Spray Drying Tower Experiments

The article presents a full set of spray drying experiments for selected products performed in a co-current spray drying tower developed at Lodz Technical University. The experiments enabled identification of process and atomization parameters (feed properties, feed rate and feed temperature, drying agent temperature, air flow rate, atomization ratio, etc.) on drying and degradation kinetics, spray structure, particle residence time, and final product properties. Drying agent temperature measurements showed, in all cases, the initial increase of gas temperature in the spray envelope caused by the spray expansion and then a decrease induced by liquid evaporation and heat losses to the environment. PDA analysis confirmed that the initial velocity of particles was a function of a diameter and also the function of the distance from the axis. Practically an identical particle size distribution was observed in each cross-sectional area of the dryer. Negative values of particle velocity in the vicinity of the axis and at the edge of the spray envelope were found which proved that recirculation of particles appeared in the column. Analysis of final product properties showed that for agglomerate-like materials a decrease of bulk density with an increase of air temperature was related to morphological changes that occurred during drying and affected the shape of particles, surface structure, etc. The experiments proved that air/liquid ratio for two-fluid atomization and gas temperature were the most decisive factors controlling drying and degradation process rate and final product properties.     

Optimization of Process Parameters for Spray Drying of Fermented Soy Milk

Generally used as an inexpensive source of high-quality protein with many other health-promoting properties, soy milk offers an interesting alternative when fermented. Fermentation with lactic acid bacteria brings about the value addition to soy milk, making a nutritious probiotic food product. Dehydration helps to achieve longer shelf life and easier transportation and storage, enabling wider distribution of the product. The present work pertains to optimization of process parameters for spray drying of fermented soy milk using response surface methodology (RSM). The process parameters studied include inlet air temperature, aspirator speed (air flow rate), feed flow rate, and atomization pressure. The experiments were designed using the central composite design tool. Residual moisture content was found to be low at higher inlet air temperature, lower feed flow rate, higher atomization pressure, and higher air flow rate. Porosity reduced with increased atomization pressure. Higher product yield was obtained at high air flow rate and low feed flow rate. The increase in the atomization pressure increases the cohesiveness between particles, resulting in reduced flowability. An increase in the inlet air temperature greatly reduces the viability and the isoflavone aglycone content in the product. Protein denaturation during the process was found to reduce the product solubility.     

Drying of Inorganic Particulate Compounds

Inorganic particulates are usually dried in a fixed bed, fluidized bed, or spray dryers. These compounds are easy to dry, once their physical structure, with high porosity, allows moisture content removal with low resistances. For fluidized bed of alumina particle evaluations, a laboratory-scale drying unit was built. The drying experiments were carried out with alumina particles with different diameters to evaluate temperature and air flow rate effects on drying kinetics and bed height. In another case, the dehydration of a mixture of rare-earth chlorides in a fluidized bed was studied, aiming at the production of anhydrous rare-earth chlorides, used to obtain mischmetal by electrolytic and metallothermic processes. The spray drying experiments were carried out in a pilot plant. Spray drying is a technique largely applied in industrial processes to dry solutions or suspensions, converting their solid parts into a dried powder. A set of rare-earth drying experiments was carried out, aiming at the development of techniques to obtain a powder that could satisfy international morphological requirements. The results allowed evaluating the effects of air flow rate, feed concentration, atomizer model, rotation velocity, and atomization pressure on powder density and particle size distribution.     

Drying of Inorganic Particulate Compounds

ABSTRACT

Inorganic particulates are usually dried in a fixed bed, fluidized bed, or spray dryers. These compounds are easy to dry, once their physical structure, with high porosity, allows moisture content removal with low resistances. For fluidized bed of alumina particle evaluations, a laboratory-scale drying unit was built. The drying experiments were carried out with alumina particles with different diameters to evaluate temperature and air flow rate effects on drying kinetics and bed height. In another case, the dehydration of a mixture of rare-earth chlorides in a fluidized bed was studied, aiming at the production of anhydrous rare-earth chlorides, used to obtain mischmetal by electrolytic and metallothermic processes. The spray drying experiments were carried out in a pilot plant. Spray drying is a technique largely applied in industrial processes to dry solutions or suspensions, converting their solid parts into a dried powder. A set of rare-earth drying experiments was carried out, aiming at the development of techniques to obtain a powder that could satisfy international morphological requirements. The results allowed evaluating the effects of air flow rate, feed concentration, atomizer model, rotation velocity, and atomization pressure on powder density and particle size distribution.     

Experimental Study of Spray Drying and Atomization with a Two-Fluid Nozzle to Produce Inhalable Particles

A series of 50 experiments was performed to investigate particle size and yield from three laboratory spray dryers with two-fluid nozzles, using an aqueous solution of egg albumin as the feed. First principles theory suggests that the main parameters affecting final particle size should be atomization gas flowrate and velocity, feed solution flowrate, solution concentration, and inlet and outlet gas temperature. The experiments demonstrated that atomization gas velocity at the nozzle correlated better than volumetric gas flowrate to the final particle size obtained. Increasing atomization gas flow gave a decrease in particle size, levelling off at high nozzle gas velocities approaching sonic values. Liquid flowrate had little effect, and hybrid ratios such as the ALM (atomization gas to liquid flow ratio) did not correlate well to measured final particle size for this system. This seems likely to apply to aqueous systems with temperature limitations, where liquid flowrates will be relatively low compared to gas flowrates (both atomization and main gas flow). Particle size generally increased with solution concentration, and in some cases scaled exactly, assuming a constant initial droplet size and final particle density. All experiments were performed below the boiling point and therefore temperature had little effect. Particles of 2–3 microns were obtained at high atomization gas flows, indicating initial droplet sizes of 4–7 microns at most, while lower flowrates gave substantially larger particles and a wider size distribution.     

Combined Crystallization and Drying in a Pilot-Scale Spray Dryer

Combined crystallization and drying of lactose solutions was performed in a pilot-scale spray dryer over a wide range of operating conditions. The effect of different parameters, including temperature, moisture content, atomizing air flow rate, liquid feed rate, main drying air flow rate, and particle size, on the degree of crystallinity of the spray-dried powders was analyzed. Water-induced crystallization (WIC) and modulated differential scanning calorimetry (MDSC) were used to assess the effect of these parameters on the degree of crystallinity of the spray-dried powders. The particles were characterized in terms of the final moisture content using WIC and distinctive differences in the peak heights, which are indicative of the particle crystallinity, were found for spray-dried particles using different drying conditions, supporting the results from MDSC. MDSC showed that decreasing the inlet air temperature by 40°C increased the degree of crystallinity in the particles threefold from 22 to 72%. A decrease in the inlet air temperature may decrease the particle temperature, resulting in wetter particles, and a lower temperature meant a longer particle drying time and allowed the particles to rearrange themselves into a more crystalline form. Up to 72% crystallinity is achievable in a pilot-scale spray dryer by suitable adjustment of the operating conditions. The results suggest differences in the rate of crystallization and particle size between small and pilot-scale spray dryers.     

DRYING KINETICS AND PARTICLE RESIDENCE TIME IN SPRAY DRYING

A unique experimental equipment for extensive trials on the spray drying kinetics and particles residence time involving “in situ” analysis of the properties of continuous and dispersed phases was designed, built, and tested. Advanced experimental techniques (including laser techniques) to determine current parameters of spray drying process (temperature, humidity, moisture content) and current structure of spray (particle size distribution, particle velocities, etc.) were employed. Full scale spray drying tests of baker's yeast and maltodextrin enabled identification of the effect of process parameters on drying kinetics and spray residence time in the tower. Quantitative relationship describing spray drying kinetics as a function of atomization ratio and drying agent temperature were determined. The experimental results proved that spray residence time was controlled by atomization ratio and airflow rate. Drying kinetics in spray drying process is presented for the first time in the literature.     

DRYING KINETICS AND PARTICLE RESIDENCE TIME IN SPRAY DRYING

ABSTRACT

A unique experimental equipment for extensive trials on the spray drying kinetics and particles residence time involving “in situ” analysis of the properties of continuous and dispersed phases was designed, built, and tested. Advanced experimental techniques (including laser techniques) to determine current parameters of spray drying process (temperature, humidity, moisture content) and current structure of spray (particle size distribution, particle velocities, etc.) were employed. Full scale spray drying tests of baker's yeast and maltodextrin enabled identification of the effect of process parameters on drying kinetics and spray residence time in the tower. Quantitative relationship describing spray drying kinetics as a function of atomization ratio and drying agent temperature were determined. The experimental results proved that spray residence time was controlled by atomization ratio and airflow rate. Drying kinetics in spray drying process is presented for the first time in the literature.     

Artificial Neural Network Modeling of the Deposition Rate of Lactose Powder in Spray Dryers

A spray dryer is the ideal equipment for the production of food powders because it can easily impart well-defined end product characteristics such as moisture content, particle size, porosity, and bulk density. Wall deposition of particles in spray dryers is a key processing problem and an understanding of wall deposition can guide the selection of operating conditions to minimize this problem. The stickiness of powders causes the deposition of particles on the wall. Operating parameters such as inlet air temperature and feed flow rate affect the air temperature and humidity inside the dryer, which together with the addition of drying aids can affect the stickiness and moisture content of the product and hence its deposition on the wall. In this article, an artificial neural network (ANN) method was used to model the effects of inlet air temperature, feed flow rate, and maltodextrin ratio on wall deposition flux and moisture content of lactose-rich products. An ANN trained by back-propagation algorithms was developed to predict two performance indices based on the three input variables. The results showed good agreement between predicted results using the ANN and the measured data taken under the same conditions. The optimum condition found by the ANN for minimum moisture content and minimum wall deposition rate for lactose-rich feed was inlet air temperature of 140°C, feed rate of 23 mL/min, and maltodextrin ratio of 45%. The ANN technology has been shown to be an excellent investigative and predictive tool for spray drying of lactose-rich products.     

Spray drying conditions and encapsulating composition effects on formation and properties of sodium diclofenac microparticles

This paper reports the preparation and characterization of sustained release sodium diclofenac microparticles by spray drying. Aqueous dispersions of ethyl cellulose (Surelease®) and Eudragit RS 30 D® were evaluated as controlled release polymers. The product properties (product moisture, size distribution, particle morphology, flow properties, total drug load, in-vitro dissolution studies, and encapsulating efficiency) were determined as a function of inlet temperature of the spray drying, the feed flow rate and composition of the microencapsulating formulation. In general, lower values of the product moisture content were observed at higher drying temperatures. The spray-dried product was composed mainly by rounded-shape and multi-size particles. The mean particle diameters of the Eudragit based microparticles tended to be slight bigger than the Surelease based microparticles. The spray dried microparticles showed delayed drug dissolution rates, sustaining the drug release for several hours. These findings confirm the feasibility of the spray drying for preparation of microparticles with sustained release properties. The physical and chemical properties of the microparticles can be changed by varying the spray drying parameters as well as the microencapsulating formulation.     

Theoretical study of the inactivation of phosphatase during spray drying of skim-milk

A theoretical calculation is presented of the drying history of skim-milk droplets under spray drying conditions. From the unsteady state diffusion equation the water concentration distribution is calculated as a function of time; simultaneously the thermal degradation of the enzyme alkaline phosphatase is calculated and integrated over the particle. Effects accounted for are the temperature and concentration dependence of the water diffusion coefficient and of the degradation rate constant, and the shrinkage due to water loss. Droplet geometries considered are the “solid sphere” model (fully liquid droplets) and the “hollow sphere” model (with air bubble in the centre). The effect on final phosphatase retention of the following process variables was investigated: dissolved solids content of the feed, air temperature, particle size, and gas bubble size.     

不同干燥方式制备白果粉的性能比较

天然产物白果会因干燥方式的不同,而使得干燥白果粉性能有所差别。本研究分别采用喷雾干燥(SP)与真空冷冻干燥(FD)对白果浆进行干燥处理。然后对两种干燥白果粉的性能(含水量、颗粒度、色泽、蛋白质质量分数)进行对比来比较各自的优越性。喷雾干燥采用参数:风量120 m³/h,进料浓度8%(质量分数),进气温度205℃,出气温度100℃,雾化器转速32000 r/min。真空冷冻干燥先在-40℃下预冻4h后,再在真空度300 Pa下-50℃低温干燥48 h。结果发现含水量SP相似文献   

Single-droplet drying processes at varying environmental conditions

Abstract

Modeling and numerical simulations of the single-droplet drying process are commonly executed based on the assumption of constant boundary conditions. In this study, the validity of this assumption and its influence on the model prediction of the final particle morphology is investigated. Accordingly, numerical simulations of the single-droplet drying process were conducted at different drying conditions. Five boundary conditions were examined: (a) constant inlet drying air condition based on the most commonly used assumption, (b) varying drying conditions, (c) constant average drying conditions, (d) partially varying drying conditions whereby all drying conditions were changed apart from the droplet’s relative velocity, and (e) velocity varying condition whereby all the drying conditions were averaged apart from the relative velocity of the droplet. The boundary conditions for the last four cases were calculated using three-dimensional simulations of the spray drying process of the particles that possessed pure solvent properties. The final product morphologies have been examined, i.e., the morphologies of hollow or full porous particles as predicted by the simulations of the single-droplet drying process. It has been found that the variation of the drying boundary conditions had considerable influence on the droplet’s shrinking rate as well as on the efficiency of the process, while the dried particle morphology depended on its shell strength. The influence was more pronounced when the initial droplet diameter and its shell strength increased.     

LEAFLASH SPRAY DRYER: INVESTIGATION OF THE ATOMIZATION PROCESS

The atomization process of the LEAFLASH spray dryer has been investigated by laser diffractometry and video imaging. The LEAFLASH atomizer is a particular pneumatic nozzle where the pressurized gas is the hot drying air. The drying and the atomization processes are interrelated in the spray dryer. Consequently the mixing of the liquid droplets and the drying medium is very efficient, permitting to work with short drying duration and reduced chamber volume. The mean diameter and the drop size distribution are measured at the outlet of the nozzle by laser diffraction. We studied the coupling effects of the air temperature (150 to 300° C) and pressure (1.20 to 1.50 bars abs) and of the dry matter content of the liquid feed (aqueous maltodextrin solution, 20 to 55% w/ w) on the droplets/ size distribution and on the general pattern of the spray. Analyses of video images of the generated spray give the general pattern of the spray and an estimation of the liquid velocity     

循环流化床中C类颗粒连续干燥的研究

循环流化床(CFB)作为一种新兴反应器,其结构简单、气固接触效率高、处理量大,成为气固二相干燥应用研究的新方向.文中在自建的循环流化床(内径0.104 m×高2.35 m)内,以玉米淀粉(dp=8 μm,ρp=800 kg/m3)为C类颗粒,进行了连续干燥.实验初步研究了进料速率、进风温度及气速等操作参数对淀粉平均停留...     

COMBINED CONVECTIVE AND INFRARED DRYING OF A CAPILLARP POROUS BODY

Abstract

This work investigates the effect of spray drying conditions on some properties of tomato powder prepared by spray drying of tomato pulp. A pilot scale spray dryer (Buchi, B-191) with cocurrent regime and a two-fluid nozzle atomizer was employed. Sixty-four different experiments were conducted keeping constant the feed rate, the feed temperature, and the atomizer pressure, and varying the compressed air flow rate, the flow rate of drying air, and the air inlet temperature. Tomato powders were analyzed for moisture, solubility, density (bulk and packed), and hygroscopicity. Analysis of experimental data yielded correlations between powder properties and the above-mentioned variable operating conditions. Regression analysis was used to fit a full second order polynomial, reduced second order polynomials and linear models to the data of each of the properties evaluated. F values for all reduced and linear models with an R ² ≥ 0.70 were calculated to determine if the models could be used in place of full second order polynomials.     

Spray Drying of Mannitol as a Drug Carrier—The Impact of Process Parameters on Product Properties

Powders intended for the use in dry powder inhalers have to fulfill specific product properties, which must be closely controlled in order to ensure reproducible and efficient dosing. Spray drying is an ideal technique for the preparation of such powders for several reasons. The aim of this work was to investigate the influence of spray-drying process parameters on relevant product properties, namely, surface topography, size, breaking strength, and polymorphism of mannitol carrier particles intended for the use in dry powder inhalers. In order to address this question, a full-factorial design with four factors at two levels was used. The four factors were feed concentration (10 and 20% [w/w]), gas heater temperature (170 and 190°C), feed rate (10 and 20 L/h), and atomizer rotation speed (6,300 and 8,100 rpm). The liquid spray was carefully analyzed to better understand the dependence of the particle size of the final product on the former droplet size. High gas heater temperatures and low feed rates, corresponding to high outlet temperatures of the dryer (96–98°C), led to smoother particles with surfaces consisting of smaller crystals compared to those achieved at low outlet temperatures (74–75°C), due to lower gas heater temperatures and higher feed rates. A high solution concentration of the feed also resulted in the formation of comparably rougher surfaces than a low feed concentration. Spray-dried particles showed a volume-weighted mean particle size of 71.4–90.0 µm and narrow particle size distributions. The mean particle size was influenced by the atomizer rotation speed and feed concentration. Higher rotation speeds and lower feed concentrations resulted in smaller particles. Breaking strength of the dried particles was significantly influenced by gas heater temperature and feed rate. High gas heater temperatures increased the breaking strength, whereas high feed rates decreased it. No influence of the process parameters on the polymorphism was observed. All products were crystalline, consisting of at least 96.9% of mannitol crystal modification I.     

Agglomeration in Spray Drying Installations (The EDECAD Project): Stickiness Measurements and Simulation Results

Spray drying is used for the manufacture of many consumer and industrial products such as instant dairy and food products, laundry detergents, pharmaceuticals, ceramics, and agrochemicals. During spray drying, agglomerates of powder particles are formed that determine the instant properties of the powder. Agglomeration during spray drying is considered to be a difficult process to control. The main cause of this is the complex interaction of the process variables: the atomization process, the mixing of spray and hot air, the drying of suspension droplets, and the collision of particles, which might lead to coalescence or agglomeration. As a consequence, agglomeration during spray drying is operated by trial and error. In an EC-sponsored project, named the EDECAD project and coordinated by NIZO food research, an industrially validated computer model, using CFD technology, to predict agglomeration processes in spray drying machines is developed. A Euler-Lagrange approach with appropriate elementary models for drying, collision, coalescence, and agglomeration of the dispersed phase is used. The main result of the EDECAD project is a so-called design tool, which establishes relations between the configuration of the drying installation (geometry, nozzle selection), process conditions, product composition, and final powder properties. The design tool has been validated on pilot plant scale and industrial scale. This article presents the setup and results of dynamic stickiness tests and some CFD simulation and validation results.     

Agglomeration in Spray Drying Installations (The EDECAD Project): Stickiness Measurements and Simulation Results

Spray drying is used for the manufacture of many consumer and industrial products such as instant dairy and food products, laundry detergents, pharmaceuticals, ceramics, and agrochemicals. During spray drying, agglomerates of powder particles are formed that determine the instant properties of the powder. Agglomeration during spray drying is considered to be a difficult process to control. The main cause of this is the complex interaction of the process variables: the atomization process, the mixing of spray and hot air, the drying of suspension droplets, and the collision of particles, which might lead to coalescence or agglomeration. As a consequence, agglomeration during spray drying is operated by trial and error. In an EC-sponsored project, named the EDECAD project and coordinated by NIZO food research, an industrially validated computer model, using CFD technology, to predict agglomeration processes in spray drying machines is developed. A Euler-Lagrange approach with appropriate elementary models for drying, collision, coalescence, and agglomeration of the dispersed phase is used. The main result of the EDECAD project is a so-called design tool, which establishes relations between the configuration of the drying installation (geometry, nozzle selection), process conditions, product composition, and final powder properties. The design tool has been validated on pilot plant scale and industrial scale. This article presents the setup and results of dynamic stickiness tests and some CFD simulation and validation results.     

Spray drying of mannitol carrier particles with defined morphology and flow characteristics for dry powder inhalation

This study was dealing with the spray drying of tailored mannitol particles as carriers in dry powder inhalation formulations. A self-constructed spray tower equipped with a laminar rotary atomizer was used to generate very narrow particle-size distributions. A design of experiments with rotation speed and drying temperature as factors was applied for the preparation of a broad set of different mannitol particles. Drying parameters affected particle properties like particle size, particle shape, surface roughness, and flowability significantly. Here, rotation speed was mainly affecting droplet and therefore particle size. Further, it was found that the inner particle temperature, and so the pressure inside the early particle shell, plays an important role during particle formation as emerging water vapor at higher temperatures served for indented particles and rough surface structures. Lower drying temperatures resulted in spherical and smooth particles as the inner temperature remained below the boiling temperature. The occurrence of these particle properties could further be related to mannitol carrier particle flow dynamics as large indented carriers were found to be less flowable than small spherical ones. In general, it was possible to control particle properties by the parameters of the spray drying process.