结合水对冷冻干燥过程影响的研究

本文通过分析三种结合水去除机理下的数学模拟结果，并辅以一定的实验验证进行了结合水对冷冻干燥过程影响的研究。以脱脂牛奶的瓶装冻干为对象，对残余水含量、物料温度、干燥时间、湿含量分布等参数，进行了比较和分析。结果表明，结合水对冷冻干燥过程有重大影响；结合水在升华阶段的解吸过程不能忽略，这一冻干机理对冻干时间与物料干燥层的湿含量分布的预测，以及对冷冻干燥过程的现象描述与规律阐述都极为重要。     

瓶装物料的冷冻干燥过程模拟与实验验证

对于瓶装物料的冷冻干燥，在前面工作＾「１」的基础上，以脱脂牛奶为物料对冻干过程进行实验研究和模拟计算，结果表明物料的温度分布近瓶壁处的温度较中心部分为高，因此说明瓶壁的热传导不可忽略：同时对模拟值与实验值进行比较，其结果吻合良好。     

梅州金柚柚子皮的真空冷冻干燥工艺研究

目的以梅州金柚柚子皮为原料,研究柚皮真空冷冻干燥工艺技术,确定最佳工艺参数和加工工艺,为柚皮综合利用提供参考依据。方法通过单因素实验和正交实验设计,以冻干速率作为考察指标,研究了压力(真空度)、加热温度、物料厚度对真空冷冻干燥速率的影响。结果实验表明,对冻干柚皮干燥速率的影响主次顺序为加热温度、压力(真空度)、物料厚度,最佳工艺条件分别为:加热温度50℃、压力(真空度)40 Pa、物料厚度5 mm,在此干燥工艺条件下,产品在色泽等方面保持较好。结论该正交试验筛选出的工艺稳定可行。     

药品真空冷冻干燥过程监控技术研究进展

对药品冻干过程进行优化的关键是在保证药品质量不受损害的情况下尽量缩短干燥时间。因此,对冻干过程进行准确的监控是十分重要的,既要保证药品的温度保持在合理的范围内,对干燥结束时间进行准确地判断,同时又要对冻干过程压力和温度进行良好的控制以达到冻干过程的最优化。本文对近年来药品真空冷冻干燥过程监控技术的研究进展进行了综述,主要有基于动态参数估计法(DPE)的监控系统、基于卡尔曼滤波法的监测系统、露点法判断一次干燥结束点、模型预测控制法(MPC)。提出药品真空冷冻干燥监控技术的研究应着重于以下几点:考虑辐射、对流和导热3种传热方式在冻干传热过程中所占的比重,建立二维、三维冻干模型以更加精确地监测药品冻干过程的参数,在此基础上研究对加热隔板温度和冻干室压力的实时最优控制策略,以对药品冻干过程进行及时、有效地控制。     

瓶装物料的冷冻干燥二维模型的建立与求解

本文对瓶装物料的冻干建立了一个考虑因素较为全面的二维数学模，该模型了侧面传热、结合水解吸和水蒸气温升对冻干过程的影响。根据冻干过程和模型方程的特点，本文把二循环对称分裂格式、预测－校正格式等算法联立起来对模型进行了数值求解，这些工作比目前的“只建模，不求解”或“虽求解，但模型简单、适用范围窄”的研究进行了一步。     

冻干技术及其在药品生产中的应用

对冻干技术的工作原理进行介绍 ,详细分析在初级干燥阶段和辅助干燥阶段物料的干燥过程及特性 ,物料温度在冻干过程中的变化及其参考性 ,以及影响冻干产品质量的若干问题和相应的解决措施     

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。     

微波辐射在木质纤维原料热化学加工中的应用

<正>木质纤维原料热化学加工包括木质原料的干燥、炭化、干馏、气化、活性炭制造、松根干馏、桦皮干馏等。不论进行哪种热化学加工均离不开加热能源,其中尤以活性炭制造要求更高。 传统的加热方式有电加热、水蒸气加热和烟道气加热等,它们是根据热传导、对流和辐射原理使热量从外部传至物料内部,加热速度慢,受热不均,且能耗高。微波加热技术与传统加热技术不同,它是通过被加热体内部偶极分子高频往复运动,产生“内摩擦热”而使被加热物料温度升高,不需任何热传导过程,就能使物料内外部同时加热、同时升温,加热速度快而均匀,仅需传统加热方式的几分之一或几十分之一时间就可达到加热目的。近20年来微波辐射研究取得了迅速发展,涉及的领域也相当广泛。但利用微波辐射技术取代传统加热方式应用于木质纤维原料热化学加工方面却报道极少。     

径向热质传递对瓶装物料冷冻干燥的影响

基于经验证了的二维冻干模型对瓶装物料的冷冻干燥过程进行了数值计算 ,利用计算结果对径向热质传递的影响进行了分析 .结果表明 :瓶侧面的径向传热影响显著 ,但忽略水蒸气在径向上的传递作用不会给模拟计算结果带来明显误差 .     

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。     

Heating Policies during the Primary and Secondary Drying Stages of the Lyophilization Process in Vials: Effects of the Arrangement of Vials in Clusters of Square and Hexagonal Arrays on Trays

The dynamic behavior of the primary and secondary drying stages of the lyophilization process were studied when (a) single vials located at different positions on the tray were individually being dried, and (b) the vials on the tray are arranged in clusters of square and hexagonal arrays and all the vials on the tray are simultaneously being dried. For both cases (a) and (b), fast drying times and relatively more uniform distributions of temperature and concentration of bound water at the end of the secondary drying stage are obtained by heat input control that runs the lyophilization process close to the melting and scorch temperature constraints. The heating control policies for the systems of case (b) are found to be more conservative and significantly more complex than those for the systems of case (a), because in case (b) there are vials on the tray that are in their secondary drying stage while other vials on the same tray have not yet completed their primary drying stage. Furthermore, the analysis and synthesis of the results presented in this work (i) indicate the minimum number of vials and their relative locations on the tray that have to be monitored by sensors so that the dynamic drying state of all the vials being dried simultaneously on the tray, could be satisfactorily determined in real time and appropriate, if necessary, control action could be applied, and (ii) suggest changes in the design of the freeze drying equipment so that the production rate of the freeze dryer could be improved and the product could also have enhanced properties of stability and quality at the end of the lyophilization process.     

Heating Policies during the Primary and Secondary Drying Stages of the Lyophilization Process in Vials: Effects of the Arrangement of Vials in Clusters of Square and Hexagonal Arrays on Trays

Abstract

The dynamic behavior of the primary and secondary drying stages of the lyophilization process were studied when (a) single vials located at different positions on the tray were individually being dried, and (b) the vials on the tray are arranged in clusters of square and hexagonal arrays and all the vials on the tray are simultaneously being dried. For both cases (a) and (b), fast drying times and relatively more uniform distributions of temperature and concentration of bound water at the end of the secondary drying stage are obtained by heat input control that runs the lyophilization process close to the melting and scorch temperature constraints. The heating control policies for the systems of case (b) are found to be more conservative and significantly more complex than those for the systems of case (a), because in case (b) there are vials on the tray that are in their secondary drying stage while other vials on the same tray have not yet completed their primary drying stage. Furthermore, the analysis and synthesis of the results presented in this work (i) indicate the minimum number of vials and their relative locations on the tray that have to be monitored by sensors so that the dynamic drying state of all the vials being dried simultaneously on the tray, could be satisfactorily determined in real time and appropriate, if necessary, control action could be applied, and (ii) suggest changes in the design of the freeze drying equipment so that the production rate of the freeze dryer could be improved and the product could also have enhanced properties of stability and quality at the end of the lyophilization process.     

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

Abstract:

The problem of operating freeze drying of pharmaceutical products in vials loaded on trays of freeze dryer to obtain a desired final bound water content in minimum time is formulated as an optimal control problem. Two different types of freeze dryer designs were considered. In the type I freeze dryer design, upper and lower plate temperatures were controlled together, while in the 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. Only the scorch temperature was considered as a constraint on the system state variables during the secondary drying stage, because all the free water content (frozen water) is removed from the solid matrix during the primary drying stage of freeze drying. Necessary conditions of optimality for the secondary drying stage of freeze drying process in vials were derived and presented by using rigorous multidimensional unsteady-state mathematical models. The theoretical approach presented in this work was applied in the freeze drying of skim milk. Significant reductions in drying times of the secondary drying stage of the freeze drying process in vials were observed and more uniform bound water and temperature distributions in the material being dried were obtained compared to the conventional operational policies.     

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

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.     

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.     

SIMULATION AND DESIGN OF BEATING PROFILES IN HEAT CONTROLLED FREEZE-DRYING OF PHARMACEUTICALS IN VIALS BY THE APPLICATION OF A SUBLIMATION CYLINDRICAL MODEL

A finite element method (FEM) with axial symmetry conditions and isoparametric elements has been applied to describe the freeze drying of a certain pharmaceutical contained in vials in industrial like conditions. Several operating strategies vere proved on the basis of considering three different stages during freeze-drying in relation with the modification of heating and product temperature evolutions. The model offers interesting perspectives to find the most adequate combination of operating conditions in order to reduce drying time.     

Some Aspects of Freeze Drying of Dairy Biomaterials

ABSTRACT

Different theoretical and experimental aspects of freeze drying of dairy biomaterials are reported. The following dairy biomaterials were chosen for investigations: three kefir bacterial cultures and one bacterial concentrate of a dairy vaccine. Experiments were performed both at one-region conductive or radiative heating and at combined two-region conductive-radiative heating. Emphasis was put on quality interactions between physical and biological properties of the material to be dried and freeze drying process parameters. Qualitative estimations of the following properties of biomaterials: a) colour, b)suppleness to caking and c) suppleness to scraping born the hot surface in dependence with the process parameters were performed using four-step subjective scales. On the basis of this estimations a synthetic quality criterion SQC was defined whose numerical value reflects general product quality. The results of mathematical modelling, numerical solution of the model and comparison with experimental data indicated that the process was heat transfer controlled and that the main factors resulting in good product quality and high SQC are low temperature of the conductive heated surface and vacuum chamber pressure affecting sublimation temperature. The influence of the sample freezing parameters on the elimination of the foaming or puffing and on the product quality was observed and examined. Furthermore, preliminary measurements of the dauy biomaterials viability after freeze drying were presented.     

EFFECTS OF HEATING METHODS ON VACUUM FREEZE DRYING

The heat and mass transfer during freeze drying of raw beef by different heating methods is studied theoretically and experimentally. The difference between radiant heating and microwave heating in freeze drying process has been analyzed. The results obtained are important for the selection of the heating methods in practical freeze dryers.     

冷冻干燥法制备层状多孔羟基磷灰石支架过程中的溶剂升华行为

采用水基羟基磷灰石(hydroxyapatite,HA)浆料,经冷冻干燥和烧结工艺(1 250℃烧结3 h)制备了层状多孔HA支架.研究了冷冻温度、干燥压力和干燥温度对水基HA浆料中溶剂升华行为的影响.结果表明:随着冷冻温度的降低,多孔HA支架的层间距逐渐减小,支架的升华时间增加;由于样品的干燥过程同时受到传热和传质的...     

EFFECTS OF HEATING METHODS ON VACUUM FREEZE DRYING

ABSTRACT

The heat and mass transfer during freeze drying of raw beef by different heating methods is studied theoretically and experimentally. The difference between radiant heating and microwave heating in freeze drying process has been analyzed. The results obtained are important for the selection of the heating methods in practical freeze dryers.