were observed to dissolve rapidly by breaking down into smaller particles.     

Characteristics of Milk Powders Produced by Spray Freeze Drying

Skim and whole milk powders were manufactured at lab scale by spray freeze drying (SFD), using liquid nitrogen as the cryogen. The polydispersity of droplet/particle sizes was limited using an encapsulator nozzle to atomize the feed. Particle morphology was examined using a scanning electron microscope. Samples were compared with equivalent spray-dried powders in tests of wettability and dissolution in water. The spray freeze-dried powders were found to be highly porous, with a uniform structure of pores throughout the entire particles. When tested in water, SFD skim milk powders wetted roughly three times as fast as industrially spray-dried agglomerated skim milk powders and were observed to dissolve rapidly by breaking down into smaller particles.     

An Experimental Investigation of the Wall Deposition of Milk Powder in a Pilot-Scale Spray Dryer

A pilot-scale, co-current spray dryer has been used to investigate the effect of varying the swirl vane angle for the inlet air, inlet air temperature and liquid feed flowrate on the wall deposition flux of skim milk powder. The spray dryer was a cylinder-on-cone unit with a diameter of 0.8 m and a height of 2 m. It was fitted with adjustable swirl vanes surrounding a Delavan GA1 two-fluid atomizer. Swirl vane angles of 0, 25, and 30°, inlet air temperatures of 170, 200, and 230°C and feed flowrates of 1.4, 1.6 and 1.8 kg h^-1 were used. Inlet air swirl was found to significantly influence the wall deposition flux, with the highest swirl vane angle of 30° giving rise to the largest wall deposition flux. The difference between the particle and sticky-point temperatures of the skim milk powder was also found to be important in influencing the wall deposition flux. The wall deposition flux was the highest, at 16 g m^-2 h^-1, when the outlet particle temperature was furthest above the sticky-point temperature, and this occurred at the lowest value of the inlet air temperature (170°C) and highest product moisture content. No significant effect on the wall deposition flux was evident when using a nonstick food grade material (nylon), adhesive tape or stainless steel as the surface materials for the wall deposition tests. Therefore, it is likely that cohesion occurs at a similar rate to adhesion in the wall deposition of milk powder. Grounding the spray dryer also did not have a significant effect on the wall deposition flux. Relating the wall deposition flux to the sticky-point curve in this way suggests that the same trends (increased wall deposition fluxes above the sticky-point curve) may apply for other materials as well.     

Spray Drying of Skim Milk Mixed with Milk Permeate: Effect on Drying Behavior,Physicochemical Properties,and Storage Stability of Powder

The possibility of using milk permeate (MP) to lower the protein level of skim milk powder (SMP) in producing powders of 34% and lower protein is explored. Skim milk suspensions with various levels of MP were prepared by mixing SMP and MP powder (MPP) at the ratios of 1:0, 7:3, 3:7, and 0:1: from 34 to 5.3% protein. The suspensions were dried in a spray dryer with inlet and outlet temperatures of 180 and 80°C, respectively. Increasing permeate concentration in the mixture showed a greater tendency to stickiness manifested by lowered the cyclone recovery of the powder as more powder stuck on the wall of the dryer. Increasing permeate concentration in the resultant powder did not significantly affect the bulk density but led to a reduction in the particle size and also made the powder slight green and yellowish in color. It also found to lower the glass transition temperature (T_g ) of the skim milk powder (SMP) and induce crystallization of lactose at lower water activity (a_w  ≥ 0.328 for SMP:MPP of 3:7 and 0:1 compared to a_w  ≥ 0.0.432 for SMP:MPP of 1:0 and 3:7). Addition of MP in SMP lowered the T_g values of the resulting powders. The permeate fraction in spray-dried SMP/MPP mixtures found to lower the critical a_w and moisture content, suggesting the SMP mixed with MPP is more likely to become sticky than SMP alone (at 34% protein) when stored at a similar water activity and moisture content.     

Spray Drying of Skim Milk Mixed with Milk Permeate: Effect on Drying Behavior, Physicochemical Properties, and Storage Stability of Powder

The possibility of using milk permeate (MP) to lower the protein level of skim milk powder (SMP) in producing powders of 34% and lower protein is explored. Skim milk suspensions with various levels of MP were prepared by mixing SMP and MP powder (MPP) at the ratios of 1:0, 7:3, 3:7, and 0:1: from 34 to 5.3% protein. The suspensions were dried in a spray dryer with inlet and outlet temperatures of 180 and 80°C, respectively. Increasing permeate concentration in the mixture showed a greater tendency to stickiness manifested by lowered the cyclone recovery of the powder as more powder stuck on the wall of the dryer. Increasing permeate concentration in the resultant powder did not significantly affect the bulk density but led to a reduction in the particle size and also made the powder slight green and yellowish in color. It also found to lower the glass transition temperature (T_g) of the skim milk powder (SMP) and induce crystallization of lactose at lower water activity (a_w ≥ 0.328 for SMP:MPP of 3:7 and 0:1 compared to a_w ≥ 0.0.432 for SMP:MPP of 1:0 and 3:7). Addition of MP in SMP lowered the T_g values of the resulting powders. The permeate fraction in spray-dried SMP/MPP mixtures found to lower the critical a_w and moisture content, suggesting the SMP mixed with MPP is more likely to become sticky than SMP alone (at 34% protein) when stored at a similar water activity and moisture content.     

Effects of Process Variables on the Denaturation of Whey Proteins during Spray Drying

The effects of varying feed concentration (20–40% w/v) and outlet temperature (60 to 120°C) on whey protein denaturation (determined by DSC) and solubility (at pH 4.6) have been investigated in a pilot-scale co-current spray dryer. The study confirms that low outlet gas temperatures (60 and 80°C) produce the lowest amount of denaturation and solubility loss, with almost complete denaturation observed at 120°C along with a less dramatic reduction in solubility. Slightly more denaturation and loss of solubility was found with a 40% feed concentration. It is hypothesized that crust formation, resulting in high particle temperatures while still maintaining a wet core, is likely to lead to high levels of denaturation.     

Effects of Process Variables on the Denaturation of Whey Proteins during Spray Drying

The effects of varying feed concentration (20-40% w/v) and outlet temperature (60 to 120°C) on whey protein denaturation (determined by DSC) and solubility (at pH 4.6) have been investigated in a pilot-scale co-current spray dryer. The study confirms that low outlet gas temperatures (60 and 80°C) produce the lowest amount of denaturation and solubility loss, with almost complete denaturation observed at 120°C along with a less dramatic reduction in solubility. Slightly more denaturation and loss of solubility was found with a 40% feed concentration. It is hypothesized that crust formation, resulting in high particle temperatures while still maintaining a wet core, is likely to lead to high levels of denaturation.     

Physicochemical Characteristics of Date Powder Produced in a Pilot-Scale Spray Dryer

Date fruit is a good source of bioactive compounds and natural sugar. It has the potential to be utilized as a substitute for added sugar. Although several forms of dates—such as fresh dates, date paste, and date syrup—are available in the market and used for different applications, free-flow date powder would be highly beneficial in improving shelf-life, ease of handling, and blendability with various foods prepared domestically and in industry. The objective of this study was to produce date powder in a pilot-scale spray dryer and determine its physicochemical qualities. Date powder was produced at eight processing conditions (2 carrier agents (maltodextrin (MD) and gum arabic (GA) × 2 inlet air temperature (150°C and 170°C) × 2 feedstock flow rates (25 ml/min and 40 ml/min)). To the carrier agent was added at 0.4 kg per 1.0 kg of date fruits (dry weight basis), and the feedstock to the spray dryer was prepared at 20% concentration. Date powder was obtained in all eight treatments. Color (L*a*b* values), moisture content, bulk density, wettability, solubility index, hygroscopicity, microstructure analysis (using scanning electron microscope (SEM)), and total phenolic compounds were determined for the spray-dried date powder. The physicochemical characteristics of date powder varied significantly with respect to the processing conditions. Although physical properties of date powder were significantly affected by the carrier agent, there was no difference in total phenolic compounds between date powders produced with MD and GA. An SEM study revealed that date powder produced with MD had smooth, regular-shaped spherical particles but with severe agglomeration. Date powder with GA had relatively smaller particles of irregular sphere with dented surfaces.     

An Experimental Investigation of Lime Juice Drying in a Pilot Plant Spray Dryer

One of the major problems in spray drying of fruit juices such as lime juice is stickiness and thermoplasticity of their compositions. Lime juice consists of invert sugars and citric acid, which have low glass transition temperatures. Due to this characteristic, the particles stick on the dryer wall upon their collision with it. As a result, drying of these materials is very difficult. In order to solve this problem, various percent of silicon dioxide and maltodextrin (DE5), based on total soluble solid content of lime juice, have been used to reach a suitable drying condition. A cool chamber wall spray dryer was used in this investigation in order to decrease the probability of particles stickiness on the wall. Our investigation revealed that an addition of 10% silicon dioxide and 20% maltodextrin (DE5) to lime juice is the optimum amount for a complete and successful drying of lime juice. Sampling of particles from different longitudinal distances in the dryer tower is carried out to find the particle moisture contents as they fly downward in the dryer. The results show a very fast decrease in entrance moisture contents. Based on our experimental data, the variation of moisture contents are presented as a function of radial distance from central line and longitudinal distance from the entrance region.     

An Experimental Investigation of Lime Juice Drying in a Pilot Plant Spray Dryer

One of the major problems in spray drying of fruit juices such as lime juice is stickiness and thermoplasticity of their compositions. Lime juice consists of invert sugars and citric acid, which have low glass transition temperatures. Due to this characteristic, the particles stick on the dryer wall upon their collision with it. As a result, drying of these materials is very difficult. In order to solve this problem, various percent of silicon dioxide and maltodextrin (DE5), based on total soluble solid content of lime juice, have been used to reach a suitable drying condition. A cool chamber wall spray dryer was used in this investigation in order to decrease the probability of particles stickiness on the wall. Our investigation revealed that an addition of 10% silicon dioxide and 20% maltodextrin (DE5) to lime juice is the optimum amount for a complete and successful drying of lime juice. Sampling of particles from different longitudinal distances in the dryer tower is carried out to find the particle moisture contents as they fly downward in the dryer. The results show a very fast decrease in entrance moisture contents. Based on our experimental data, the variation of moisture contents are presented as a function of radial distance from central line and longitudinal distance from the entrance region.     

Characterization of polyanhydride microsphere degradation by DSC

Microspheres (2.91 μm diameter) were formed from poly(fumaric-co-sebacic anhydride) (P(FASA)) using a phase inversion microencapsulation technique. Blank microspheres, protein-loaded microspheres, and raw polymer were degraded in water for varying lengths of time to determine how degradation affects morphology and crystallinity. The rate of degradation was subsequently characterized using differential scanning calorimetry (DSC) and step-scan alternating DSC (SSADSC). As evident by the changing melting peak ratios during degradation, the protein-loaded microspheres were found to degrade at a more rapid rate than both the blank microspheres and the raw polymer, respectively. This was most likely because the release of protein from the microsphere surface led to an increased surface area available for degradation of this surface-eroding polymer.     

A Three-Dimensional Simulation of a Spray Dryer Fitted with a Rotary Atomizer

Spray dryers fitted with rotary atomizers are commonly used in diverse industries to produce engineered powders on a large scale. Scale-up of such units is still largely empirical and based on prior experience and know-how. In the present study, a three-dimensional spray dryer with rotary atomizer is investigated numerically with a commercial CFD code. Continuous-phase, i.e., air, conservation equations are formulated in the Eulerian model while the droplet or particle equations are set up in the Lagrangian model. Two-way coupling between the continuous and dispersed phases is taken into account in the governing equations. The stochastic approach is used to predict the particle trajectories. The RNG k - ε turbulence model was used. Typical results, viz. air velocity, temperature, humidity profiles, and particle trajectories are presented and discussed. Compared with the pressure nozzle spray dryer, more volume of drying chamber is used effectively by the rotating disc type spray dryer. It is found that evaporation and drying take place mainly in the region and in the vicinity of first contact between air and spray. A parametric study is presented and, where appropriate, comparison is made with experimental data obtained with the simulated spray dryer.     

A Three-Dimensional Simulation of a Spray Dryer Fitted with a Rotary Atomizer

Abstract

Spray dryers fitted with rotary atomizers are commonly used in diverse industries to produce engineered powders on a large scale. Scale-up of such units is still largely empirical and based on prior experience and know-how. In the present study, a three-dimensional spray dryer with rotary atomizer is investigated numerically with a commercial CFD code. Continuous-phase, i.e., air, conservation equations are formulated in the Eulerian model while the droplet or particle equations are set up in the Lagrangian model. Two-way coupling between the continuous and dispersed phases is taken into account in the governing equations. The stochastic approach is used to predict the particle trajectories. The RNG k ? ? turbulence model was used. Typical results, viz. air velocity, temperature, humidity profiles, and particle trajectories are presented and discussed. Compared with the pressure nozzle spray dryer, more volume of drying chamber is used effectively by the rotating disc type spray dryer. It is found that evaporation and drying take place mainly in the region and in the vicinity of first contact between air and spray. A parametric study is presented and, where appropriate, comparison is made with experimental data obtained with the simulated spray dryer.     

Preparation of Nickel Powders by Spray Pyrolysis of Nickel Formate

The preparation of nickel powders by the ultrasonic spray pyrolysis of Ni(HCOO)₂ was studied. Phase-pure nickel powder was obtained at as low as 350°C. HCOOH was a reducing source for nickel formation. Moreover, metallic nickel was obtained at a residence time as short as 0.1 s at 600°C. A broad range of particle morphologies, which included agglomerated nanoparticles, nonagglomerated submicrometer particles, hollow particles, and spherical dense particles, were obtained from Ni(HCOO)₂ pyrolysis and were shown to depend on the precursor solution and the operating condition.     

Superheating of the melting kinetics in polymer crystals: a possible nucleation mechanism

Melting kinetics of polymer crystals has been examined experimentally by calorimetric methods utilizing the combination of a conventional differential scanning calorimetry of heat flux type (CDSC-HF) and a temperature-modulated DSC (TMDSC). The superheating effect in the kinetics has been discussed based on a modeling of the melting kinetics. For low-density polyethylene and linear polyethylene, the melting rate showed nearly linear dependence on the degree of superheating, which indicates the kinetics controlled by heat diffusion or by surface kinetics on rough interface. For isotactic polypropylene, poly(ethylene terephthalate) and poly(?-caprolactone), the dependence is non-linear and close to the limiting case of exponential dependence, which indicates nucleation-controlled kinetics of melting. A possible mechanism of the activation process in the melting kinetics has been discussed in consideration of the specific feature of polymer crystals far from its most stable state. The consistency of the results of CDSC-HF and TMDSC has been confirmed by this analysis with a calibration of peak temperature for the instrumental thermal delay in CDSC-HF.     

Experimental Study and CFD Modeling of Wall Deposition in a Spray Dryer

The wall deposition phenomenon in a pilot-scale spray dryer was investigated based on mathematical modeling and experimental trials. For this purpose, the governing equations were obtained and solved numerically by applying a mathematical modeling technique and an open-source computational fluid dynamics (CFD) software. The wall deposition, velocity distribution of the existing phases, and droplet trajectory in the drying chamber were determined. The effect of the operating parameters including the feed flow rate, inlet concentration of dissolved solid, and initial droplet diameter on the air flow pattern, droplet trajectory, and wall deposition was investigated. Through the experiments, the wall deposition of powder product in different positions of the drying chamber was measured. In modeling part of this study, we attempted to determine the effect of particle diameter on the percentage of wall deposition and the position where it occurred.

The model results obtained for wall deposition were compared with collected experimental data and good agreement was observed.     

Effects of MgH2/Mg(BH4)2 Powders on the Thermal Decomposition Behaviors of 2,4,6‐Trinitrotoluene (TNT)

The thermal properties of 2,4,6‐trinitrotoluene (TNT), TNT/MgH₂, and TNT/Mg(BH₄)₂ were investigated by differential scanning calorimetry (DSC) and accelerating rate calorimetry (ARC). The results show that addition of MgH₂ or Mg(BH₄)₂ to TNT has a great effect on the DSC decomposition process. The exothermic decomposition peak of TNT disappeared and was replaced by a slow exothermic trend in the curves of both TNT/MgH₂ and TNT/Mg(BH₄)₂. The kinetic triplet of TNT formulations were calculated by ARC data. The results show that TNT/MgH₂ and TNT/Mg(BH₄)₂ have lower onset temperatures, apparent activation energies (E) and frequency factors (A) than neat TNT. A change of the TNT decomposition mechanism is also discussed.