Modeling of Vacuum Desorption in Freeze-Drying Process

Abstract

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.     

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。     

Studies on the Microwave Freeze Drying Technique and Sterilization Characteristics of Cabbage

The vacuum freeze-drying (FD) technique used in the food industry can yield a high-quality product, but it is very expensive and requires a long processing time. Besides, the quantity of microorganisms in FD products can often exceed the required standard. As a result, it will be important to develop a new freeze-drying technique. In this article, cabbage was used as a model material, and the microwave field was used as a heat source to supply sublimation heat so that the drying time was shortened greatly. The effect of the microwave sterilization during the drying process was evaluated. Effects of the pressure, thickness of material being dried, and the input microwave power on such indices as drying time and the microorganism number were studied. Compared with the method of ordinary freeze drying, microwave freeze drying (MFD) can greatly reduce the drying time and has a notable sterilization effect.     

Studies on the Microwave Freeze Drying Technique and Sterilization Characteristics of Cabbage

The vacuum freeze-drying (FD) technique used in the food industry can yield a high-quality product, but it is very expensive and requires a long processing time. Besides, the quantity of microorganisms in FD products can often exceed the required standard. As a result, it will be important to develop a new freeze-drying technique. In this article, cabbage was used as a model material, and the microwave field was used as a heat source to supply sublimation heat so that the drying time was shortened greatly. The effect of the microwave sterilization during the drying process was evaluated. Effects of the pressure, thickness of material being dried, and the input microwave power on such indices as drying time and the microorganism number were studied. Compared with the method of ordinary freeze drying, microwave freeze drying (MFD) can greatly reduce the drying time and has a notable sterilization effect.     

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.     

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。     

A MATHEMATICAL MODEL FOR THE CONTINUOUS VACUUM DRYING OF HIGHLY VISCOUS FOODSTUFFS

An improved mathematical model for the continuous vacuum drying of highly viscous and heat-sensitive food-stuffs was proposed. The process of continuous vacuum drying was presented as a moving boundary problem of moisture evaporation in cylindrical coordinates. Boundary condition of the first kind for the known functional dependence of the drying body surface temperature on time was considered. Finally, the appropriate system of differential equations was solved numerically and the values of drying rate, integral moisture content of the material, moving boundary position as well as temperature in any point of the material and at any moment of time were obtained. This procedure was applied to continuous vacuum drying of foods such as natural cheese and fresh fish meat paste.     

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.     

Drying Kinetics and Energy Consumption in Vacuum Drying Process with Microwave and Radiant Heating

The general objective of this work is to analyze energy input in a vacuum process with the incorporation of microwave heating. Thus, necessary criteria for designing an efficient freeze-drying operation are considered through the analysis of strategies based on the combination of different intensities of radiant and microwave heating. The other aim of this research topic is to study the kinetics of drying in relation to mass transfer parameters. Five freeze-drying strategies using both heating systems were used. Consequently, energy input could be related to diffusivity coefficients, temperature and pressure profiles during dehydration of the product and analyzed in comparison to a conventional freeze-drying process.     

微波及辐射真空干燥过程中的干燥动力学及能量消耗

The general objective of this work is to analyze energy input in a vacuum process with the incorporation of microwave heating. Thus, necessary criteria for designing an efficient freeze-drying operation are considered through the analysis of strategies based on the combination of different intensities of raxiiant and microwave heating.The other aim of this research topic is to study the kinetics of drying in relation to mass transfer parameters.Five freeze-drying strategies using both heating systems were used. Consequently, energy input could be related to diffusivity coefficients, temperature and pressure profiles during dehydration of the product and analyzed in comparison to a conventional freeze-drying process.     

黑加仑真空冷冻与微波真空联合干燥工艺研究

以黑加仑为原料,对其进行了真空冷冻与微波真空联合干燥工艺的研究。结果表明：先真空冷冻后微波真空干燥（FDMV）的组合方式是可行的;联合干燥合理工艺参数为：微波功率1．34kW。绝对压力11kPa,转换含水率为20％（wb）;通过试验验证,联合干燥生产的脱水黑加仑的感官品质和营养成分接近真空冷冻干燥,联合干燥方式对节省干燥时间和降低能耗是有效的。     

冷冻干燥过程强化中冷冻阶段优化的研究进展

冷冻干燥产品质量高,但时间长、能耗高。本文综述了冷冻干燥过程强化中冷冻阶段的优化方法,控制冷冻速率、调节冰晶成核和退火处理可以获得大而均匀的冰晶从而提高升华干燥阶段速率,但物料内部比表面积的减小会降低解吸干燥阶段速率,这类常规的冷冻阶段优化方法对弱吸湿性的物料有一定的强化效果。有机溶剂具有较高的蒸气压,作为共溶剂时可以增加传质推动力,但较低的有机溶剂残留量要求阻碍了其进一步应用。“初始非饱和多孔介质冷冻干燥”的技术思想是将液体物料首先制备成具有一定初始孔隙的冷冻物料,然后再进行冷冻干燥。物料具有的初始孔隙为水蒸气的迁移提供了便捷的通道,而且纤薄的固体基质也有利于结合水的解吸,可以同时强化升华干燥阶段和解吸干燥阶段。该技术思想是过程低消耗和产品高质量的完美结合,为解决冷冻干燥过程速率低的问题提供了新的方案。     

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。     

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.     

具有预制孔隙多孔介质冷冻干燥的多相传递模型

基于局部质量非平衡假设,建立了多相多孔介质热、质耦合传递数学模型,理论验证具有预制孔隙的初始非饱和多孔物料对冷冻干燥过程的强化作用。模型考虑了多孔介质的吸湿效应,构建了3种吸附-解吸平衡关系。模型使用基于有限元法的COMSOL Multiphysics软件平台数值求解,并与实验数据进行了比较。结果表明,初始非饱和冷冻物料能够有效地强化冷冻干燥过程。采用不同函数形式的吸附-解吸平衡关系模拟的干燥曲线均与实验数据非常吻合。通过分析物料内部的饱和度、温度和质量源分布,探讨了初始非饱和物料冷冻干燥过程的传热传质机理。初始非饱和物料的干燥速率控制因素主要是传热。模拟考察环境辐射温度对冷冻干燥过程影响的结果表明,所建模型具有良好的预测能力。     

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。     

升华干燥过程的(火用)损失分析

通过对物料在升华干燥过程中的Yong损失分析，建立了升华干燥过程的Yong损失分析模型。结合升华干燥动力学模型和Yong损失分析模型，以牛肉为冷冻干燥过程的模型物料，计算了物料表面加热温度、干燥室压力和物料厚度等操作条件的变化对升华干燥过程Yong损失的影响。计算结果表明：随着干燥室压力的增大，物料的Yong损失减小;随着物料表面加热温度的降低，Yong损失减小：随着物料厚度的减小，Yong损失逐渐减小；在冷冻干燥过程中，Yong损失主要集中在升华干燥阶段，在解析干燥阶段，物料表面加热温度的升高不会引起Yong损失的大幅度增加。     

固态食品常压吸附流化冷冻干燥的研究

至今为止,冷冻干燥技术得到应用的只有真空冷冻干燥一种,本文提出了常压吸附剂流化冷冻干燥,并具体阐述了数学模型和实验装置。通过与真空冷冻干燥进行比较,认为常压吸附流化冷冻干燥值得进一步深入研究,具有发展和应用前景。     

Strawberry drying: Development of a closed-cycle modified atmosphere drying system for food products and the performance evaluation of a case study

In the present study, a closed-cycle modified atmosphere drying (CC-MAD) system was developed as an alternative drying technique to facilitate drying processes for agricultural commodities appropriate to highly humid and sunny regions with a better quality. An absorption dehumidifying system was designed for working pseudo-continuously with the most efficient absorbent in terms of moisture absorption, desorption rate, and capacity. The system, assisted by a solar panel for absorbent regeneration, was tested, while its optimum working condition was determined by strawberry drying. This unique process was comparatively carried out using hot-air and freeze-drying techniques in terms of processing time and final product quality. Strawberry slices (5?mm thickness) were dried successfully using CC-MAD. The optimum drying conditions of CC-MAD were determined as drying temperature of 60°C, drying air/gas velocity of 3?m/s and drying medium oxygen level of 9.47%. The loss of ascorbic acid was significantly reduced by CC-MAD technique. These losses were found to be 2.9, 6.9, 27.2, and 23.8% by freeze-drying, CC-MAD, hot-air drying, and hot-air drying combined with CC-MAD, respectively. The total monomeric anthocyanins loss was also significantly reduced by the CC-MAD technique (20.3%), in a similar way to that of freeze-drying (18.1%) in comparison with hot-air drying (40.4%). In addition, CC-MAD (12,446?kJ/kg fresh product at 4?h drying time) is three times more advantageous in terms of energy cost compared with freeze-drying (30492.8?kJ/kg fresh product at 24?h drying time) and six times faster in terms of drying time. This new drying system can be used as an alternative to freeze-drying in the drying of foods, especially in products sensitive to oxidation.     

薄膜蒸发技术在低聚糖生产中的应用

目前低聚糖的干燥技术主要有喷雾干燥以及冷冻干燥,存在操作温度过高、成本较高、不能处理大批量物料等缺点。为了解决这些问题,本文提出了以刮膜式薄膜蒸发器对低聚糖提取液进行单步干燥操作。实验分析了设备的处理性能,并利用响应面法拟合得到了温度、压强、进料速度与单位面积蒸发速率之间关系的数据模型。模型可以很好地符合实际结果。在温度、压强、进料速度分别设定为70.0℃、1.0kPa、0.50L/h的条件下,最终得到的产物含水率为2.1%。这表明,工艺路线以及预测方法是可行的,工艺保证了物料较好的流动性,达到了较高的分离效率,得到了质量较高的最终产品。