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.     

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.     

Heat and mass transfer model of dielectric-material-assisted microwave freeze-drying of skim milk with hygroscopic effect

A new porous media mathematical model for freeze-drying was developed based on the adsorption-desorption relationship proposed in this paper. A finite difference solution was obtained from a moving boundary problem for the dielectric-material-assisted microwave freeze-drying process. Silicon carbide (SiC) was selected as the dielectric material; and frozen skim milk was used as the aqueous solution to be dried. Simulation results showed that the dielectric material can significantly enhance the microwave freeze-drying process. The drying time was 33.1% shorter than that of ordinary microwave freeze-drying under typical operating conditions. When the solid content of the solution to be freeze-dried was very low, or the solid product had a very small loss factor, microwave heating was less effective without the assistance of dielectric material. The mechanisms of heat and mass transfer during drying were analyzed based on profiles of ice saturation, temperature and vapor concentration. Drying rate-controlling factors were discussed. A comparison was made between the model predictions and the reported experimental data.     

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.     

吸湿多孔介质冷冻干燥传质传热模型

本研究在作者提出的吸附—解吸平衡关系的基础上,建立了一个全新的考虑吸湿效应的多孔介质冷冻干燥数学模型。模型用有限差分法进行求解,并带有一个移动边界,以模拟介电材料辅助的微波冷冻干燥过程。介电材料选用碳化硅（SiC）,原料液为脱脂奶。模拟结果表明：介电材料能够有效强化微波冷冻干燥过程。在典型操作条件下,介电材料辅助的微波冷冻干燥所用的时间比普通微波冷冻干燥减少33.1%。当料液中固体含量较低或者固体产品的损耗因子较小时,介电材料对微波加热的效果不明显。基于冰饱和度、温度和水蒸气浓度的分布,本文分析了干燥过程中的传质传热机理,并对干燥速率控制因素进行了讨论。     

具有预制孔隙的维生素C水溶液微波冷冻干燥

设计和组装了一套实验室规模的多功能微波冷冻干燥装置，探究了具有初始孔隙的非饱和物料微波冷冻干燥过程。以维生素C为溶质，采用“软冰”冷冻技术制备了初始饱和与非饱和的冷冻样品。结果表明，软冰冷冻制备的样品能够避免崩塌。在35℃和20 Pa条件下，初始非饱和物料的干燥时间比饱和物料缩短了30.4%。SEM表征显示，非饱和物料具有疏松的球状孔隙结构、连通性好，有利于水蒸气的迁移。采用吸波材料碳化硅辅助的微波加热能够进一步强化冷冻干燥过程。在相同条件下，非饱和物料的微波冷冻干燥(5 W功率)时间比常规冷冻干燥(0 W功率)缩短了28.1%，比饱和物料的常规冷冻干燥缩短了50.0%。吸波材料辅助的初始非饱和物料微波冷冻干燥实现了传热传质的同时强化。     

吸波材料辅助的液体物料微波冷冻干燥多物理场耦合模型

为了研究吸波材料辅助微波加热对传统冷冻干燥过程的强化作用,建立了多孔介质温度、浓度和电磁场耦合的多相传递模型;以烧结的碳化硅(SiC)为吸波材料、以甘露醇水溶液为待干料液进行了微波冷冻干燥实验,并测定了甘露醇固体的介电特性。模拟和实验结果均表明,吸波材料对初始非饱和多孔物料微波冷冻干燥具有显著的强化作用。初始非饱和样品微波冷冻干燥时间比传统冷冻干燥缩短了18%,比常规饱和样品传统冷冻干燥缩短了30%。模拟结果与实验数据吻合良好。这表明提出的新型干燥方法确实能够实现过程传热传质的同时强化。通过考察样品内部温度、饱和度和电场强度的实时分布,分析了微波冷冻干燥过程的传热传质和电磁波传播与耗散机理。在微波冷冻干燥过程中,初始非饱和样品累计吸收的辐射能和微波能的总和与传统冷冻干燥相当。这说明,该干燥方法只是提高了能量效率,从而大幅缩短了冷冻干燥时间。     

SIMULATION OF FLUIDIZED-BED DRYING OF CARROT WITH MICROWAVE HEATING

ABSTRACT

A mathematical model of coupled heat and mass transfer was applied to batch fluidized-bed drying with microwave heating of a heat sensitive material—carrot. Four kinds of microwave heating with intermittent variation were examined. The numerical results show that different microwave heating patterns can affect the fluidized bed drying significantly. Changing the microwave input pattern from uniform to intermittent mode can prevent material from overheating under the same power density. Supplying more microwave energy at the beginning of drying can increase the utilization of microwave energy while keeping temperature low within the particle. For a particle diameter of 4 mm, fluidization velocity of 2 m/s, inlet airflow temperature of 70°C and the bed area factor of 80, the drying time are 750 and 1000 s, respectively, for the two good operating conditions with on/off periods of 125/375 s and 375/375 s. The cumulative microwave energy absorbed by particles at the end of drying is 1415 and 2300 kJ/kg (dry basis), respectively.     

Drying of Potato Tissue Pretreated by Ohmic Heating

The influence of the ohmic heating pretreatment on convective drying of potato tissue was investigated. The degree of material damage Z under the different modes of electrical treatment is studied and the electroporation phenomena is assumed to be the main reason of material disintegration. The relations between Z, electric field strength E, energy input W, and temperature of ohmic heating T are analyzed. Two different damage stages, short and long, are revealed in this study. It is shown that ohmic treatment at relatively low fields (E < 100 V/cm) results in incomplete damage of material, but allows to obtain material with high disintegration degree Z ≈ 0.7 at E > 70 V/cm. The electric field strength E and the total electric energy input W influence considerably the drying rate. The highest drying rates are always observed for more energy consuming freeze-thawed pretreatment, but the AC pretreatment seems to be promising for enhancing the air drying processes.     

Optimization of Microwave Drying Biomass Material of Stem Granules from Waste Tobacco Using Response Surface Methodology

Tobacco stems, an underutilized waste in the tobacco industry, can be transformed into a viable product through the preparation of biomass material of stem granules. Response surface methodology (RSM) was used to optimize microwave drying of stem granules from waste tobacco. The effects of microwave power (35–40 kW), moisture content (25–35%), material thickness (30–50 mm), and drying time (90–150 s) on filling power and yield of stem granules were studied. Gas chromatography–mass spectroscopy (GC-MS) and scanning electron microscopy (SEM) were used to determine volatile components and microstructures of stem granules dried under optimal conditions. The filling power and yield of stem granules could be adequately fitted to a quadratic model (R ² = 0.951) and a two-factor interaction model (R ² = 0.887), respectively. The optimal conditions for microwave drying of stem granules were 35 kW, 30%, 30 mm, and 150 s. When prepared under optimal conditions, the filling power and yield of stem granules were 7.94 cm³/g and 64.06%, respectively, which differed by only 4.53 and 3.50% from model predictions. The quadratic and two-factor interaction models provided a reasonably accurate (<5% error) assessment of optimal conditions for microwave drying of biomass material of stem granules from waste tobacco stems.     

A Review on Freeze Drying of Drugs with tert-Butanol (TBA) + Water Systems: Characteristics,Advantages, Drawbacks

Organic cosolvent systems have been evaluated for their potential and increasing use for freeze drying of solutions to produce stabilized powders of marketed pharmaceutical products. The formulations most often investigated include tert-butanol (TBA) + water mixtures. These organic cosolvent systems present many interesting advantages: high freezing temperatures, very short sublimation time, low sublimation enthalpies, high equilibrium vapor/solid pressure values, and low toxicity.

Thus, some main characteristics of water + TBA systems have been reviewed, especially regarding its interesting thermodynamic properties (sublimation enthalpy, equilibrium vapor pressure), impact of freezing conditions on morphological properties of frozen formulations (nucleation, crystal size and shape), influence of operating parameters (total pressure, temperature) on sublimation times, and organic cosolvent and water residual contents.

The crystal morphology of frozen formulations prepared with TBA revealed unexpected results compared with the results reported in the literature for water-based formulations in terms of the complex relationships between freezing rates, supercooling, nucleation temperatures, and solvent crystal morphology (size and shape).

It has been proved that optimum freeze-drying cycles are established by simultaneously taking into account the impact of formulation variables, especially the tert-butanol content, and classical freeze-drying variables during the freezing step (nucleation temperatures, freezing rates) and the sublimation step (shelf temperature, total pressure) to maximize the drying rates and to minimize the residual solvent levels while preserving the main quality attributes of the freeze-dried powder.     

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.     

3D Numerical Simulation of Thawing Frozen Wood Using Microwave Energy: Frequency Effect on the Applicability of the Beer–Lambert Law

In this article, the frequency effect on the applicability of Beer–Lambert's law for thawing frozen wood using the microwave energy was analyzed. To this end, we use Maxwell's equations to determine the absorbed power and characterize the critical slab thickness L _crit of three Canadian eastern wood species: trembling aspen (Populus tremuloides Michx), yellow birch (Betula alleghaniensis), and sugar maple (Acer saccharum). The critical thickness L _crit above which the Beer–Lambert law is valid is estimated as a hyperbolic function in the frequency domain: L _crit = m/f ⁿ (f is the frequency of microwave radiation; m and n are adjustment constants). The nonlinear heat conduction problem involving phase changes such as wood freezing is solved by a three-dimensional volumetric specific enthalpy-based finite element method. The dielectric and thermophysical properties are functions of temperature and moisture content. The specific volumetric enthalpy approach is validated by experimental testing. For instance, we studied the frequency effect on the thawing of frozen trembling aspen wood.     

Analysis of Heat and Mass Transfer during High-Temperature Drying of Pinus radiata

This article describes the analysis of heat and mass transfer coefficients for a single board of Pinus radiata (D. Don) timber over a range of high temperature and superheated steam drying conditions. The calculated heat transfer coefficients were in the range 20 to 60 W m^?2 K^?1. The mass transfer coefficients were of the order of 2 × 10^?8 to 3 × 10^?7 kg m^?2 s^?1, based on the vapor pressure difference, and of the order of 0.002 to 0.04 m s^?1 (expressed in terms of mass transfer velocity) based on vapor concentration difference between the surface of the board and the bulk drying medium.     

Drying behavior of prina (crude olive cake) using different types of dryers

The purpose of this research is to investigate the drying kinetics and determine the suitable drying method of prina, which is obtained after pressing of olives in olive oil factories, and which cannot be used efficiently in certain sectors. Drying experiments were performed at drying temperatures of 60°C, 70°C, and 80°C at a fixed air velocity of 2 m/s using a hot air dryer and with microwave powers of 90 W, 360 W, and 600 W using a microwave dryer. The prina layer thicknesses were selected as 7, 9, and 11 mm for both drying methods. The minimum energy consumption values were measured as 42.0 Wh for 600 W power level and 7 mm layer thickness, and 10260 Wh for 7 mm layer thickness and 80°C temperatures. It was found that energy consumption during hot air drying was more than that of microwave drying. As a result, the suitable dryer and thickness of layer were selected as microwave dryer and 7 mm, respectively. The results of statistical analyses showed that the most suitable model to define the drying behavior of prina samples were found to be the Page model for the microwave dryer and Wang &; Singh model for the hot air dryer. Also, penetration depth, the loss tangent value (tanδ), dielectric constant of material (?^?), and dielectric loss factor (?^??) of dried prina were calculated as 34.51 cm, 0.1059, 75.65, and 8.01, at 2450 MHz, respectively.     

具有初始孔隙的多孔物料冷冻干燥

实验研究了具有一定孔隙的非饱和多孔物料对液体物料冷冻干燥过程的影响。以甘露醇为主要溶质的待干料液采用“液氮制冰激凌法”制备非饱和物料进行冷冻干燥,并与常规饱和的冷冻物料相比较。结果表明,非饱和冷冻物料确实能够显著地强化液体物料的冷冻干燥过程。干燥产品SEM形貌分析显示,初始非饱和冷冻物料具有连续均匀的固体骨架和孔隙,固体基质更加纤细,孔隙空间更大,可以大大减小传质阻力。考察物料内部各点的温度变化发现,初始非饱和物料内部冰晶确实发生整体升华,但仍然存在主要升华区域;非饱和多孔物料的冷冻干燥过程主要是传热控制,而常规饱和物料冷冻干燥主要是传质控制。操作压力对过程的影响可以忽略。采用辐射/导热组合加热方式可改善初始非饱和多孔物料冷冻干燥过程的传热,进一步缩短干燥时间。     

A New Model and Quality of Unfrozen and Frozen Cooked Rice Dried in a Microwave Vibro-Fluidized Bed Dryer

This study aimed to develop a suitable drying model for microwave vibro-fluidized bed drying in a single-mode applicator (MVFB-SMA drying) of cooked rice with and without prefreezing treatment and to investigate the effects of prefreezing treatment and drying temperature (110–185°C) on quality of dried cooked rice. During the process of drying cooked rice from 60 to 10% (wet basis), results indicated that drying rate increased, whereas drying time decreased with prefreezing treatment and increased drying temperature. The drying rate and drying time of unfrozen and frozen cooked rice ranged from 0.196 to 0.497 g water/g dry matter/min and 0.228 to 0.554 g water/g dry matter/min; and from 7 to 2.5 min and 5.5 to 2 min, respectively. A new model was proposed in this study (MR = exp(?k t ⁿ ) + bt + c) to compare with 11 commonly used drying models. The new model describes the MVFB-SMA drying data most satisfactorily. The values of effective diffusivity were between 1.70 × 10^?7 and 5.72 × 10^?7 m²/s for the unfrozen sample and between 1.99 × 10^?7 and 5.86 × 10^?7 m²/s for the frozen sample. Their activation energy values were 23.66 and 21.19 kJ/mol, respectively. Prefreezing treatment provided a whiter product with a less uniform porous structure and higher bulk density. Slower ability to rehydrate was also observed for the frozen cooked rice dried at 160 and 185°C. An increase in drying temperature resulted in changes in whiteness, microstructure, bulk density, and rehydration capability. No prefreezing treatment and drying at 160°C seemed to be the optimal process condition for cooked rice, ensuring whiteness, a porous structure, low bulk density, and high rehydration capability.     

Simulation of Jet Drying of a Moist Cylinder at Low Reynolds Number

A numerical analysis of the process of jet drying of a moist cylinder was conducted. The drying jet was a laminar 2D jet stationed at three different distances (D/H = 0.22, 0.25, and 0.33) from the moist cylinder to investigate the jet effectiveness on heat and mass transfer. The diameter of the object and initial jet height were fixed in all cases. Temperature and mass distributions were obtained inside the object for different jet velocities. A finite volume method was used to solve the governing equations for momentum and energy with a commercial code. Calculations were performed for three different Reynolds numbers, namely, Re = 100, 200, and 300. It was found that heat and mass transfer increased with decreasing the distance, D/H, between the jet and the cylinder. In addition, increasing Reynolds number showed a positive effect on heat and mass transfer. Locally, jet drying was found to be most effective near the stagnation point on the leading side of the cylinder.     

Effect of Cryoprotectant and Freeze-Drying Process on the Stability of W/O/W Emulsions

In order to protect a hydrophilic drug and to prolong its further delivery, the formulation of multiple emulsions could be worthy. However, the double emulsions are not stable, their structure can change, leading to the formation of a single emulsion as the destruction of the system, and the drug can release easily from the globules in liquid state. The freeze-drying technology could be used to produce dry emulsion, the powder form being much more stable. The aim of this work was to study the influence of a cryoprotectant and a freeze-drying process on the stability of W/O/W emulsions. Samples were frozen at two different freezing rate (ν _f  = 0.55°C/min and 1.25°C/min) and successively dried at two different sublimation temperature (T _s  = ? 10°C and ? 20°C). The particle size distributions were measured by granulometer and UV spectrophotometer was performed to investigate the leakage of internal constituent. The glass transition temperature (T _g ) of the double emulsions was analyzed by DSC. The particle sizes became even smaller after freeze drying, except when κ-carrageenan is used as a cryoprotectant. In that case, the particles became aggregated after freeze drying, whatever the process conditions. The mean size is considerably reduced when the globules are diluted at low concentration in glucose and trehalose solution. When the concentration is increased, the size distribution is not significantly affected. The leakage of the internal aqueous phase to the external one during freeze drying was measured as an indicator of the structure stability. It is affected by the nature of the cryoprotectant and the conditions of the freeze-drying process. The leakage of the internal phase was smaller when cycle III (ν _f  = 1.25°C/min, T _s  = ? 10°C) was processed. From our experiments, we suppose that the water transfer from the inner phase to the outer aqueous phase results in the diminution of the globules size in double emulsion. The T _g of the double emulsions diluted with trehalose and glucose were determined at ? 33.8°C and ? 47.1°C. In contrast, the T _g of double emulsion with κ-carrageenan and HES did not appear.     

构建微波冷冻干燥质扩散系数的一种新方法

针对现有微波冷冻干燥模型中必须依靠实验以确定扩散系数的问题．提出一种构建扩散系的新方法。根据毛细管低压气体输运理论，利用物料本身的细微结构、气体分子平均自由程、气体状态参数和气体物性参数来构建扩散系数，在此基础上建立微波冷冻干燥模型。并结合牛肉的微波冷冻干燥行模型可靠性分析。结果表明，新建模型能够很好地描述微波冷冻干燥过程温度场的变化及其特征．升过程干燥曲线的理论值与实验值之间的相对误差小于10％。