偏心转盘塔萃取净化湿法磷酸的研究

探讨了偏心转盘塔用于蒸馏水/湿法磷酸/磷酸三丁酯（TBP）和航空煤油实验体系的萃取特性,研究了转盘雷诺数、停留时间、相比等因素对萃取和反萃取的影响。结果表明：在优化的操作条件下,偏心转盘塔具有较高的萃取效率。萃取的最佳操作条件：当相比为4、停留时间为30 min、转盘雷诺数约为2 300时,磷萃取率可达53.77%;反萃取的最佳操作条件：当相比为6、停留时间为25 min、转盘雷诺数约为6 500时,磷反萃率可达到90.66%。     

The interaction of solute transfer,contaminants and drop break-up in rotating disc contactors: Part I. Correlation of drop breakage probabilities

The breakage process of single drops in RDC liquid-liquid extraction columns has been investigated. The breakage probability and daughter drop size distribution were the measured characteristics. Binary systems, non-equilibrated ternary systems with mass transfer in both directions (c → d and d → c) and systems with surface active agent added were used in the experiments. A model of the breakage probability was developed based on a modified Weber number, taking into account the applied shearing stress and the resisting interfacial tension force. It is shown that breakage probability can be estimated if interfacial tension is known as a function of interfacial conditions.     

Hydrodynamic and mass transfer parameter correlations for the rotating disc contactor

The normal, fragmented manner in which various model hydrodynamic and mass transfer parameters are measured and correlated separately, in the vain hope that accurate predictions of extraction column performance will be eventually possible, is avoided here. The ‘forward mixing’ model parameters are all determined simultaneously, in experiments with two sizes of rotating disc contactor where all required measurements, including drop size distributions and continuous phase profile compositions, are made during solute transfer between phases. Accurate predictions from the derived correlations of dispersed phase hold-up fraction, drop size distributions and extraction efficiency are the result.     

Prediction of axial mixing coefficients in rotating disc and asymmetric rotating disc extraction columns

The correlation of axial mixing in the continuous and dispersed phases of rotating disc and asymmetric rotating disc columns is presented. Published experimental results on continuous-phase axial mixing for both single- and two-phase flows, obtained with tracer injection methods and by solute concentration profiles, are considered. The correlation developed is based on 1055 data points for 32 liquid systems obtained by 19 different investigators. The axial mixing in rotating disc columns is found to be up to 20% larger than in asymmetric rotating disc columns. Data for the dispersed phase are harder to correlate than those for the continuous phase. Since the available results are often contradictory, the correlation for the dispersed-phase coefficient is thus less accurate than that for the continuousphase coefficient.     

The Interaction of solute transfer,contaminants and dro break-up in rotating disc contactors: Part II. The coupling of the mass transfer and breakage processes via interfacial tension

In order to investigate the influence of solute transfer and of surface active agents on the drop breakage process in liquih liquid extraction columns, their effect on the interfacial tension has to be studied in detail. The difficulty encountered is that the interfacial tension during solute transfer continuously changes and that no simple apparatus is commercially available which can measure these varying interfacial tension values. An attempt has been made here to theoretically predict them. The equations developed to predict the interfacial tension variation can be combined with a model for the breakage process and hence drop size distributions can be calculated from stage to stage. Applying a new combined film mass transfer coefficient model which takes into account the effect of contaminants, single drop extraction performance has been calculated for simplified conditions of constant bulk concentration in the continuous phase. Calculated efficiencies have been compared with experimental data and a good simulation of contaminant effects and dependency on drop size has been found. The calculations were restricted to low dispersed phase hold-up values, so that coalescence effects could be ignored. This work provides the required support for a procedure to be applied to counter-current flow extraction columns.     

Dispersed-phase holdup and mass transfer in a rotating disc contactor with perforated skirts

Dispersed-phase holdup and extraction efficiency were measured in a pilot-plant scale rotating disc contactor (RDC) with perforated skirts (RDCS) with kerosene-o-cresol-water system. The data for the RDCS were examined using the data in this work and the available correlations proposed for the plain RDC. A comparison between the data measured in the RDCS and those in the RDC indicated that the RDCS has rather better extraction efficiency compared with the RDC.     

Use of axial dispersion model for determination of Sherwood number and mass transfer coefficients in a perforated rotating disc contactor

The mass transfer process in a perforated rotating disk contactor (PRDC) using a toluene-acetone-water system was investigated.The volumetric overall mass transfer coefficients are calculated in a PRDC column.Both mass transfer directions are considered in experiments.The influences of operating variables containing agitation rate,dispersed and continuous phase flow rates and mass transfer in the extraction column are studied.According to obtained results,mass transfer is significantly dependent on agitation rate,while the dispersed and continuous phase flow rates have a minor effect on mass transfer in the extraction column.Furthermore,a novel empirical correlation is developed for prediction of overall continuous phase Sherwood number based on dispersed phase holdup,Reynolds number and mass transfer direction.There has been great agreement between experimental data and predicted values using a proposed correlation for all operating conditions.     

Liquid—liquid extraction column (rotating disc contactor)—model parameters from drop size distribution and solute concentration measurements

The practical application of an extraction column model which takes into account the influence of drop-size distribution (i.e. the ‘forward mixing’ model) is brought forward by the generation, from experimental data, of values of the mass transfer and axial dispersion coefficients required by the model. Values of these coefficients were generated from drop-size distribution and solute concentration profile measurements in a 22 cm diam. rotating disc contactor. The use of the Handlos-Baron drop mass transfer model is justified. The resulting continuous phase transfer coefficients were found to be dependent only on disc speed. Continuous phase axial dispersion coefficients were much higher than tracer-correlation predicted values at higher flows, and larger drop sizes. An explanation for this is presented.     

Hydrodynamics of a vibrating perforated plate extraction column

Hydrodynamic behaviour of several liquid-liquid systems has been measured in a 5 cm diameter extraction column agitated by finely perforated plates vibrating at frequencies (f) 10–100 Hz and amplitudes (a) 0.024–1.5 mm. The Sauter mean droplet diameter is generally in the range 0.1 to 1 mm. It has been correlated empirically with af², system properties and operating conditions. Dispersed phase holdup, when plotted against the product af, showed minimum values corresponding to the transition from mixer-settler to emulsion regime. Holdup was also found to be affected by mass transfer and its direction. Entrainment of fine droplets in the continuous phase occurs at high agitation levels, but can be reduced by the addition of coalescence plates at the base of the column. Energy dissipation rates greatly exceed predictions from the quasi-steady-state model.     

转盘塔内甲基异丁基酮萃取湿法磷酸实验研究

溶剂萃取法是一种经济有效的湿法磷酸净化方法。在转盘塔中,以甲基异丁基酮（MIBK）为萃取剂,开展了净化湿法磷酸的实验研究。考察了搅拌转速、相比对磷酸萃取率、杂质离子选择性、洗涤效果和反萃效果的影响。研究结果表明：萃取过程适宜的相比（溶剂与磷酸的体积比）为4,搅拌转速为200~400 r/min,在此条件下磷酸萃取率为85%;洗涤过程的搅拌转速不应大于100 r/min,适宜的洗涤酸用量为溶剂相体积的10%~15%,在此条件下铁离子（Ⅲ）和镁离子脱除率均在90%以上、铝离子脱除率大于70%、硫酸根脱除率为50%~60%;反萃过程搅拌转速不应大于200 r/min,适宜的反萃水用量为溶剂相体积的9%~15%。MIBK对阳离子的脱除效果较好,但是对阴离子的脱除效果不佳。经过萃取、洗涤和反萃3个过程,磷酸收率为57.8%~70.3%,磷酸中铁离子（Ⅲ）含量可以达到工业级磷酸标准,但是硫酸根的含量无法达标,需要结合其他方法进一步脱除。     

新型转盘萃取塔研究开发与工业应用

采用激光多普勒测速仪(LDV)和计算流体力学(CFD)软件,对转盘萃取塔(RDC)内的单相流流场进行了测量和模拟。发现塔内存在沟流和级间的旋涡流动,级间返混严重,为此发明了一种装有级间转动挡板的新型转盘萃取塔(NRDC)。NRDC与传统的RDC的区别在于安装了设计独特的转动挡板。这些转动挡板安装在2个转盘之间,固定在转动轴上,并与固定环处于同一水平面。LDV测量和CFD模拟结果发现,NRDC可有效抑制沟流和级间旋涡流动。传质实验和流体力学表明,NRDC的传质效率比RDC高20%—40%,而液泛速度大致相当。成功地将NRDC用于引进RDC的扩能改造和新塔的设计中。     

Axial mixing and mass transfer in a vibrating perforated plate extraction column

The axial mixing and countercurrent mass transfer characteristics of a 5 cm diameter extraction column agitated by vibrating perforated Teflon plates have been investigated. The dispersed phase was an organic liquid (usually kerosene) and the continuous phase was water. Axial mixing was measured in both phases using pulse tracer techniques; in the continuous phase the axial mixing was estimated to have a significant effect on mass transfer, but axial mixing in the dispersed phase had a negligible effect. Mass transfer was measured for several different solutes; n-butyric acid, benzoic acid and phenol. The overall heights of a transfer unit (cont. phase) were in the order of 10-20 cm for the organic-acids but higher for transfer of phenol from very dilute solutions. The characteristics of the vibrating plate column have been compared with those of other types of extractor and suggestions are made for further development.     

Steady state hydrodynamics and mass transfer characteristics of a karr extraction column

The steady state hydrodynamics of the holdup in a 15 cm column agree quite well with mechanistic predictions at conditions approaching flooding. In the presence of mass transfer (acetic acid from the dispersed kerosene phase to the continuous water phase), the holdup data below flooding are not well predicted by the model due to enhanced droplet coalescence. The prediction of holdup at flooding is a function of the ratio of the flow rates but is independent of the physicochemical properties of the extraction system, and therefore can be used to estimate the flooding holdup regardless of the occurrence of mass transfer. In the second part of the paper, steady state mass transfer characteristics of the column were also simulated using a mechanistic model. Despite the difficulty of estimating parameters such as the mass transfer coefficient, the model curves could be arbitrarily adjusted to fit observed exit concentrations. These steady state results provide useful insights on the non-linearity of the system from a control viewpoint.     

Factors affecting oil extraction/water adsorption in sequential extraction processing of corn

The sequential extraction process (SEP) uses ethanol to extract oil and protein from cracked, flaked, and dried corn, and the dried corn simultaneously dehydrates the ethanol. Value-added co-products are possible, potentially making production of fuel ethanol more economical. The effects of solvent-to-corn (S/C) ratio, corn moisture content (MC), and number of extraction stages on ethanol drying, oil recovery, and protein loss during the simultaneous oil extraction/water adsorption step of SEP were evaluated. Extractions were carried out by using both aqueous ethanol and ethanol/hexane blends at 56°C. The S/C ratios tested were 3∶1, 2∶1 (control), 1.5∶1, and 1∶1 (w/w). More anhydrous ethanol, greater oil yields, and less co-extracted protein were obtained with higher S/C ratios. Less anhydrous ethanol and lower moisture adsorption capacities were obtained when the corn MC was ≥1.12%. Oil yields gradually decreased with drier corn, whereas protein loss increased when corn MC was <1.12%. Reducing the number of extraction stages from seven (original SEP) to five did not affect ethanol drying capability, oil yields, and protein co-extracted with oil. Using ethanol/hexane blends resulted in more anhydrous ethanol, higher oil yields, and less protein co-extracted with oil.     

微分散轮盘塔萃取净化湿法磷酸的实验研究

采用筛网孔径为75 μm的微分散轮盘萃取塔净化湿法磷酸,在TBP+煤油/磷酸/水为体系的实验条件下,研究了浓度为55%的湿法磷酸的萃取及反萃特性,考察了不同转速、总体积通量和相比对萃取率和反萃取率的影响。研究结果表明,萃取率随转速及相比的增大而增大,随总体积通量的增大而减小,最优萃取条件：转速为250 r/min,总体积通量为56.62 L/(m2?min),相比为4,磷酸萃取率可达55%;反萃率随转速的增大而增大,随相比及总体积通量的增大而减小,最优反萃条件：转速为300 r/min,总体积通量为56.62 L/(m2?min),相比为6,磷酸反萃率可达85 %。通过量纲为1化拟合出体积传质系数经验计算式为KXa=1.53×10?3p?0.28135Fr0.344493W/D,与实验规律吻合,可以为工业放大设计和优化提供了较好的实验依据。     

转盘式萃取塔有效扩散系数的预测及其在设计中的应用

A rotating disc column (RDC) with inner diameter 68 mm and 28 compartments is used in this study. Parameters including Sauter mean diameter, hold-up and mass transfer coefficient are measured experimentally under different operating conditions. The correlations in literature for molecular diffusion and enhancement factor equation including eddy diffusion, circulation and oscillation of drops are evaluated. A new equation for the effective diffusion coefficient as a function of Reynolds number is proposed. The calculated values of mass transfer co-efficient and column height from the previous equations and present equation are compared with the experimental data. The results from the present equation are in very good agreement with the experimental results, which may be used in designing RDC columns.     

Prediction of mass transfer coefficients in a pulsed disc and doughnut extraction column

A study of the mass transfer performance for a pulsed disc and doughnut extraction column has been presented for a range of operating conditions. The mass transfer performance has been investigated for both directions of mass transfer. This study has examined the mass transfer coefficients which has incorporated the effects of back‐mixing in the continuous phase. The effect of operating variables including pulsation intensity and dispersed and continuous phase velocities on volumetric overall mass transfer coefficient has been investigated. The experiments showed that mixer‐settler, transition and emulsion regimes exist in the column depending on the pulse characteristics. In the present work, effective diffusivity is substituted for molecular diffusivity in the Gröber equation for estimation of overall mass transfer coefficients. The enhancement factor is determined experimentally and there from a single empirical correlation is derived for prediction of enhancement factor in terms of Reynolds number, holdup and Eötvös number for all operating regimes and each mass transfer direction. The experimental results are in very good agreement with the values calculated by the proposed equation. © 2011 Canadian Society for Chemical Engineering     

基于均龄理论高效计算萃取塔轴向混合分布

在验证了CFD单相流场模拟的基础上,采用均龄理论计算了中试转盘塔内的轴向混合分布,并将计算结果和理论平均停留时间以及组分输运模型计算值进行对比。结果表明:均龄理论能准确预测转盘塔内的轴向混合信息,且其计算时间只需数十秒,远小于传统组分输运模型所需的两周时间,具有低计算量的特点;同时均龄理论克服了传统组分输运模型无法模拟轴向混合空间分布的缺陷,为萃取塔内部结构优化提供了更多信息,是一种高效的模拟方法。后续均龄理论模拟结果的分析预示着转盘塔内的流动近似呈现出级内全混、级间平推的特点,符合萃取操作的需求;而相对于转盘间良好的混合作用,静环间存在明显的流动死区,造成一定的非理想性,其结构有待于进一步的优化。     

Prediction of dispersed phase holdup in pulsed disc and doughnut solvent extraction columns under different mass transfer conditions

Using experimental data from a number of pulsed disc and doughnut solvent extraction columns,a unified correlation for the prediction of dispersed phase holdup that considers the effects of mass transfer is presented.Pulsed disc and doughnut solvent extraction columns(PDDC) have been used for a range of important applications such as uranium extraction and nuclear fuel recycling.Although the dispersed phase holdup in a PDDC has been presented by some researchers,there is still the need to develop a robust correlation that can predict the experimental dispersed phase holdup over a range of operating conditions including the effects of mass transfer direction.In this study,dispersed phase holdup data from different literature sources for a PDDC were used to refit constants for the correlation presented by Kumar and Hartland [Ind.Eng.Chem.Res.,27(1988),131–138] which did not consider the effect of column geometry.In order to incorporate the characteristic length of the PDDC(i.e.the plate spacing),the unified correlation for holdup proposed by Kumar and Hartland based on data from eight different types of columns [Ind.Eng.Chem.Res.,34(1995) 3925–3940] was refitted to the PDDC data.New constants have been presented for each holdup correlation for a PDDC based on regression analysis using published holdup data from PDDCs that cover a range of operating conditions and physical properties and consider the direction of mass transfer.     

水辅助溶剂法提取油砂中的沥青

开发了一种水辅助溶剂法从油砂中提取沥青的技术。该方法通过在油砂固相与有机溶剂间介入水层提取油砂中的沥青。以内蒙古扎赉特旗油砂矿为研究对象,考察了温度、剂砂质量比、提取时间、甲苯在复合溶剂中的含量及溶剂的种类与性质对沥青回收率高低的影响,结果表明：最佳提取条件为提取温度50℃,剂砂质量比1∶1,提取时间25min。沥青回收率与提取溶剂的性质紧密相关,水层介入有效降低了固体微粒组分在有机相中的含量,且便于后续的有机相与泥砂相的分离。通过对各种溶剂提取的沥青进行组分分析,发现各种溶剂对沥青提取能力的差异性源于溶剂的化学组成和结构不同。本文相关研究结果对溶剂法提取油砂中沥青技术及溶剂种类的选择具有指导作用。