Modeling of Vacuum Desorption in Freeze-Drying Process

A mathematical model of multicomponent vacuum desorption, which occurs in vacuum freeze-drying process, was developed. In freeze-drying porous biomaterials and pharmaceuticals are considered and the vacuum freeze-drying process, especially the moisture desorption in its final stage, is investigated. In this article, the drying with conductive heating and constant contact surface temperature was considered. Pressure drop is taken into account in the model formulation but was neglected in process simulation because of thin material layers undergoing freeze-drying. Model equations were solved by numerical method of lines. Moisture content and temperature distributions within the drying material were predicted from the model as a function of drying time.     

Porous frozen material approach to freeze-drying of instant coffee

Abstract

Porous frozen material with a certain initial porosity was prepared to explore its influence on freeze-drying experimentally. Soluble coffee was selected as the solute in aqueous solution and liquid nitrogen ice-cream making method was used to prepare the frozen materials. Results showed that freeze-drying can be significantly enhanced using the initially porous frozen material compared with the traditionally solid one. By keeping the same sample mass and moisture content with sole radiation heating, drying time of the porous frozen sample was about one third shorter than that of the solid one under the same tested operating conditions. SEM images of dried products revealed that the porous material had a loose and tenuous structure that was favorable to the transportation of sublimated vapor and the desorption of bound moisture. Appropriately increasing the chamber surface temperature benefited the freeze-drying process and changing the chamber pressure had little effect on the process. Combined radiation and conduction heating can further promote the freeze-drying process and save as much as 36.4% of the drying time. The porous frozen material was found to have a wider range of operating temperature and result in relatively lower residual moisture content.     

Kinetic and Quality Study of Mushroom Drying under Microwave and Vacuum

Abstract

The aim of this work is to model the drying kinetics of mushrooms under several operational conditions, to evaluate the effective diffusivity coefficient of moisture removing by a drying model and inverse calculus method in finite differences and to study the effect on the final quality of dehydrated mushrooms. Different ways of microwave vacuum drying were compared to freeze-drying. Results show that a decrement of the applied pressure produces a certain increase in the drying rate together with a lower moisture in the dehydrated product at the end. Temperature control inside the sample helps to ensure a better quality in the dehydrated product, than when controlled at the surface. Diffusivity coefficients show a correspondence with product temperature during drying. The microwave dried samples obtained with moderate power and temperature control of product shown an important degree of quality similar to that obtained by freeze-drying.     

Theoretical Study on Microwave Freeze-Drying of an Aqueous Pharmaceutical Excipient with the Aid of Dielectric Material

Abstract

A mathematic model of simultaneous heat and mass transfer for the dielectric material assisted microwave freeze-drying was derived and solved numerically using the finite-deference technique with two moving boundaries. Lactose, a typical pharmaceutical excipient, was used as the representative solid material in the aqueous solution to be freeze-dried. Silicon carbide (SiC) was selected as the dielectric material. Numerical results show that the dielectric material can significantly enhance the microwave freeze-drying process. Under typical operating conditions, the drying time is 43% shorter than that of ordinary microwave freeze-drying. Temperature variations at sublimation fronts were examined in order to determine the appropriate microwave power input. Profiles of temperature, ice saturation, vapor concentration, and pressure during freeze-drying are presented, and rate-controlling mechanisms are discussed.     

VACUUM CONTACT DRYING OF SELECTED BIOTECHNOLOGY PRODUCTS

ABSTRACT

The paper is mainly concentrated on investigations of the vacuum contact drying of the following biomaterials: (1) beer yeast, (2) whey and its components: proteinaceous liquid, lactose, post-lactose liquid, (3) saturated solution of the citric acid, (4) post-fermentation broth of the fodder antibiotic bacitracin. The investigations of vacuum contact drying process in which dried material adheres closely to a hot surface were performed. In order to make possible the determination of optimal process parameters the measurements were performed for various constant temperatures of the hot surface, total pressures in vacuum chamber and layer thickness of biomaterials.

The effective thermal properties for dry layers of selected biomaterials depending on temperature and total pressure were also experimentally determined.

A mathematical model of the vacuum contact drying for most intensive regime of its performance i.e. boiling one was presented. It will enable the process simulation and estimation of the dryers efficiency depending on process parameters.

In addition, investigations of beer yeast viability depending on the hot surface temperature and the total pressure were performed.     

Numerical Investigation on Dielectric Material Assisted Microwave Freeze-Drying of Aqueous Mannitol Solution

Abstract

The dielectric material assisted microwave freeze-drying was investigated theoretically in this study. A coupled heat and mass transfer model was developed considering distributions of the temperature, ice saturation and vapor mass concentration inside the material being dried, as well as the vapor sublimation-desublimation in the frozen region. The effects of temperature and saturation on the effective conductivities were analyzed based on heat and mass flux equations. The model was solved numerically by the variable time-step finite-deference technique with two movable boundaries in an initially unsaturated porous sphere frozen from an aqueous solution of mannitol. The sintered silicon carbide (SiC) was selected as the dielectric material. The results show that dielectric material can significantly enhance microwave freeze-drying process. For case of the dielectric field strength, E = 4000 V/m under typical operating conditions, the drying time is 2081 s, 30.1% shorter and 47.2% longer, respectively, than those for E = 2000V/m and E = 6000 V/m. The heat and mass transfer mechanisms during the drying process were discussed.     

THE INFLUENCE OF PRESSURE AND TEMPERATURE ON THE KINETICS OF VACUUM DRYING OF KETOPROFEN

ABSTRACT

This paper explores the influence of temperature and pressure on drying kinetics of 2-(3-benzoylphenil propionic acid) ketoprofen, in a vacuum dryer on laboratory scale, Experimentally determined relations between moisture content and drying rate vs time, were approximated with an exponential model. Model parameters were correlated with drying conditions (temperature, pressure) and defined by functions of their potentions.

From an energy balance of the process, a mathematical model for simulating dependence of sample temperature vs drying time, and moisture content of material, has been developed.

Simulation of the drying kinetics and sample temperature, by use of those functional dependencies shows good agreement with experimental results.     

Optimal Control of the Primary Drying Stage of Freeze Drying of Solutions in Vials Using Variational Calculus

Abstract

The problem of operating freeze drying of pharmaceutical products in vials placed in trays of a freeze dryer to remove free water (in frozen state) at a minimum time was formulated as an optimal control problem. Two different types of freeze dryer designs were considered. In type I freeze dryer design, upper and lower plate temperatures were controlled together, while in type II freeze dryer design, upper and lower plate temperatures were controlled independently. The heat input to the material being dried and the drying chamber pressure were considered as control variables. Constraints were placed on the system state variables by the melting and scorch temperatures during primary drying stage. Necessary conditions of optimality for the primary drying stage of freeze drying process in vials are derived and presented. Furthermore, an approach for constructing the optimal control policies that would minimize the drying time for the primary drying stage was given. In order to analyze optimal control policy for the primary drying stage of the freeze-drying process in vials, a rigorous multi-dimensional unsteady state mathematical model was used. The theoretical approach presented in this work was applied in the freeze drying of skim milk. Significant reductions in the drying times of primary drying stage of freeze drying process in vials were obtained, as compared to the drying times obtained from conventional operational policies.     

ANALYTICAL SOLUTIONS FOR THE MOVING INTERFACE PROBLEM IN FREEZE-DRYING WITH OR WITHOUT BACK HEATING

ABSTRACT

A mathematical model for freeze-drying without back surface heating is established first in this paper by a combination of URIF (uniformly retreating ice front) and Sheng/Peck's theories. Explicit analytical expressions are obtained for the rates of interface movement and drying. The predicted drying rate and temperature profile are in good agreement with the Sheng/Peck's model results. Furthermore, the model is extended to the process of freeze-drying with back heating in which the temperature at the interface is assumed to increase along the path of movement. It is shown that the average rates for drying and interface moving may be obtained by assuming a quadric distribution for the interface temperature.     

Experimental Study on Microwave Vacuum Drying of Two-Porosity Level Media

Abstract

Microwave vacuum drying experiments were performed on a laboratory scale dryer with a two-level porosity material: a packed bed of porous alumina beads. The incident microwave power and the vacuum pressure level were fixed, the main varying parameters being the beads diameter and porosity, and the mean pore diameter. The drying kinetics and the evolution of the product temperature are presented. The drying kinetics can be divided into two main periods. The first one corresponds to the drying from the bed voids according to evaporation mechanism that we describe with a stagnant film law. The second one corresponds to the drying from the particle pores and we divide it into two parts: we suggest that the former is dominated by capillarity driven moisture transport, and the latter is limited by the desorption kinetics of the few water layers left.     

Diffuse interface model of the freeze-drying process of individually frozen products

Abstract

Vacuum freeze-drying (VFD) is a dehydration method based on the sublimation of the liquid phase contained in a certain product, previously frozen, at low pressure and temperature. Since it is a time and energy consuming process, it is crucial to select the best processing conditions to minimize drying duration, thus reducing the energy requirement. Additionally, product temperature must be monitored since it plays an important role in preserving product quality. The aim of this study was to develop a Diffuse Interface Model (DIM) for in-silico simulation of the freeze-drying process of individually frozen products. Due to the geometrical features of the samples, and to the role of radiation in the heat transfer to the product, the usual one-dimensional approach is inappropriate. Using a DIM, each cell of the computational domain can be described as a porous solid matrix filled by ice and vapor with a time-varying composition, thus allowing the use of a fixed computational grid and making the computation effort less demanding in comparison to moving interface-based models. Drying of eggplant cubic samples was considered as case study: model parameters were estimated by fitting the experimentally measured product temperature and drying time to the calculated ones. The model was proven to be reliable in providing an accurate estimate of both the drying time and the product temperature. Therefore, it can be used for off-line process design and optimization, minimizing the experimental effort required to design and optimize the process.     

MICROWAVE VACUUM DRYING KINETICS OF SOME FRUITS

ABSTRACT

Microwave vacuum drying kinetics of three fruits (namely, apple, kiwi and pear) were studied by introducing an one-parameter empirical mass transfer model, involving a characteristic parameter (drying constant), as a function of process variables. The model was tested with data produced in a microwave oven equipped with vacuum apparatus, using non-linear regression analysis. The investigation involved a wide range of microwave power and vacuum pressure levels. The parameters of the model considered were found to be greatly affected by the microwave power level while vacuum pressure affected slightly the process.     

Freeze-Drying of Skim Milk in a Cylindrical Container

Abstract

An experimental study on freeze-drying of skim milk in a cylindrical container was conducted to provide fundamental data essential for numerical studies on the process. Temperature histories at different positions were carefully measured during each experimental run and the measured temperature histories were combined to produce instantaneous temperature fields inside the container. In addition, mass reduction history by sublimation of ice was also measured with the same drying conditions. The obtained temperature fields clearly indicated multi-dimensional drying characteristics of the freeze-drying in the cylindrical container. Along with the experiments, the process was simulated with an analysis program developed for this study, based on a finite volume method with a moving grid system. The numerical and experimental results were in good agreement.     

Effect of Dielectric Material on Microwave Freeze Drying of Skim Milk

Abstract:

A simultaneous heat and mass transfer model of the dielectric material–assisted microwave freeze drying was derived in this study considering the vapor sublimation-desublimation in the frozen region. The mathematical model was solved numerically by using the finite-difference technique with two moving boundaries. Silicon carbide (SiC) was selected as the dielectric material, and the skim milk was used as the representative solid material in the aqueous solution to be freeze-dried. The results show that the dielectric material can significantly enhance the microwave freeze drying process. The drying time is greatly reduced compared to cases without the aid of the dielectric material. Profiles of the temperature, ice saturation, vapor concentration, and pressure during freeze drying were presented. Mechanisms of the heat and mass transfer inside the material sphere were analyzed. For an initially unsaturated frozen sample of 16 mm in diameter with a 4-mm-diameter dielectric material core, the drying time is 288.2 min, much shorter than 380.1 min of ordinary microwave freeze drying and 455.0 min of conventional vacuum freeze drying, respectively, under typical operating conditions.     

MICROWAVE FREEZE DRYING CHARACTERISTICS OF BEEF

ABSTRACT

Microwave freeze drying characteristics of unsaturated raw beef were studied experimentally for various levels of electric field strength, vacuum pressure, sample thickness and initial saturation. The results show that drying time is proportional to initial saturation and inversely proportional to the electric field strength and sample thickness. The effect of vacuum pressure on drying time is negligible. Some advantages of microwave freeze-drying over conventional freeze drying with radiant heating are pointed out     

Analysis of Freeze-Drying of Tropical Fruits

Abstract

Freeze-drying is a process recommended for drying of heat-sensitive products. Some advantages of this technique are that it allows the shrinkage and the degrading reactions in the material, which are common in conventional drying operations, to be minimized. The knowledge of drying kinetics is essential for modeling and optimization of a freeze-drying process. In this work, drying kinetics for pineapple, guava, and mango pulps were investigated using five empirical equations commonly applied for convective drying of foodstuffs. Increasing constant- and falling-rate periods were observed during the drying of such pulps. The best fittings for the drying kinetics of all the materials were obtained using the Page and Chen and Douglas equations.     

DRYING RELATED PROPERTIES OF APPLE

ABSTRACT

Drying related properties of apple are evaluated for various different drying methods (namely, convective, vacuum, microwave, osmotic and freeze drying), and their corresponding process conditions. The examined properties are drying kinetics, equilibrium material moisture content, density, porosity, color and viscoelastic characteristics. The effect of various process factors on these properties is described through particular mathematical models. The model parameters are estimated by fitting the corresponding model equations on a wide range of experimental data. Drying kinetics is greatly affected by the characteristic particle size and drying air temperature for convective drying, while for the case of microwave drying they are affected by the vacuum pressure and the emitted radiation power. Equilibrium material moisture content is affected by the temperature and the humidity of the surrounding air, while the osmotic pretreatment shifts the sorption isotherms to higher water activity levels. The quality properties examined, are significantly affected by the drying method. More specifically, osmotic dehydration decreases the porosity of the final product, while it prevents color deterioration and enchances the viscous nature of dehydrated apple. Freeze-dried apples develop the highest porosity, have the most elastic structure and the lowest rate of color deterioration.     

丁二磺酸腺苷蛋氨酸冻干工艺研究

为建立合适的丁二磺酸腺苷蛋氨酸冻干工艺,采用真空冷冻干燥法,对丁二磺酸腺苷蛋氨酸冻干条件如共晶点、装量、预冻程序、升华温度、升华真空度及解吸干燥温度等进行研究。结果显示：冻干工艺：装量为液面高度小于10 mm,预冻程序为预冻至-40℃,然后回温至-10℃,再降至-50℃,在真空度10～30 Pa,-25℃下升华,35℃解吸干燥。此工艺制备的丁二磺酸腺苷蛋氨酸外观好,产品质量符合国家标准。     

A Comparative Study of Low-Pressure Superheated Steam and Vacuum Drying of a Heat-Sensitive Material

Abstract

Using carrot cubes as a model heat-sensitive material, experimental investigations were conducted to examine the drying kinetics and various quality parameters of the dried product undergoing both low-pressure superheated steam and vacuum drying. Effects of operating parameters such as pressure and temperature on the drying characteristics as well as quality attributes, i.e., volume, shrinkage, apparent density, color, and rehydration behavior, of the dried product underwent the two drying processes were also evaluated and compared. Although low-pressure steam drying required longer dwell time to achieve the same final moisture content than vacuum drying, some of the quality attributes were superior to those obtained in vacuum drying.     

Freeze-Drying of the Black Currant Juice

ABSTRACT

The effect of drying temperature of the black currant juice on the retention of vitamin C and anthocyanins content as well as drying kinetics in the freeze-dried process, has been studied. Non clarified, black currant juice was freered on plates in the layer of 15 mm thick until the temperature of -30 °C in the thermal center of sample has been reached. Plates with frozen layers of juice were subject of freeze-drying process at 5 different temperatures of the heating plate (20, 30. 40, 50 and 60 °C). Studies of the retention of vitamin C and anthocyanins after, drying were carried out. freeze-drying of black currant juice should be carried out at the temperature not higher than 40°C to preserve content of vitamin C and anthocyanins.