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

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.     

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.     

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.     

Sublimation Kinetics during Freeze-Drying of Pharmaceutical Protein Formulation

The influence of total gas pressure and shelf temperature on sublimation kinetics of BSA-based formulation in glass vial as geometrical configuration was determined with a pilot freeze-dryer in standard operating freeze-drying conditions.

The sublimation rate curves showed three different periods with a plateau corresponding to a stationary regime. These kinetics data were mainly dependent on the shelf temperature and slightly influenced by the total gas pressure. Thus, the sublimation process in our conditions was mainly governed by overall heat transfer rate from the plate and from the surroundings to the sublimation front.

Moreover, it proved that the water vapor mass transfer mechanism through the dried layer occurs by molecular diffusion in Knudsen regime.

Finally, these experimental sublimation kinetics data were found in a quite fair agreement with the set up results. They confirm the validation of previous modeling of mean product temperature profiles during the freeze-drying by using the finite element code FEMLAB in real vial geometry (2-D).     

Sublimation Kinetics during Freeze-Drying of Pharmaceutical Protein Formulation

The influence of total gas pressure and shelf temperature on sublimation kinetics of BSA-based formulation in glass vial as geometrical configuration was determined with a pilot freeze-dryer in standard operating freeze-drying conditions.

The sublimation rate curves showed three different periods with a plateau corresponding to a stationary regime. These kinetics data were mainly dependent on the shelf temperature and slightly influenced by the total gas pressure. Thus, the sublimation process in our conditions was mainly governed by overall heat transfer rate from the plate and from the surroundings to the sublimation front.

Moreover, it proved that the water vapor mass transfer mechanism through the dried layer occurs by molecular diffusion in Knudsen regime.

Finally, these experimental sublimation kinetics data were found in a quite fair agreement with the set up results. They confirm the validation of previous modeling of mean product temperature profiles during the freeze-drying by using the finite element code FEMLAB in real vial geometry (2-D).     

介电材料辅助的微波冷冻干燥的实验研究

设计、加工和装配了一套实验室规模的微波冷冻干燥装置,旨在实验验证介电材料对微波冷冻干燥液体物料的强化作用。介电材料用烧结的碳化硅(SiC),石英玻璃作为介电材料的参照物;甘露醇,一种典型的药物赋形剂被选为待干溶液中的溶质。实验结果表明使用介电材料可以有效地强化微波冷冻干燥过程。与传统冷冻干燥相比干燥速率大大加快,在试验条件下干燥时间可以节省20%。微波加热逐渐生效并且主要体现在干燥过程的后半部分。当溶液中的固含量很低或者固体物质具有很小的介电损耗因子时,如果不用介电材料,微波加热的效果不明显。     

介电材料辅助的微波冷冻干燥的数值模拟

通过数值求解一个考虑吸湿效应的带有移动升华界面的多孔介质热、质传递耦合模型,理论考察介电材料对微波加热冷冻干燥过程的影响.介电材料用烧结的碳化硅(SiC).甘露醇,一种典型的药物赋形剂被选为待干溶液中的溶质.模拟结果表明在微波冷冻干燥过程中使用介电材料可以加快冷冻干燥速率,特别是在待干溶液的固含量很低或者固体产品的介电损耗因子很小的情况下尤为有效.模型预测和实验测定的干燥曲线相比较显示了良好的一致性.通过考察冰饱和度和温度的分布侧形,研究分析了物料内部的质热传递机理,并讨论了干燥速率的控制因素.     

Determination of Optimum Drying Condition of VIP Core Material by Wet Method

Vacuum insulation panel (VIP) core materials were successfully fabricated by wet method. The phase composition, microstructure, and thermal conductivity of VIP core materials were investigated. The density of VIP core materials was 176 kg/m³, while the mean thermal conductivity of VIP core materials was about 31 mW/(m · K). The mean thermal conductivities of VIPs were 2.78 mW/(m · K), 2.62 mW/(m · K), 2.47 mW/(m · K), 2.5 mW/(m · K), and 2.4 mW/(m · K), which correlated to VIP core materials that had been dried at 150°C for 30 min, 60 min, 90 min, and at 170°C for 30 min and 60 min, respectively. However, the mean thermal conductivity evaluated for VIPs with core material that had not been dried was 3.0 mW/(m · K). The thermal conductivity of VIPs with core material that had been dried reached a maximum on the third day and tended to be a steady value with time, whereas the one with core material that had not been dried recorded a high thermal conductivity value and continued to rise in a fluctuating pattern with time. According to the result of the thermogravimetric curve, drying at 150°C for 60 min showed characteristics of complete drying. In addition, the thermal conductivity of VIPs at this drying condition was low and stable. Theoretical and experimental analysis showed that the optimum drying condition for fiberglass VIP core materials was drying at 150°C for 60 min.     

冷冻干燥过程的实验研究

冷冻干燥过程的实验研究涂伟萍，田文清，杨卓如，陈焕钦，谭盈科（华南理工大学化学工程研究所，广州５１０６４１）关键词冷冻干燥；热质传递１前言冷冻干燥法最主要的特点是在冷冻干燥过程中物品内部的不可逆变化很小，能保持物品的色、香、味、形基本不变，是生产优质...     

Numerical investigation on freeze-drying of aqueous material frozen with pre-built pores

Freeze-drying of the initially porous frozen material with pre-built pores from liquid material was found experimentally to save drying time by over 30% with an initial saturation being 0.28 compared with the conventional operation with the initial saturation being 1, using mannitol as the solid material. In order to understand the mass and heat transfer phenomena of this novel process, a two-dimensional mathematical model of coupled mass and heat transfer was derived with reference to the cylindrical coordinate system. Three adsorption–desorption equilibrium relationships between the vapour pressure and saturation value namely, power-law, Redhead's style and Kelvin's style equation, were tested. Kelvin's style in exponential form of adsorption equilibrium relation gave an excellent agreement between the model prediction and experimental measurement when the equation parameter, γ, of 5000 was applied. Analyses of temperature and ice saturation profiles show that additional heat needs to be supplied to increase the sample temperature in order to promote the desorption process. Simulation also shows that there is a threshold initial porosity after which the drying time decreased with the increase in the initial porosity. Enhanced freeze-drying is expected to be achieved by simultaneously enhancing mass and heat transfer of the process.     

Scale-up and Process Transfer of Freeze-Drying Recipes

This paper proposes a simple and effective methodology for the scale-up and process transfer of freeze-drying recipes. Process modeling allows the study of the silico product evolution in a given freeze-dryer, and calculation of the operating conditions that result in the same product dynamics in different equipment. Few experiments are necessary to determine model parameters and to characterize the two freeze-dryers. The problem of the batch non-uniformity and the effect of the parameters' uncertainty are also addressed. The effectiveness of this approach is demonstrated by means of various examples.     

Combined Convective and Microwave Drying of Agglomerated Sand: Internal Transfer Modeling with the Gas Pressure Effect

In order to improve the industrial drying (hot air and microwave) of inserts made of agglomerated sand, a comprehensive internal heat and water transfer model has been proposed. In this model, the internal gas phase pressure effect was made perfectly explicit, especially the phenomena of liquid and vapour transfer by filtration and of liquid expulsion at the surface. This model was validated on the basis of the experimental mean water content and core temperature curves for drying trials at different microwave powers. Then, it was used for comparing the drying time and the internal pressure level calculated for four particular processes: a standard process with high temperature air applied all over the time, a strong process with high power microwaves applied all over, and two processes which alternate the two heating modes. It was demonstrated that the combined and alternative processes provide a real possibility for faster drying with less internal pressure and thus with less cracking risk. The microwaves should be applied only in the first hour of the process and with decreasing power. The decrease of the drying time was around 30% with regard to the hot air standard process.     

Performance Optimization of a Brick Dryer Using Porous Simulation Approach

In the present study, an innovative method for an accurate simulation and design of a chamber dryer used in the brick/ceramic industry has been proposed. A thorough investigation of currently used dryers is conducted and optimization criteria are detected and discussed. Three-dimensional modeling of the chamber dryer has been performed. In the second step, from the result of 3D modeling, the critical values for heat transfer coefficient are obtained. The governing equations for a two-dimensional brick as a porous solid are derived by combining conservation laws and Fourier's law for heat conduction and Darcy's and Fick's laws for mass diffusion in porous material. The set of partial differential equations governing heat and mass transport in a single brick together with the respective temperature and humidity boundary conditions have been solved numerically based on finite difference method. Finally, an efficient scheme for the air circulation devices, inlet air temperature and humidity, burner characteristics, flow rates, and drying process control have been proposed for a typical industrial-scale brick dryer.     

Free Heat and Mass Transfer in a Porous Enclosure with Side Vents

Free heat and mass transfer during drying in a porous enclosure with free vents has been investigated numerically. Enclosed moist air interacts with the surrounding air through freely vented ports situated on both sides perpendicular to the heated wall. Air, heat, and moisture transport structures are visualized respectively by streamlines, heat lines, and mass lines. Effects of thermal Rayleigh number, Darcy number, vent location, and enclosure inclination on the convective heat/moisture transfer rate and volume flow rate across this enclosure are discussed. For each case, partially enclosed fluid flow undergoes different phases, increasing with buoyancy ratio; that is, heat transfer–driven flow, heat- and moisture-aided flow, and moisture transfer–dominated flow. Numerical results demonstrate that the convective heat and moisture transport patterns and transport rates greatly depend on thermal Rayleigh number, properties of porous medium, and enclosure inclination. Practices for enhancing heat and moisture transfer have been suggested for drying processes.     

具有电介质核心多孔介质微波冷冻干燥过程的耦合传热传质的数值研究

利用变时间步长的有限体积法对具有电介质核心多孔介质微波冷冻干燥的耦合热质传递过程进行了数值模拟。计算结果表明：在有电介质核的多孔介质内部存在着两个升华界面,该双升华界面模型成功地模拟了该干燥过程：合理的选用电介质核心可以大大缩短干燥时间,对于几个大小分别为1．0,1.5,2．0和2．5mm的电介质核,其单位体积所需干燥时间同无核相比分别减少了8％,19％,33％,48％：在相同的电场强度下,电介质核的损耗系数越大,所需干燥时间越短。     

不粘煤的微波－对流干燥研究

从不粘煤的特性出发，讨论了不粘煤工业干燥的要求；从微波－对流综合干燥传热传质原理分析，论证了这种干燥方式用于不粘煤干燥，在降低温度、控制负荷、提高经济性等方面都有显著成效，并以翔实的试验数据为理论分析作了辅证。     

不粘煤的微波－对流干燥研究

从不粘煤的特性出发，讨论了不粘煤工业干燥的要求；从微波－对流综合干燥传热传质原理分析，论证了这种干燥方式用于不粘煤干燥，在降低温度、控制负荷、提高经济性等方面都有显著成效，并以翔实的试验数据为理论分析作了辅证。     

真空冷冻干燥非稳态热质传递模型的应用

真空冷冻干燥非稳态热质传递模型的应用齐锡龄１杜小泽２李惟毅１（１天津大学热能工程系，天津３０００７２）（２清华大学热能工程系，北京１０００８４）关键词冷冻干燥热质传递升华压力１引言通过理论计算确定真空冷冻干燥速率或干燥时间对指导生产实践很有意义。但是...     

Reduction of the Volatile Matter Evolution Rate from a Plastic Pellet during Bubbling Fluidized Bed Pyrolysis by Using Porous Bed Material

Rapid volatile matter evolution from high‐volatile fuels such as wastes and biomass is one of problems associated with fluidized bed incinerators and gasifiers. When volatile matter evolves rapidly in the vicinity of the fuel feed point, the mixing of volatile matter with reactant gas is poor, and therefore, unreacted volatile matter is expected to be released from the reactor. In the present work, reduction of the volatile matter evolution rate was attempted by employing porous solids as bed materials instead of nonporous sand. The effect of bed material on the onset of devolatilization was measured by use of a bench‐scale bubbling fluidized bed reactor. Volatile matter capture by the porous solids (capacitance effect) and the heat transfer rate within the bed, both of which affect volatile matter evolution rate, were also measured. Four types of porous solids, both with and without capacitance effect, were employed as the bed material. By employing porous solids without capacitance effect, the contributions of reduced heat transfer rate and capacitance effect to the delay of volatile matter evolution can be evaluated separately. For porous bed materials with a moderate capacitance effect (volatile matter capture of up to 20 %), the delay of the onset of devolatilization, which was measured by detecting the flame combustion of the volatile matter, was explained by the lower heat transfer between the fuel and bed. However, for a porous particle with high capacitance effect (volatile matter capture of 30 %), the capacitance effect also affected the delay of the onset of the flame combustion.     

Simulation of Superheated Steam Drying from Coupling Models

Modeling of the transfer between a porous medium and its surroundings is commonly made using transfer coefficients that are theoretically well known only under boundary layer hypothesis. The resolution of Navier-Stokes equations in the surroundings of the product in order to get information about the boundary conditions avoids the classical use of these transfer coefficients. In this article, a modeling and a simulation of superheated steam drying of a rectangular piece of porous medium is proposed using a coupling method between a porous medium code and a CFD software. In some cases of superheated steam drying, even if a thermal boundary layer exists, a mass boundary layer cannot be defined. Moreover, boiling occurs during the process. An analysis of the interfacial transfer coupled with the analysis of the temperature, moisture content, and pressure profiles inside the porous medium is proposed.