基于露点法判断冻干过程的一次升华结束点

本文根据冻干过程干燥室内的露点值和物料的水分含量有关提出一种新的方法--露点法来监控冻干过程物料的水分迁移情况.以浓度为2%(W/V)的甘露醇(冻干保护剂)为研究对象,分别取80个,160个,20个小瓶,通过不同的过充小瓶数(1个,2个),不同的溶液高度(溶液高度6.5 mm,0.32 mm)来检验露点法在监测整批样品冻干过程的灵敏性.与称重法对照,称重法即在冻干过程不同的时刻取出样品测量整批样品质量.实验结果表明露点法即使当过充小瓶率为0.625%,或者溶液高度为0.32mm时仍有足够的灵敏度,露点法得到的一次升华结束点与称重法结果一致.这说明非接触法露点法是一种可靠,便利的监测一次升华结束点的方法,将其应用于控制成批冻干样品大有可为.     

冻干工艺中升华结束点和残余水分测量方法简述

升华结束点和残余水分的在线测定是冷冻干燥科学实验及其工艺中的重点和难点 ,着重对其常用确定方法理论模型法、产品温度响应法、压力升高法、湿度传感器法、残余气体分析仪、脉冲核磁共振法 (NMR)、称重法 (重量传感器法 )等 7种方法加以总结和概括。指出脉冲核磁共振法和湿度传感器法将为冻干理论研究和实验研究拓展新思路     

真空冷冻干燥机节能途径浅析

真空冷冻干燥机在运行时产生较高的能耗.本文在概述真空冷冻干燥技术的基本原理和干燥过程的基础上,分析了影响真空冷冻干燥速率的主要因素,提出有效降低真空冷冻干燥机能耗的途径为:改变物料的形态和浓度、控制预冻速度和物料厚度、采用联合冻干工艺和改进真空冷冻干燥机设计,旨在为真空冷冻干燥机在实际应用中节能降耗提供借鉴.     

Rarefied gas dynamics aspects of pharmaceutical freeze-drying

Freeze-drying is a low-pressure, low-temperature condensation pumping process widely used in manufacture of bio/pharmaceutical products. Because of the need to avoid the aggressive evaporation drying, typical operating pressures in freeze-drying are below 100 Pa. Understanding relevant rarefied flow physics can help improve freeze-drying systems and processes. The paper presents various rarefied gas dynamics aspects of freeze-drying including thermal creep and conduction, pressure and concentration-gradient driven flows and sonic expansion flows with icing. In particular, flow through the duct where the Knudsen number is small enough is modeled using conventional CFD techniques. The effect of the hardware on flow in the duct is discussed in detail. Furthermore, flow and icing in the freeze-drying condenser is modeled using the direct simulation Monte Carlo (DSMC) technique. The effect of duct length on the uniformity of mass flux and ice accretion rates are discussed. It is found that by increasing the duct length, there is a trade-off between increased residual pressure and improved uniformity. The simulations show that by augmenting the DSMC method with conventional CFD technique in appropriate regimes, the gas dynamics in the entire freeze-dryer system can be modeled numerically for given sublimation rate and geometry.     

干燥技术在催化剂制备中的应用

本文对干燥技术的机理、常用的干燥方式进行了简介，重点对喷雾干燥、冷冻干燥和超临界干燥等特殊干燥方法及其在催化剂合成中的应用进行了综述。探讨了不同干燥方法的优缺点及其在催化剂工业中的应用前景。     

变温变压的优化组合对扇贝真空冷冻干燥过程影响的实验研究

为了获得调压调温的优化组合对栉孔扇贝真空冷冻干燥过程的品质、能耗和时间的综合影响,在前期研究的基础上,本文对两次变温和一次变压的温度和压力组合参数进行了五因素四水平的正交组合试验,并以能耗、冻干时间和复水率等三指标的综合加权平分值为指标,得出了各温度和压力条件影响冻干能耗及品质的主次关系为:加热板高温2>干燥室低压>加热板高温1>加热板低温>干燥室高压,各因素的最佳组合是加热板高温1为42℃,高温2为30℃,干燥室低压为25Pa,加热板低温为25℃,干燥室高压为80 Pa,在这个优化组合工艺条件下,扇贝的复水率达到83.7%,与16组实验中的最佳相比,复水率提高了12.20%,能耗下降了2.17%,干燥时间缩短了20%。     

冻干机用捕水器结霜特性研究中存在的问题

真空冷冻干燥过程中，从物料中升华出来的水分在真空泵的抽吸作用下，不断地在捕水器（也即冷阱）表面结霜，随着霜在捕水器表面不断凝结，致使其捕水效率不断降低，对真空系统形成不利的影响。但目前，对于低温、低压下的结霜机理研究极少，本文介绍了国内外有关低温冷壁面结霜的研究现状，并分析研究了真空冷冻干燥系统中冷壁面结霜过程中存在的问题。     

Synthesis of W-Y_2O_3 alloys by freeze-drying and subsequent low temperature sintering:Microstructure refinement and second phase particles regulation

In this work,W-Y2 O3 alloys are prepared by freeze-drying and subsequent low temperature sintering.The average size of reduced W-Y2 O3 composite powders prepared by freeze-drying method is only 18.1 nm.After low temperature sintering of these composite nanopowders,the formed W-Y2 O3 alloys possess a smaller grain size of 510 nm while maintaining a comparatively higher density of 97.8%.Besides a few submicron Y2 O3 particles(about 100-300 nm)with a W-Y-O phase diffusion layer on their surface distribute at W grain boundaries,lots of nano Y2 WO6 particles(<20 nm)exist in W matrix.Moreover,many Y6 WO12(<10 nm)particles exist within submicron Y2 O3 particles.The formation of these ternary phases indicates that some oxygen impurities in the W matrix can be adsorbed by ternary phases,resulting in the purification of W matrix and the strengthening of phase boundaries.The combined action of the above factors makes the hardness of the sintered W-Y2 O3 alloys in our work as high as 656.6±39.0 HV0.2.Our work indicates that freeze-drying and subsequent low temperature sintering is a promising method for preparing high performance W-Y2 O3 alloys.     

甘露醇冷冻干燥室内真空压力特性的研究

冷冻干燥室的真空系统为冷冻干燥提供了真空环境,真空压力特性对冷冻干燥过程顺利进行至关重要,本文以甘露醇溶液的冷冻干燥过程为例,从三个方面对冷冻干燥室内真空压力特性进行了研究:一、真空度对冷冻干燥物料质量称量的影响;二、真空度对冷冻干燥物料瓶内温度的影响;三、真空度对冷冻干燥物料一次干燥速率的影响.通过实验,得出结论:真...     

食品真空冷冻干燥过程工艺参数分析

针对目前国内冻干食品企业制定食品冻干工艺和食品冻工设备设计需要,系统分析了食品真空冷冻干燥过程的主要工艺参数及其之间的关系; 为冻干食品企业制定食品冻干工艺及食品真空冷冻干燥设备工程设计确定技术参数提供参考。     

Physicochemical interaction mechanism between nanoparticles and tetrasaccharides (stachyose) during freeze-drying

Nanoparticle suspensions are thermodynamically unstable and subject to aggregation. Freeze-drying on addition of saccharides is a useful method for preventing aggregation. In the present study, tetrasaccharides (stachyose) was employed as an additive. In addition, we hypothesize the interactive mechanism between stachyose and the nanoparticles during freeze-drying for the first time. The mean particle size of the rehydrated freeze-dried stachyose-containing nanoparticles (104.7?nm) was similar to the initial particle size before freeze-drying (76.8?nm), indicating that the particle size had been maintained. The mean particle size of the rehydrated normal-dried stachyose-containing nanoparticles was 222.2?nm. The powder X-ray diffraction of the freeze-dried stachyose-containing nanoparticles revealed a halo pattern. The powder X-ray diffraction of the normally dried stachyose-containing nanoparticles produced mainly a halo pattern and a partial peak. These results suggest an interaction between the nanoparticles and stachyose, and that this relationship depends on whether the mixture is freeze-dried or dried normally. In the case of normal drying, although most molecules cannot move rapidly thereby settling irregularly, some stachyose molecules can arrange regularly leading to some degree of crystallization and potentially some aggregation. In contrast, during freeze-drying, the moisture sublimed, while the stachyose molecules and nanoparticles were immobilized in the ice. After sublimation, stachyose remained in the space occupied by water and played the role of a buffer material, thus preventing aggregation.     

快速铸造收缩-扩张形气膜孔空心涡轮叶片

本文将光固化成形技术和凝胶注模成形技术集成在一起,间接自由成形了带有收缩-扩张形气膜孔空心涡轮叶片整体式陶瓷铸型.通过建立收缩-扩张形气膜孔型芯干燥收缩受阻模型,推导了临界干燥收缩率计算公式,实验研究了凝胶注模成型坯体冻干特性.结果表明:冻干收缩率随着失水程度增加而增大,在失去约50%水分之后,干燥收缩停止;预冻温度越...     

低温真空干燥对胡萝卜品质的影响

以胡萝卜为对象,研究了低温真空干燥对胡萝卜的营养成分(如还原糖、维生素C等)及复水特性影响,并将低温真空干燥与真空冷冻干燥及热风干燥进行了对比。实验表明:经过热风干燥和真空冷冻干燥后胡萝卜的维生素C损失率分别是低温真空干燥的2.47倍和2.14倍。低温真空干燥可以较好的保持胡萝卜的组织结构完整性,并且减少营养物质的流失。     

Genipin-crosslinked gelatin scaffolds for articular cartilage tissue engineering with a novel crosslinking method

A novel crosslinking method with directly crosslinking the gelatin gel, being cut to a disc of chosen size beforehand, for the fabrication of porous gelatin scaffold was proposed. This novel method of gel-crosslinking was compared with the traditional methods of mixing-crosslinking and scaffold-crosslinking. The structure of the scaffold fabricated by the gel-crosslinking method shows uniformly distributed and interconnected pores which can be much smaller than those made by the other two methods. All three methods have the last step as freeze-drying; nevertheless, freeze-drying once more will increase the uniformity of the structure and the interconnecting pores. Crosslinking of gelatin was carried out at room temperature with glutaraldehyde (GTA) or genipin (GP). In vitro cell culture of Wistar rat's joint chondrocytes demonstrates that the GTA-crosslinked scaffold is much worse than the GP-crosslinked one; a tissue containing collagen and glycosaminoglycan was produced in the GP-crosslinked scaffold in just 9 days after cell seeding, and a tissue with a cell distribution resembling that of the native cartilage was developed after 30 day cell culture. It was concluded that the novel method is feasible for application in articular cartilage tissue engineering.     

Preparation and mechanical properties of dense polycrystalline hydroxyapatite through freeze-drying

High purity hydroxyapatite (HAp) powders were synthesized through the wet-chemical method and subsequent freeze-drying or heat-drying, respectively. Dense polycrystalline HAp ceramics were obtained by sintering the powder compacts in air in the temperature range 1100–1350°C. Results show that the freeze-drying method can produce highly homogeneous, fine-grained HAp powders. The relative density, Vickers hardness and flexural strength of the sintered freeze-dried HAp ceramics increased with the sintering temperature, reaching a maximum at around 1350°C, and the highest values obtained were 99.0%, 820 and 110 MPa, respectively. All these mechanical properties of the freeze-dried HAp ceramics are much higher than those of the conventionally heat-dried HAp ceramics. The drying method can significantly influence the properties of the HAp powders as well as the HAp ceramics.     

生物制药中的冷冻干燥技术

随着我国生物技术的迅速发展,冻干技术在生物制药行业的应用越来越广泛,本文介绍了冻干设备的结构及功能、冻干过程及冻干主要工序洁净要求及工艺流程方框图等,供参考.     

Preparation and characterization of an amine-modified graphene aerogel for enhanced carbon dioxide adsorption

Journal of Materials Science - A 3D porous graphene aerogel (GA) was prepared via one-step hydrothermal method and freeze-drying technology, in which organic amine reagents were used as...     

连用DCS与显微方法的冷冻干燥系统及实验研究

研制了一种真空冷冻干燥装置,并在其中引入了DSC热分析和显微观察的功能,利用此连用DSC与显微方法的冷冻干燥系统,对低温保护剂海藻糖(trehalose)和聚乙烯醇(PVA)的水溶液进行了冷冻干燥实验,主要考察冷冻速率和溶液用量等不同冷冻条件对溶液冻结特性和升华过程的影响,并通过冻干溶液多孔结构的显微照片估计溶液冻结后形成冰晶的情况.实验结果表明,加快冷冻速率会导致不完全冻结并形成大量的细小冰晶,增加样品用量同样会引起过冷度增大,导致冰晶尺寸减小,使升华阻力增大,升华速率减慢.     

二次蒸汽加热系统在真空冷冻干燥设备中的应用研究

为有效降低真空冷冻干燥设备运行能耗，在两套SZDG75型大型食品真空冷冻干燥设备上，分别采用了水作为载热流体的加热系统和二次蒸汽作为载热流体的加热系统，进行了冻干加工实际生产应用对比实验。实验结果表明，当进行小葱冻干加工时，在相同的实验条件下采用二次蒸汽加热系统的冻干设备的加工时间，比采用水加热系统的冻干设备缩短了1个小时，设备运行电耗降低11％，综合效果明显。     

High rate electrochemical performances of nanosized ZnO and carbon co-coated LiFePO4 cathode

The high rate electrochemical performances of ZnO and carbon co-coated LiFePO₄ have been studied by X-ray diffraction, high-resolution transmission electron microscope, electrochemical impedance spectroscopy, cyclic voltammetry and galvanostatic measurements. The carbon coated LiFePO₄ material was prepared by a freeze-drying method, and the diffusion coefficient and exchange current of these materials were calculated from their electrochemical impedance spectroscopy. The electrode delivered a reversible capacity of about 90% of the theoretical capacity when cycled between 2.5 and 4.2 V and showed stable cycle performance at high charge/discharge rates. This study showed that the co-coating process and freeze-drying method can effectively improve the electrochemical performances of LiFePO₄ materials.