Toward Optimal Operation Conditions of Freeze-Drying Processes via a Multilevel Approach

Freeze drying (lyophilization) offers an attractive dehydration method for valuable food and biological products, because it is capable of preserving product quality and biological activity while extending their shelf life. However, despite these benefits in terms of product quality, freeze drying is also a notoriously energy-intensive and time-consuming process. This requires an expensive operation to construct an efficient optimal decision-making tool able to drive the operation through the most effective paths that minimize time and maximize product quality. Here we propose an integrated approach to operational design and control of the freeze-drying process that combines dynamic modeling with efficient optimized off-line and on-line control. The required mass and energy balance equations still contain inherent nonlinearity, even in their lumped parameter version. This results in a set of complex dynamic, computationally costly optimization problems solved by selected global stochastic optimization algorithms. Real-time disturbances and model uncertainties are addressed via the proposed hierarchical multilevel approach, allowing recalculation of the required control strategies. The framework developed has been revealed as a useful tool to systematically define off-line and on-line optimal operation policies for many food and biological processing units.     

水溶液的冷冻干燥问题(英文)

Freeze drying or lyophilization of aqueous solutions is widely used in pharmaceutical industry.The increased importance of the process is gaining a worldwide interest of research.A growing body of literature has demonstrated that the scientific approach can result in improved product quality with minimum trial and error empiricism.Formulation and process development need a systematical understanding of the physical chemistry of freezing and freeze drying,material science and mechanisms of heat and mass transfer.This paper presents an overview on freeze drying of aqueous solutions based on publications in the past few decades.The important issues of the process are analyzed.     

The drying strategy of atmospheric freeze drying apple cubes based on glass transition

Freeze drying (FD) yields the best quality of dried apple cubes but at the cost of long drying time and also the overall cost. To achieve economical freeze drying along with a high quality product an atmospheric freeze drying (AFD) technique was developed to dry apple cubes. The effect of different air temperature loading scheme on product quality and drying process was studied during AFD. According to the glass transition temperature of apple, a step-up temperature loading strategy for AFD process was developed to reduce the drying time by almost half and provided a similar good product quality.     

多孔纤维状物质的冷冻干燥模型

通过对草菇进行冷冻干燥实验,研究了过程中样品的中心温度及水分率随时间的变化关系．对冻干过程中物料干燥层和冰冻层进行质量和热量衡算,建立了升华─吸附─解吸数学模型．实验值与模型计算值吻合良好．     

液体物料冷冻干燥的热点问题

液体物料冷冻干燥广泛应用于制药工业。其过程工艺的重要性正赢得世界范围的研究关注。文献已证实科学方法能够用最少的试差来提高产品质量。过程工艺的建立和规划需要系统地理解冷冻、冷冻干燥、材料科学和质热传递等物理化学过程。本文就液体物料冷冻干燥过程做了简要评述,并对其过程的热点问题做了分析。     

Untersuchungen zur Steigerung der Trocknungsgeschwindigkeit der Gefriertrocknung

Freeze‐drying offers the advantage of mild drying. However, a drawback is the long drying time. One way to reduce the drying time is to use dynamic freeze‐drying. Here, the heat transfer to the product is improved and the forming dry layer is permanently removed. Thus, the heat and mass transfer resistance is reduced and it is dried in the vicinity of the ice crystals. This results in an increase of the drying rate, since it can be dried in the first drying section.     

Atmospheric Freeze Drying—Modeling and Simulation of a Tunnel Dryer

Drying is an important unit operation in processing of foods and other biotechnological products. Vacuum freeze drying is said to be the best drying technology regarding product quality of the end product, but the disadvantages are, among others, expensive operational costs and batch drying. Atmospheric freeze drying was introduced to lower the production costs of high-quality dried foods, and the need of simulation tools became important in estimations of the industrial drying processes.

A simplified mathematical model (AFDsim) is developed based on uniformly retreating ice front (URIF) considerations. The model is used to calculate theoretical drying curves of atmospheric freeze dried foods in a tunnel dryer. Studies of thermal and mass transfer properties during drying are essential for understanding the changes in product quality and for designing and dimensioning the drying process. The model can be used to simulate industrial atmospheric freeze drying of different foodstuff in a tunnel. The results from AFDsim modeling are in good accordance with the experimental results.     

Atmospheric Freeze Drying—Modeling and Simulation of a Tunnel Dryer

Drying is an important unit operation in processing of foods and other biotechnological products. Vacuum freeze drying is said to be the best drying technology regarding product quality of the end product, but the disadvantages are, among others, expensive operational costs and batch drying. Atmospheric freeze drying was introduced to lower the production costs of high-quality dried foods, and the need of simulation tools became important in estimations of the industrial drying processes.

A simplified mathematical model (AFDsim) is developed based on uniformly retreating ice front (URIF) considerations. The model is used to calculate theoretical drying curves of atmospheric freeze dried foods in a tunnel dryer. Studies of thermal and mass transfer properties during drying are essential for understanding the changes in product quality and for designing and dimensioning the drying process. The model can be used to simulate industrial atmospheric freeze drying of different foodstuff in a tunnel. The results from AFDsim modeling are in good accordance with the experimental results.     

Controlled freezing and freeze drying: a versatile route for porous and micro‐/nano‐structured materials

Freeze drying is a process whereby solutions are frozen in a cold bath and then the frozen solvents are removed via sublimation under vacuum, leading to formation of porous structures. Pore size, pore volume and pore morphology are dependent on variables such as freeze temperature, solution concentration, nature of solvent and solute, and the control of the freeze direction. Aqueous solutions, organic solutions, colloidal suspensions, and supercritical CO₂ solutions have been investigated to produce a wide range of porous and particulate structures. Emulsions have recently been employed in the freeze drying process, which can exert a systematic control on pore morphology and pore volume and can also lead to the preparation of organic micro‐ and nano‐particles. Spray freezing and directional freezing have been developed to form porous particles and aligned porous materials. This review describes the principles, latest progress and applications of materials prepared by controlled freezing and freeze drying. First of all the basics of freeze drying and the theory of freezing are discussed. Then the materials fabricated by controlled freezing and freeze drying are reviewed based on their morphologies: porous structures, microwires and nanowires, and microparticles and nanoparticles. The review concludes with new developments in this area and a brief look into the future. Copyright © 2010 Society of Chemical Industry     

Optimal control of a freeze dryer—I Theoretical development and quasi steady state analysis

A mathematical model which describes the nonsteady state heat and mass transfer operations during the freeze drying process is presented. With the use of this model the problem of operating a freeze dryer to obtain a fixed final moisture content in minimum time is formulated as an optimal control problem. Radiator energy output and total pressure in the drying chamber are considered control variables. Constraints are placed on the system state variables by the scorch point of the dried product and the melting point of the frozen interface. A quasi steady state analysis is performed which provides general guidelines about the optimal control policy at the beginning of the drying process (when neither of the state constraints is active), as well as during operation when the process may be heat and/or mass transfer limited.     

The Effect of Glass Transition Temperature on the Procedure of Microwave–Freeze Drying of Mushrooms (Agaricus bisporus)

Freeze drying (FD) yields the best quality of dried mushroom but at the cost of a long drying time and high overall cost. Air drying (AD) gives an unacceptably poor quality product. To achieve faster drying along with a high-quality product, a microwave–freeze drying (MFD) technique was developed to dry mushrooms. The relationship between dried mushroom quality and the glass transition temperature during the MFD process was studied to optimize the MFD process. According to the change tendency of the glass transition temperature of mushroom during MFD, a step-down microwave loading scheme for the MFD process was developed to obtain good product quality.     

An effective rate approach to modeling single‐stage spray drying

An effective rate approach (ERA) is proposed to achieve a fast and reliable prediction of dryer outlet conditions for a given single‐stage spray drying system operated under a range of scenarios. This approach is improved from existing methods based on simple mass and energy balances due to the incorporation of a reliable drying rate model, which is the reaction engineering approach for the material of interest. It allows quick solution procedure without the need to solve the partial differential equations that govern the heat and mass transfer in the spray drying process. By following a generic procedure, this technique has been exercised on the experimental results from running a monodisperse droplet spray dryer, that is, a well‐established experimental platform for model validation. The proposed ERA has been shown to be rather promising. It could become a powerful approach for proactive control and optimization for existing spray drying facilities. © 2015 American Institute of Chemical Engineers AIChE J, 61: 4140–4151, 2015     

Separation of CNF agglomerates from a ceramic suspension by spray drying technique

Aqueous silicon nitride based composite suspensions with the addition of 3.1 wt% of carbon nano-fibers (CNFs) were dried using two different drying techniques: spray drying and freeze drying. The paper deals with optimisation of parameters of the spray drying processwith the aim of maximising the yield and improve the quality of the granulate. Freeze drying was selected as a reference drying method, because no powder separation can occur in the course of the process. Prepared suspensions were spray dried at 4 different temperatures: 80, 110, 140 and 180 °C. After each run, two types of granules were obtained: from the separation flask and from the product vessel. Thermo-gravimetric analysis together with SEM examination show that spray drying results in separation of CNFs agglomerates. The granules from separation flask are always enriched by CNFs agglomerates whilst the granules from product vessel have reduced content of CNFs agglomerates. Sintering of spray-dried granules from the product vessel resulted in the composite with uniform microstructure, low amount of CNFs agglomerates and high relative density.     

Experimental Investigation of the Recovery of Soaked Paper Using Evaporative Freeze Drying

The aim of this article is to develop an experiment and a procedure to investigate the restoration of water-damaged paper and archival materials using freeze drying in order to allow a reproducible test and comparison of the influence of different operating conditions on drying time and restored paper quality. Firstly, a reproducible method for the preparation of soaked samples simulating water-damaged paper has been developed. Then, the samples have been freeze-dried in a laboratory-scale apparatus that allowed monitoring the temperature as well as the weight of the samples. The technique of evaporative freezing, which reduces the drying time required, has been used in this case. An innovative procedure for the visualization of the progress of the drying process has been validated, thus allowing the validation of a simple phenomenological model of the time evolution of the ice core volume; in addition, data on the residual moisture of the dried paper sheets in different zones have been given. Finally, optimization of this particular drying process by using simple or more sophisticated approaches has been discussed.     

草菇,菠萝的冷冻干燥过程及影响因素分析

从草菇、菠萝做冷冻干燥试验所得的冻干曲线和冻干时间,用分子运动论的观点分析了温度、压力等因素对冷干燥过程的影响。     

Effect of Drying and Dewatering on Yttria Precursors with Transient Morphology

The influence of drying and dewatering of a yttrium hydroxynitrate precursor with transient morphology was investigated. The ability of this precursor to form soft agglomerated nanoparticles after calcination is dependent on the dewatering method. Freeze drying leads to finer particles than other dewatering methods that involve removal of the solvent from its liquid state. As water is directly removed by sublimation during freeze drying, this method inhibits the formation of solid bridges between hydroxynitrate platelets. These bridges, which form with the other dewatering methods, destabilize the spheroidization process of the platelets during subsequent firing at high temperatures.     

食品冷冻干燥过程的模型及影响因素

在合理简化的基础上,得到了只需较少参数的冷冻干燥过程一维数学模型。通过对胡萝卜和土豆食品的冷冻干燥实验,研究了加热方式、加热搁板温度和干燥室真空度对干燥时间的影响,模型的数值解与实验值吻合良好。     

PRODUCT QUALITY MULTI-OBJECTIVE DRYER DESIGN

Design of conveyor-belt dryers constitutes a mathematical programming problem involving the evaluation of appropriate structural and operational process variables so that total annual plant cost involved is optimized. The increasing need for dehydrated products of the highest quality, imposes the development of new criteria that, together with cost, determine the design rules for drying processes. Quality of dehydrated products is a complex resultant of properties characterizing the final products, where the most important one is color. Color is determined as a three-parameter resultant, whose values for products undergone drying should deviate from the corresponding ones of natural products, as little as possible. In this case, product quality dryer design is a complex multi-objective optimization problem, involving the color deviation vector as an objective function and as constraints the ones deriving from the process mathematical model. The mathematical model of the dryer was developed and the fundamental color deterioration laws were determined for the drying process. Non-preference multi-criteria optimization methods were used and the Pareto-optimal set of efficient solutions was evaluated. An example covering the drying of sliced potato was included to demonstrate the performance of the design procedure, as well as the effectiveness of the proposed approach.     

EXERGY ANALYSIS FOR THE FREEZING STAGE OF THE FREEZE DRYING PROCESS

The mathematical expressions for exergy and the exergy analysis of the freezing stage of the freeze drying process are presented. The exergy analysis indicates that very substantial reductions in the magnitudes of the total exergy loss and of the exergy input due to the heat that must be removed during the freezing stage, can be obtained when the freezing stage is operated through the use of a rational distribution in the magnitude of the temperature of the cooling source. The rational distribution in the magnitude of the temperature of the cooling source should provide significant savings in the utilization of energy during the freezing stage of the freeze drying process as well as satisfactory freezing rates that form ice crystals that are continuous and highly connected and their shape and size are such that the pores of the porous matrix of the dried layer generated by sublimation during the primary drying stage, have a pore size distribution, pore shape, and pore connectivity that are appropriate to allow high rates for mass and heat transfer during the primary and secondary drying stages of the lyophilization process.