超临界流体萃取筛板塔中二氧化碳/醇/水体系流体力学特性和传质性能的初步研究

在内径25mm的连续逆流超临界流体萃取筛板塔中,对超临界二氧化碳/乙醇/水和二氧化碳/异丙醇/水2种体系的流体力学特性和传质性能进行了实验研究;对实验数据进行了分析处理,得到了描述超临界流体萃取筛板塔流动特性的关联式,应用柱塞流模型对超临界流体萃取筛板塔的传质性能进行了模拟计算.     

超临界流体萃取塔的应用设计及理论研究

设计了超临界流体萃取塔系统，并对其流体力学特性和传质性能进行了研究，为工业设计提供了理论依据。在连续逆流操作的超临界填料萃取塔、筛板萃取塔和喷淋萃取塔中，应用超临界二氧化碳-异丙醇-水、超临界二氧化碳-乙醇-水两种实验体系对流体力学模型和传质模型进行了实验验证，计算结果与实验数据符合较好。     

超临界流体填料萃取塔流体力学和传质性能(Ⅱ) 传质性能

根据双膜理论,建立了超临界流体填料萃取塔液相总体积传质系数关联式;依据柱塞流模型,应用超临界二氧化碳-异丙醇-水和超临界二氧化碳-乙醇-水2种实验体系在内径为25mm的塔内对金属板波和金属丝网θ环2种填料的传质性能进行了模拟计算。结果表明,本文提出的传质数学模型能较好地描述超临界流体填料萃取塔的传质性能。     

超临界流体填料萃取塔流体力学和传质性能(Ⅰ) 流体力学数学模型

推导和建立了描述超临界流体填料萃取塔两相流体力学特性的数学模型。在25mm内径的连续逆流填料萃取塔中,应用超临界二氧化碳-异丙醇-水、超临界二氧化碳-乙醇-水2种实验体系和金属板波、金属丝网θ环2种填料对流体力学模型进行了实验验证,计算结果与实验数据符合较好。     

往复振动筛板塔对低界面张力体系萃取过程的强化

对低界面张力体系正丁醇-丁二酸-水在往复振动筛板塔中的萃取性能进行研究,体系中水为萃取剂,萃取正丁醇中的丁二酸。实验考察了两相流速、相比、传质方向和筛板振动速率对流体力学性能和传质性能的影响,并且与相同操作条件下固定筛板萃取塔的性能作对比。结果表明,筛板振动速率不高于3.5 cm/s的情况下体系没有发生乳化现象,相比增大到2.8时接近液泛点,实验稳定性较差。流速和相比增大能够获得更好的液滴分布和更大的体积传质系数,但增大的幅度要综合考虑设备的最大通量和两相在塔内的停留时间。分散相到连续相的传质方向传质相界面积大,更有利于提高传质效率。相同操作条件下,连续相中的轴向混合远大于分散相的轴向混合。与固定筛板塔的萃取性能相比,振动筛板改善液滴分布、增大处理能力和强化传质的作用都很明显。     

超声强化超临界流体萃取机理的研究

从实验和理论上对超声强化超临界流体萃取的机理进行了研究。采用自行设计的内插式超声强化超临界流体萃取装置,运用数码显微成像系统和透射电镜观察了有、无超声作用下超临界流体萃取中空化测试材料和海藻细胞微观结构的前后变化,分析了超声对超临界流体萃取海藻中二十碳五烯酸（EPA）和二十二碳六烯酸（DHA）的传质和萃取率的影响,并根据声化学原理对超临界流体中附加超声场时能否产生空化现象进行了探讨。实验结果发现超声对超临界二氧化碳流体中的空化材料和海藻细胞壁不产生破坏作用,不会产生声空化效应,但提高了海藻中EPA和DHA的萃取传质效果。其实验结果与理论推导相一致。结果表明：超声强化超临界流体萃取的机理不是源于超声空化,而是超声在微环境内产生的机械波动效应和热效应。     

超临界二氧化碳萃取技术

超临界流体萃取(Supercritical Fluid Extraction)技术是一种新型的化工分离技术.本文综述了超临界流体萃取技术的发展.超临界流体的特性,介绍了超临界二氧化碳萃取技术在中草药,食品工业,香料工业和环保技术方面的应用,并对超临界二氧化碳萃取技术的现状和前景进行了分析.     

轻重相交替进料筛板萃取塔中的传质性能研究

针对间歇操作萃取工艺生产能力低,而逆流连续操作萃取工艺返混严重等问题,研究提出了轻重相交替进料操作的萃取工艺,并对轻重相交替进料筛板萃取塔中的传质性能进行了研究。以煤油-苯甲酸-水为萃取体系,采用单个液滴的传质模型来计算萃取塔的分散相总传质系数,并研究了分散相流速、连续相流速、液滴上升速度以及塔板间距对分散相总传质系数的影响。实验得到分散相总传质系数Kod的数值在3.49?10?5~5.47?10?5 m?s?1,总分散相存留分数在1.63%~4.37%。结果表明轻重相交替进料筛板萃取塔的分散相总传质数高于Kühni搅拌萃取塔、脉冲萃取塔和振动挡板塔,并且流量变化对Kod的影响小,返混效应弱,总分散相存留分数小,不易液泛。     

超临界流体喷淋萃取塔流体力学特性和传质性能

在内径为25mm的连续逆流喷淋塔内进行了流体力学特性和质量传递性能的研究,实验压力为(8～14)MPa,实验温度为35℃,实验体系为CO_2/异丙醇/水和CO_2/乙醇/水.建立了描述连续逆流超临界流体喷淋萃取塔的流体力学关联式,根据双膜理论,建立了用于计算液相总体积传质系数的质量传递模型.流体力学关联式和质量传递模型的计算值与实验结果符合较好.     

超临界流体中的质量传递原理

本文较详细地论述了超临界流体中质量传递原理,介绍了物质在超临界流体中的传质系数、分子扩散系数的理论关联与实验测定,为超临界萃取传质过程的研究、超临界萃取装置的设计与放大提供参考。     

EVALUATION OF PACKED COLUMNS IN SUPERCRITICAL EXTRACTION PROCESSES

The purpose of the present work is to add to the base of knowledge in the use of packed columns when used in supercritical extraction service. Experimental studies were performed on a 2·54 cm diameter supercritical fluid extraction column operated in both spray and packed column arrangements. The packing used was 6· mm Raschig rings with a surface area of 722 m²/m³. The supercritical systems studied were carbon dioxide/ethanol/water and carbon dioxide/isopropanol/water at 102 atmospheres and 35^°C and 102 atmospheres and 40^°C, respectively. In order to compare supercritical with conventional extraction, similar data were obtained in the same column with the toluene/acetone/water system at one atmosphere and 24^°C.     

Performance of Spray,Sieve Tray,and Packed Contactors for High Pressure Extraction

Abstract

The performance of various contactors in high pressure extraction service was studied. The mass transfer efficiency of a spray column and columns filled with sieve trays, 1.27 cm ceramic Raschig rings, and no. 15 metal Intalox saddles were obtained from a “windowed” high pressure extraction column with an internal diameter of 9.88 cm and a column height of 168 cm. The extraction column has an internal diameter of 9.88 cm and a contacting height of 168 cm. Glass windows in the extractor allowed visual observation and photography. Supercritical and liquid carbon dioxide were used to extract isopropanol from water at pressures of 81 to 150 atmospheres and 297 to 318 [ddot]K. The sieve tray extractor yielded the highest mass transfer efficiency followed closely by Raschig rings and metal Intalox saddles. The spray column was by far the least efficient. The mass transfer efficiency was observed to be independent of the operating conditions studied in this work. Sauter mean drop diameters and dispersed phase (free) hold-up were also obtained in this work. These data will provide a reliable high pressure mass transfer and hydraulic database for future correlation and design efforts.     

Mass transfer in a countercurrent spray column at supercritical conditions

Mass transfer characteristics were determined for countercurrent extraction in a spray column with supercritical carbon dioxide solvent. Feeds were 5 and 10 vol% aqueous ethanol and iso-propanol at 25–65°C and 6.89–15.51 MPa. Results obtained in a 22 mm inside diameter column showed enhanced extraction efficiencies over comparable liquid-liquid systems. The models based on conventional liquid-liquid extraction were modified to correlate overall mass transfer coefficients for supercritical conditions. The constant value in the model of measuring individual mass transfer coefficient was influenced by the density of carbon dioxide and the system used.     

计算传质法预测精馏塔效率(英文)

A computational mass transfer model is proposed for predicting the concentration profile and Murphree efficiency of sieve tray distillation column. The proposed model is based on using modified two equations formulation for closing the differential turbulent mass transfer equation with improvement by considering the vapor injected from the sieve hole to be three dimensional. The predicted concentration distributions by using proposed model were checked by experimental work conducted on a sieve tray simulator of 1.2 meters in diameter for de-sorbing the dissolved oxygen in the feed water by blowing air. The model predictions were confirmed by the ex-perimental measurement. The validation of the proposed model was further tested by comparing the simulated re-sult with the performance of an industrial scale sieve tray distillation column reported by Kunesh et al. for the strip-ping of toluene from its water solution. The predicted outlet concentration of each tray and the Murphree tray effi-ciencies under different operating conditions were in agreement with the published data. The simulated turbulent mass transfer diffusivity on each tray was within the range of the experimental result in the same sieve column re-ported by Cai et al. In addition, the prediction of the influence of sieve tray structure on the tray efficiency by using the proposed model was demonstrated.     

Hydrodynamic and mass transfer performance of multiple upcomer extraction trays

The multiple upcomer (MU) extraction tray was specifically developed for aromatics extraction processes. Hydro-dynamic and mass transfer experiments have been carried out with n-butanol/succinic acid/water as an experimental system in a MU tray extraction column of 0.1 m diameter. The dispersed phase hold-up, drop size and overall efficiency were measured and the hydrodynamic and mass transfer parameters were correlated. The flooding velocities and the overall efficiency predicted from the correlation for this column agreed well with the experimental data.     

Supercritical fluid extraction from dried banana peel (Musa spp., genomic group AAB): Extraction yield, mathematical modeling, economical analysis and phase equilibria

Supercritical fluid extraction from dried banana peel (Musa spp., subgroup Prata, genomic group AAB, popularly known in Brazil as Enxerto) was studied. The aspects investigated were: overall extraction curve (OEC), mass transfer modeling of the yield curves, economical analysis of the process and phase equilibrium data for the pseudo-ternary system of banana peel extract, carbon dioxide and ethanol. The extraction operating conditions evaluated were: pressure ranging from 100 bar to 300 bar, temperature from 40 to 50 °C and constant solvent flow rate of 5.0 gCO₂/min. Experimental extraction data were correlated using three kinetic models based on mass transfer equations (logistic, diffusion and Esquível models). Phase equilibrium measurements were performed using pressure from 64.9 bar to 239.9 bar and mass fraction of supercritical extract from 0.52 to 3.55 wt%. Yield results ranged from 0.6 to 6.9% d.b. (dry basis). The lowest deviation between experimental and correlated data was obtained by the Logistic model, except for the curve at 300 bar and 40 °C which was best represented by the Esquível model. The economical analysis identified the possibility to apply the supercritical fluids to obtain extracts from banana peel in an industrial scale. Phase equilibrium for the supercritical extract from banana peel with carbon dioxide modified by ethanol exhibited liquid-liquid, vapor-liquid (bubble point) and vapor-liquid-liquid phase transitions. A crossover phenomenon for the systems evaluated was observed for pressures between 200 bar and 240 bar, for both groups of assays, i.e., supercritical extraction and phase equilibrium.