Extraction of Hydrocortisone from the Fermentation Liquor with Annular Centrifugal Contactors

Abstract

A continuous countercurrent extraction process for the recovery of hydrocortisone from the fermentation liquor has been developed with annular centrifugal contactors. When the hydrocortisone was extracted from the fermentation liquor with the butyl acetate, the distribution ratio increased with increase of the hydrocortisone concentration in the equilibrium aqueous phase. Both the laboratory tests and the plant tests have been finished with Φ20 mm and Φ230 mm annular centrifugal contactors respectively. In the laboratory tests, when the rotor speed was 3400～4200 r/min, the fermentation liquor flow was 30～50 mL/min and the phase ratio (V_O/V_A) was 0.36～0.50, the percent recovery of hydrocortisone was higher than 92%. In the plant tests, when the rotor speed was 2000 r/min, the fermentation liquor flow was 2000 L/h and the butyl acetate flow was 1000 L/h, the percent recovery of hydrocortisone was about 96.5～98%.     

Evaluation of Annular Centrifugal Contactors for the Extraction of Acetic Acid from Aqueous Streams

This study investigates the use of annular centrifugal contactors for the liquid-liquid extraction of acetic acid from an acidic aqueous phase into an organic phase consisting of 1.5 M Tributyl Phosphate in n-Dodecane. Initial break time tests were performed in order to investigate the mixing/separation viability of the organic/aqueous system, and after determining that centrifugal contactors could be used to perform the liquid-liquid extraction, hydraulic tests established the combination of rotation rate and throughput which should be used to ensure proper separation of the two outlet phases. Finally, extraction efficiency data was collected to examine the system conditions that provided the most efficient removal of acetic acid.     

Separation of Ionic Liquid Dispersions in Centrifugal Solvent Extraction Contactors

Abstract

Separations of dispersions formed by mixing immiscible organic room‐temperature ionic liquids (IL)/hydrocarbon/and aqueous systems using a centrifugal solvent‐extraction contactor have been successfully demonstrated in proof‐of‐concept testing. This accomplishment is significant in that physical property factors that are typical of ionic liquid systems (e.g., similar densities of the bulk phases, low interfacial tensions, and high viscosities) are typically unfavorable for dispersion separation, particularly in continuous processes. Efficient separation of dispersions containing ionic liquid solvents is essential for utilization of these compounds in liquid‐liquid extraction applications to maximize both solute transfer efficiency and solvent recovery. Efficient solvent recovery is of particular concern in IL applications because of the high cost of most IL solvents.

This paper presents the results of initial experiments with three hydrophobic ionic liquids to determine how their physical properties affect phase mixing and phase disengagement in contact with an aqueous solution using a centrifugal contactor. While the results of the reported work are promising, additional work is needed to optimize existing mathematical models of contactor hydraulics to address special considerations involved in IL‐based processes and to optimize the equipment itself for IL applications.     

Application of Annular Centrifugal Contactor on Separating Indium from Iron

Abstract

It is hard to separate indium from iron in sulfuric acid leachate without reducing Fe³⁺ to Fe²⁺ with di(2-ethylhexyl) phosphoric acid (HDEHP) by the equilibrium extraction process. A nonequilibrium extraction process with annular centrifugal contactors is studied through the extraction kinetics difference between In and Fe. The mass transfer velocities of In and Fe were determined. Laboratory- and industry-scale extraction tests with miniature and industry scale annular centrifugal contactors, respectively, were conducted. The results indicate the mass transfer velocity of In is much faster than that of Fe, the contact time between the two phases is very short in the contactor, and the In can be well separated from Fe in the nonequilibrium extraction process with annular centrifugal contactors.     

环隙式离心萃取器界面半径的测定与关联

采用“快速放液法”测定转筒内的存留量，并用合适的相分布模型计算出相应的界面半径，即实验值。系统研究了转速、流比、重相堰直径、流量、两相密度差和粘度６个参数对环隙式离心萃取器界面半径的影响。用多元回归关联了６个自变量，拟合了界面半径的经验公式。计算值与实验值吻合较好，平均误差３．０３％，可用来确定２０ｍｍ环隙式离心萃取器最佳工作条件。     

Demonstration of an Improved Total Partitioning Process for High Level Liquid Waste Using Annular Centrifugal Contactors

High level liquid waste (HLLW) produced from the reprocessing of the spent nuclear fuel still contains moderate amounts of uranium, transuranium (TRU) actinides, ⁹⁰Sr, ¹³⁷Cs, etc., and thus constitutes a permanent hazard to the environment. The partitioning and transmutation (P&T) strategy has increasingly attracted interest for the safe treatment and disposal of HLLW, in which the partitioning of HLLW is one of the critical technical issues. An improved total partitioning process, including a TRPO (tri-alkylphosphine oxide) process for the removal of actinides, a CESE (crown ether strontium extraction) process for the removal of Sr, and a calixcrown ether extraction process for the removal of Cs, has been developed to treat Chinese HLLW at the Institute of Nuclear and New Energy Technology (INET), Tsinghua University, China. A demonstration test of the improved total partitioning process was carried out using 74-stage 10-mm-dia annular centrifugal contactors and simulated HLLW. The test results showed that the decontamination factors were >1.2 × 10⁶, 4600, and 7500 for Nd, Sr, and Cs, respectively. In the test, Nd was used to simulate Am. During the test, 74-stage 10-mm-dia annular centrifugal contactors worked stable continuously with no stage failing or interruption of the operation.     

Development of a Solvent Extraction Model for Process Tests in Short Residence Time Centrifugal Contactors

A computer program has been developed for optimization and modelling of counter–current solvent extraction processes. The distribution between the phases is calculated by either D-ratio functions or by a novel kinetic model for the transfer between the phases. The kinetic model is important to use when slow extraction kinetics yields D-ratios far from equilibrium. Transfer rate data was investigated in a single stage centrifugal contactor, modified for internal recirculation of the phases. Using this methodology a demonstration process for the recovery of minor actinides in a counter–current centrifugal contactor system using CyMe₄-BTBP was modelled with excellent agreement towards the experimental values.     

离心萃取器在咖啡因工业生产中的应用

在咖啡因工业生产中,一般是采用静态混合器为萃取设备、氯仿为萃取剂来回收母液中的咖啡因,主要缺点是萃取率只在90％左右以及氯仿损失大。离心萃取器是一种高效的液一液萃取设备,具有许多显著优点,为此,采用了4台Ф230离心萃取器代替静态混合器组成串联逆流萃取流程,对该生产环节进行了技术改造,结果表明,萃取率提高到了99％,氯仿用量降低到了25％。     

用离心萃取器连续逆流提取氢化可的松的研究

采用环隙式离心萃取器进行了提取氢化可的松的研究。用醋酸丁酯从发酵液中萃取氢化可的松 ,其传质过程受扩散因素控制 ,且分配系数随平衡水相浓度的增大而增大。开发了用环隙式离心萃取器连续逆流提取氢化可的松的工艺流程 ,当转速为 340 0～ 380 0r/min ,总流量为 40～ 75mL/min ,V(O ,有机相 )∶V(A ,水相 )为 (0 35～ 0 42 )∶1 0 0时 ,氢化可的松的萃取率为91 0 8%～ 93 16 % ,而厂家现行生产工艺采用的V(O)∶V(A)是 0 7∶1 0 ,氢化可的松的萃取率为90 %。因而 ,新工艺提高了氢化可的松的萃取率 ,降低了萃取剂耗量     

Annular Centrifugal Contactors for Solvent Extraction

Abstract

Annular centrifugal contactors suitable for laboratory use in solvent extraction work have been designed and tested for both hydraulic performance and mass-transfer efficiency. The 2-cm contactors have nominal flow rates of 80 mL/min and mass-transfer efficiencies of at least 85% as measured by the extraction of uranium. These contactors work well for organic-to-aqueous (O/A) flow ratios greater than 0.8. Multistage units allow proposed flow sheets to be tested on a continuous basis in the laboratory. Scale-up to larger plant-size units is straightforward.     

Thirty Stage Annular Centrifugal Contactor Thermal Profile Measurements

A thirty stage 5 cm annular centrifugal contactor cascade was assembled and tested to obtain thermal profiles during both ambient and heated input conditions of operation. Thermocouples were installed on every stage as well as feed inputs, and real-time data was taken during experiments lasting from two to eight hours at total flow rates of 0.5 to 1.4 liters per minute. Ambient temperature profile results show that only a small amount of heat is generated by the mechanical energy of the contactors. Steady state temperature profiles mimic the ambient temperature of the lab but are higher toward the middle of the cascade. Heated inlet solutions gave temperature profiles with smaller temperature gradients, more driven by the temperature of the inlet solutions than ambient lab temperature. Temperature effects of solution mixing, even at rotor speeds of 4000 rpm, were not measurable.     

Radioactive Tracer Tests of Two Improved TRPO Processes for High-Level Liquid Waste Using Annular Centrifugal Contactors

High-level liquid waste (HLLW) produced from the reprocessing of the spent nuclear fuel still contains moderate amounts of uranium, transuranium (TRU) actinides, and fission products, and thus constitutes a permanent hazard to the environment. The partitioning and transmutation (P&T) strategy has increasingly attracted interest for the safe treatment and disposal of HLLW, in which the partitioning of HLLW is one of the critical technical issues. Two improved trialkylphosphine oxide (TRPO) processes for the removal of actinides have been developed to treat Chinese HLLW, based on the original TRPO process. In one improved process N,N-diethylhydroxylamine as a reducing agent was used for reducing Np(V) and Np(VI) to Np(IV) in order to improve the extraction efficiency of Np. In the other improved process, ammonium vanadate as an oxidizing agent was used for oxidizing Np(V) and Np(IV) to Np(VI) in order to improve the extraction efficiency of Np. Radioactive tracer tests of two improved TRPO processes were carried out using 30-stage 10-mm-diam annular centrifugal contactors and simulated HLLW containing U, Np, Pu, and Am. The test results showed that the decontamination factor of total α activity was >1 × 10⁵. During the test, 30-stage 10-mm-diam annular centrifugal contactors worked in a stable manner continuously, with no stage failing or any interruption of the operation.     

Determination of the Liquid Hold-up Volume and the Interface Radius of an Annular Centrifugal Contactor using the Liquid-Fast-Separation Method

Annular centrifugal contactors (ACCs), which use centrifugal force to separate the dispersion of two immiscible liquids of different densities, have been utilized in many industrial fields, such as the petroleum, hydrometallurgy, wastewater treatment, pharmaceutical processing, protein extraction, enantioselective chemical separation, biodiesel synthesis, and nuclear industries. Detailed hydrodynamic information, such as the liquid hold-up volume and the interface radius, is very important for successful design and operation of ACCs. A new method, namely, the liquid-fast-separation method, was developed to (1) obtain the parameters of the liquid hold-up volume, the actual phase ratio (aqueous phase/organic phase, a/o) of two phases in the mixing zone, and the interface radius, and (2) investigate the effects of the rotor speed, the total flow rate, the flow ratio (a/o), and the diameter of the heavy phase weir on these parameters. The experimental results indicated that the parameters of the liquid hold-up volume, the actual phase ratio (a/o) of two phases in the mixing zone, and the interface radius could be obtained using the liquid-fast-separation method. Moreover, the effects of the rotor speed, the total flow rate, the flow ratio (a/o), and the diameter of the heavy phase weir on these parameters could also be obtained. These results provide a more complete understanding of the fluid flow in ACCs to enable further advancements in their design and operation.     

Hydraulic and Mass-Transfer Performance of a 20-Mm-Diameter Annular Centrifugal Contactor for the Solvent Extraction of Cesium by Bis(2-Propyloxy)Calix[4]-Crown-6 in n-Octanol

A calixcrown extraction process using bis(2-propyloxy)calix[4]-crown-6 (iPr-C[4]C-6) as extractant and n-octanol as diluent for the separation of cesium from Chinese High Level Liquid Waste (HLLW) has been developed at INET. Chinese HLLW is acidic defense waste with high salt content, which is now stored in underground stainless steel tanks. The intention is to use a process to extract cesium from HLLW conducted on multistage 20-mm-diameter annular centrifugal contactors (ACCs), so it is necessary to study the hydraulic and mass-transfer performance of a 20-mm-diameter ACC for the extraction system. In this work, the effects of the parameters such as the rotor speed, the diameter of heavy weir, and the acid concentration on the hydraulic performance were investigated. An operational envelope of the 20-mm-diameter ACC for the n-octanol/aqueous solution system was identified. The mass-transfer efficiency of the single stage 20-mm-diameter ACC for the extraction and stripping of cesium with iPr-C[4]C-6 in n-octanol was studied by varying several parameters, such as the rotor speed, the total flow rate, and the flow ratio. The extraction stage efficiency is greater than 95% at suitable operating conditions for extracting Cs⁺ with 0.025 mol/L of iPr-C[4]C-6 in n-octanol from HNO₃ solution containing Cs⁺. The stripping stage efficiency of Cs⁺ (< 90%) is lower than the extraction stage efficiency of Cs⁺.     

茶叶中咖啡因的提取研究进展

咖啡因是茶叶中的一种生物碱,现代医学研究表明咖啡因在生理上有重要作用,是一种中枢神经系统兴奋剂,能促进新陈代谢,影响神经、心脏和肾脏的功能,对人类的健康发挥着积极作用。目前,茶叶中咖啡因的提取有多种方法,但提取率和产品纯度存在较大的差异。重点介绍了茶叶中咖啡因提取方法的研究进展。     

从茶叶中提取天然咖啡因技术综述

综述用中低档茶及茶叶废料提取咖啡因的各种工艺技术,并对其特点和前景进行评价。     

超临界二氧化碳流体提取咖啡因研究进展

介绍了超临界流体萃取技术，综述了超临界二氧化碳流体提取咖啡因研究进展，并对其中的一些具有代表性的工艺进行了详细的阐述和评价。     

Synergistic Extraction of Lanthanides in a Liquid-Liquid Countercurrent Centrifugal Extractor

We have developed a liquid-liquid countercurrent centrifugal extractor that induces Taylor vortices in the annular fluid region. To demonstrate extraction of multiple species (Nd/Sm/Eu/Gd/Dy) with N,N,N′,N′-tetraoctyl diglycolamide (TODGA), additional chemical agents, such as a surfactant (sodium bis(2-ethylhexyl) sulfosuccinate (AOT)), a synergist (nonanoic acid) and a masking agent (N,N,N′,N′-tetraethyl-3,6-dioxaoctane-1,8-diamide (DOODA(C2))) were employed. When only TODGA was utilized, extraction performance was not effective due to the insufficient dispersion even under a high rotating speed. By combining TODGA and other chemical agents, the separation performance was improved considerably in the countercurrent flow of aqueous and organic phases due to the synergistic effect and improved dispersion.     

Single Centrifugal Contactor Test of a Proposed Group Actinide Extraction Process for Partitioning and Transmutation Purposes

In this work a solvent comprising of tri-butyl phosphate and bis-triazinyl, bi-pyridine in cyclohexanone has been used in a single centrifugal contactor test to evaluate its GANEX process potential. It was found that the density of the aqueous phase had to be increased to facilitate phase separation in the centrifuge. The kinetics of the system was also found to be relatively slow in the equipment of choice, especially regarding the stripping. However, it was still possible to recover more than 87% of all actinides in one extraction step with minor fission product contaminations using a flowrate of 30 mL/h.     

茶叶中咖啡碱的微波辅助萃取研究

研究了茶叶中料液质量比、浸提温度、浸提时间、提取液pH值、微波功率、微波作用时间等因素对咖啡碱溶出效果的影响,通过正交实验,对微波辅助萃取茶叶中咖啡碱的工艺条件进行了研究。结果表明：料液质量比1：30,浸提温度90℃,浸提时间30min,提取液pH值为6,微波功率350W,微波作用20s,茶叶中咖啡碱的浸出率可达3．90％以上。