缓冲盐溶液反萃分离红霉素A、C的研究

用NaH2PO4-Na2HPO4缓冲盐溶液反萃醋酸丁酯相中的红霉素,以纯化酯相中的红霉素A。分别考察了缓冲盐pH值、相比(体积比)、温度对红霉素A、C反萃取的影响。实验结果表明:随着pH值的增加,红霉素A的反萃率大大减少,红霉素C的反萃率先增加后减小,当pH=8时,酯相中红霉素A纯度最高且损失最低;随着相比(A/O)的增加,红霉素A、C的反萃率及酯相中的红霉素A纯化效果都略有提高,但综合考虑反萃剂用量和红霉素A损失,可知相比(A/O)为2∶1时较优;随着温度的增加,红霉素A、C的反萃率都大大减小,且酯相中的红霉素A纯度略有下降,但因红霉素A反萃损失较少,可考虑在328 K时,反萃2次,除去大量红霉素C的同时损失较少的红霉素A。     

复合溶剂萃取麦白霉素的研究

研究了用异辛醇和航空煤油(4∶1V/V)的混合物萃取麦白霉素的工艺条件及其经济技术优越性。结果表明,麦白霉素的萃取溶剂消耗量由6.7kg/10亿单位降至2.47kg/10亿单位,降低生产成本41元/10亿单位,提取的总收率与用醋酸丁酯时相当,产品质量合格;革除了从萃余液中回收溶剂的工艺步骤,大大降低了能耗。     

稀释剂对三烷基氧膦萃取草酸的影响

In liquid-liquid solvent extraction processes, diluents have a strong influence on the extraction mechanism and efficiency. In this study, benzene, cyclohexane, trichloromethane, carbon tetrachloride, methyl isobutyl ketone (MIBK), butyl acetate, and 1-octanol were used as diluents in the extraction of oxalic acid by trialkylphos-phine oxide (TRPO). The effects of extractant concentration, initial concentration of oxalic acid and diluent type on the extraction equilibrium partition coefficient are analyzed. The sequence of the extraction ability by different diluents is MIBK > butyl acetate > cyclohexane=benzene > carbon tetrachloride > 1-octanol > trichloromethane. Extraction mechanism was analyzed and extraction model parameters were evaluated.     

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     

2,3-丁二醇萃取-精馏耦合工艺开发研究

在前期液-液相平衡研究的基础上,得出正丁醇、乙酸乙酯及乙酸丁酯在萃取2,3-丁二醇时的不同特点.并根据其特点,分别设计了2条创新的间歇-循环的萃取-精馏耦合工艺.根据乙酸乙酯、乙酸丁酯分配系数小、相比(质量比)要求较大的特点,设计萃取-精馏耦合工艺一(即溶剂循环、料液间歇进料),该工艺具有相比逐渐增大、溶剂循环萃取的特...     

Kinetic analysis of benzyl alcohol oxidation by alcohol oxidase in aqueous—organic two-phase systems

Alcohol oxidase-catalyzed oxidation of benzyl alcohol to benzaldehyde was studied in three two-liquid phase systems involving butyl acetate, xylene and n-decane. A more highly hydrophobic solvent resulted in more favorable partitioning of the substrate into the aqueous phase and less deleterious effect on the enzyme activity. As a result, the overall production of aldehyde was highest with the n-decane system and lowest with the butyl acetate system. In addition, the organic solvent served as an extractant for the product, which acted both as a competitive inhibitor and as a denaturant of the enzyme. The time courses of benzaldehyde production were simulated by a simple mathematical model assuming Michaelis–Menten kinetics in the aqueous phase, enzyme deactivation by organic solvents and the equilibrium partitioning of the reagents between the two phases.     

由辣椒粉浸出液萃取辣椒碱

以市售干辣椒为原料、95%乙醇为浸出剂,实验研究了溶剂萃取法由辣椒粉浸出液中萃取纯化辣椒碱的工艺条件. 在模拟体系和实际体系中均以正己烷和乙酸丁酯为萃取剂,考察了pH值和有机相/水相体积比对辣椒碱收率的影响. 结果表明酸化萃取步骤为工艺控制步骤. 模拟体系中pH值为11、体积比为7:1时乙酸丁酯对辣椒碱的萃取收率均大于90%,表明以乙酸丁酯为萃取剂,可以提高辣椒碱的浓缩度. 实际体系萃取结果与模拟体系趋同,但约20%的辣椒碱不能被萃取. 实际体系优化的工艺条件为辣椒粉用量50 g,250 mL 95%乙醇2次浸出,辣椒碱收率为97.0%;浸出液浓缩为浸膏并溶解于NaOH溶液中,在pH值13, O/W体积比1:1时萃取,再用盐酸调节水相pH<11,O/W体积比为1:5时用乙酸丁酯萃取,辣椒碱的收率为浸出量的80%左右.     

溶剂萃取1,2-环己二醇的研究

采用萃取平衡实验法,首次研究了用有机溶剂萃取水相中1,2-环己二醇的萃取热力学性质,为1,2-环己二醇的分离、提纯建立了一种新方法并提供了基础数据。考察了乙酸乙酯和乙酸丁酯作为萃取剂,苯、甲苯、环己烷、正庚烷、甲基丙基酮、1,2-二氯乙烷作为稀释剂时,对萃取水相中1,2-环己二醇的影响,并证实了该萃取过程为吸热过程。     

液体石蜡萃取法回收废水中的乙酸丁酯

为实现制药工业低浓度含乙酸丁酯废水的资源化利用, 通过考察生物质及乙酸丁酯的初始浓度、萃取温度、萃取时间、相比(萃取剂与含酯废水的体积比)等因素对萃取率的影响, 建立了以液体石蜡为萃取剂的对含酯模拟废水的萃取回收体系。结果表明:生物质浓度对萃取效果影响不大, 当相比为1:1、时间15min、温度25℃时, 对含酯0.7g/100mL的模拟废水, 液体石蜡的萃取率可达98%。利用多级萃取, 将已负载乙酸丁酯的萃取剂液体石蜡继续处理新鲜废水, 验证了萃取剂对乙酸丁酯的富集能力强而稳定。通过选取适宜相比进行多级萃取, 可将乙酸丁酯富集于液体石蜡中, 从而明显降低后处理的能耗。对萃取相进行减压蒸馏, 可将乙酸丁酯从液体石蜡中分离出来。经检测, 蒸馏液为质量浓度约98%的乙酸丁酯, 且含水量低于0.1%, 可回用作药物提取剂;同时液体石蜡得以再生, 且萃取效果良好。     

新型己内酰胺萃取剂的筛选和评价

Mixed solvent of 1-octanol and cyclohexane with 60% （by mass） 1-octanol content was selected as a new extractant for caprolactam extraction. Compared with benzene or toluene, the new extractant has larger extraction capacity and much lower toxicity. Although the extraction capacity of the new extractant is smaller than that of pure 1-octanol, 1-octanol solubility of the new extractant in aqueous phase is much smaller. Because of its physical properties of lower density, lower viscosity, and higher interfacial tension, the new extractant performed much better phase separation ability than pure 1-octanol. The new extractant showed certain selectivity when dealing with lactam oil. The mixed solvent of 1-octanol and cyclohexane with 60% （by mass） 1-octanol content is a promising extractant for caprolactam extraction.     

Synergistic Solvent Extraction of Lanthanides (III) with Mixtures of Tetraphenylmethylenediphosphine Dioxide and Picrolonic Acid from HCl Solutions

The solvent extraction of lanthanides(III) from hydrochloric acid solutions into the organic phase containing neutral bidentate extractant tetraphenylmethylenediphosphine dioxide (L) and picrolonic acid (HP) has been studied. A considerable synergistic effect was observed in the presence of HP in the organic phase containing neutral bidentate organophosphorus ligand. The extraction equilibrium was investigated and the equilibrium constants were calculated. It was found that the lanthanide(III) ions are extracted from weak acidic solutions as LnP₃L and LnP₃L₂ complexes. The mixture L–HP offers higher extraction efficiency toward Ln(III) than mixtures of L with 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 or picric acid.     

Improved extraction of penicillin G using hydrocarbon sulfoxides

Extraction of penicillin G with sulfoxide extractants, petroleum sulfoxide (PSO) and di‐isooctyl sulfoxide (DISO) was researched systematically. Based on research of the extraction equilibrium of penicillin G, the suitable extraction and re‐extraction conditions were determined, and then extraction cascade and bench‐scale experiments were carried out. The performance of extraction systems composed of PSO and DISO, with sulfonated kerosene as the diluent, is superior to that of n‐butyl acetate owing to the low solubility of these new extractants in water. Their consumption during the extraction process was lower, and the recovery step of extractants from aqueous raffinate was eliminated. Copyright © 2004 Society of Chemical Industry     

连续逆流提取氢化可的松的实验研究

首先对以乙酸丁酯为萃取剂从发酵液中萃取氢化可的松的液液平衡数据进行了测定,并在此基础上进行了多级逆流模拟试验和单级试验,最后以五级混合澄清槽为萃取设备,进行了连续逆流萃取试验。在选定的实验条件下,氢化可的松的萃取率可以达到98.7%,乙酸丁酯的消耗量相比现行的错流萃取工艺下降了50%。     

Extraction of erythromycin‐A using colloidal liquid aphrons: I. Equilibrium partitioning

Colloidal liquid aphrons (CLAs) are surfactant‐stabilised solvent droplets which have recently been explored for use in pre‐dispersed solvent extraction (PDSE). In this work, the equilibrium partitioning of a microbial secondary metabolite, erythromycin, has been studied using both CLAs (formulated from 1% (w/v) Softanol 120 in decanol and 0.5% (w/v) SDS in water) and surfactant‐containing, two‐phase systems. The equilibrium partitioning of erythromycin was found to be strongly influenced by the extraction pH, and exhibited a marked change either side of the pK_a of the molecule. A modified form of the Henderson–Hasselbach equation could be used as a simple design equation to predict the equilibrium partition coefficient (m_eryt = C_org /C_aq) as a function of pH. For extraction experiments with dispersed CLAs where pH > pK_a, m_eryt values as high as 150 could be obtained and the erythromycin could be concentrated by factors of up to 100. Experiments were also carried out in surfactant‐containing, two‐phase systems to determine the effect of individual surfactants used for aphron formulation on erythromycin partitioning. For extraction at pH 10 neither the Softanol (a non‐ionic surfactant) nor SDS (an anionic surfactant) had any influence on the equilibrium erythromycin partition coefficients. For stripping at pH 7, however, it was found that recovery of erythromycin from the organic phase decreased with increasing concentration of SDS, although again the Softanol had no influence on the equilibrium. The effect of SDS was attributed to a specific electrostatic interaction between individual erythromycin and SDS molecules under stripping conditions. The m_eryt values and concentration factors achievable in the two‐phase systems were considerably less than those for the PDSE experiments. The physical properties of the two‐phase systems, ie density, viscosity, interfacial tension, etc, and the equilibrium distribution of the surfactants were also determined in relation to subsequent studies on the kinetics of erythromycin extraction. © 2000 Society of Chemical Industry     

溶剂萃取法净化萃余酸制磷酸二氢钾

 研究了以氯化钾和湿法磷酸净化后的萃余酸为原料,利用正丁醇为萃取剂回收萃余酸中湿法磷酸制备磷酸二氢钾的新方法。研究了正丁醇含水量、萃取时间、萃取温度及萃余酸用量等因素对产品产量的影响,确定了适宜的工艺条件。实验结果表明,优化的工艺条件为：m（萃余酸）∶V（正丁醇）为127.4 g/L、m（水）∶V（正丁醇）为95 g/L、温度为30 ℃、萃取时间为60 min、m（氯化钾）∶V（正丁醇）为26.075 g/L。本研究提供了一种回收利用萃余酸的经济、简单的方法。     

三烷基氧磷萃取对氨基苯酚的性能

以三烷基氧磷(TRPO)为反应萃取剂,研究了稀释剂种类、溶液pH值等因素对对氨基苯酚稀溶液反应萃取分配系数(D)的影响,提出了同时考虑反应萃取和物理萃取作用的分配系数的表达式.结果表明：TRPO对对氨基苯酚的萃取主要通过与其中性分子的氢键缔合和溶剂化效应实现,D值的变化与中性分子的摩尔分数有关;稀释剂的极性对对氨基苯酚的萃取影响较小;除20%TRPO/正庚烷体系外,拟合实验数据得到的表观萃取平衡常数变化较小;体系的物理萃取分配常数则随TRPO浓度的增大而增大,且符合稀释剂和TRPO的物理萃取能力的简单加和;酸性、碱性和中性的反应萃取剂都可有效地萃取对氨基苯酚,萃取能力为二(2-乙基己基)磷酸＞ TRPO ＞ 三烷基胺,相应的操作pH值为2～3、4～5和6.5～7.5,应用时可根据体系的pH值范围选用相应的萃取剂,而不必调节溶液的pH值.     

Fractionation of Carboxylic Acids Mixture Obtained by Succinic Fermentation using Reactive Extraction

Formic, acetic, and succinic acids have been selectively separated from their mixture obtained by A. succinogenes fermentation using reactive extraction with tri-n-octylamine (TOA) dissolved in three solvents with different polarities (n-heptane, butyl acetate, and dichloromethane) without and with 1-octanol addition. This technique allows recovering formic and acetic acids from the mixture, the raffinate containing only succinic acid. The extractant concentration and organic phase polarity control the selectivity of acids extraction. Thus, at pH = 1, the selectivity factor increased from 92, in the absence of 1-octanol; to 148, in the presence of this alcohol in organic phase. The corresponding optimum concentrations of TOA in the solvent were 30 and 50 g/l, respectively. The total separation of monocarboxylic acids from the mixture with succinic acid is possible by a multi-stage extraction process, adjusting the extractant concentration in each stage to that stoechiometrically needed for reactions with formic and acetic acids only. The addition of 1-octanol reduces the number of required extraction stages.     

溶剂萃取法分离氢化可的松和表氢化可的松

针对工业上现有结晶分离工艺的缺点,提出了分离氢化可的松及其光学异构体表氢化可的松的新方法——溶剂萃取法。实验发现,在常规醇类、酮类、酯类、醚类、氯代烃类和芳香烃等溶剂中,乙酸丁酯具有较好的萃取分离性能,以乙酸丁酯为萃取剂用溶剂萃取法分离氢化可的松粗品可获得纯度为９８％以上的氢化可的松,已达到工业生产水平。文中还研究了乙醇含量、温度、盐析效应和ｐＨ对分配的影响。     

Monolayer Behavior of Hydroxyoxime Extractants

Abstract

Efforts to elucidate solvent extraction mechanisms in hydrometallurgical systems have generally been hindered by a lack of physico-chemical data pertaining to the interfacial properties of organic-soluble extractants and their metal complexes. In an effort to address this situation, a Langmuir film balance was used to characterize the interfacial properties of purified metal extractants spread as monomolecular films at the air/water interface. This interfacial system was used as a model for studying the interactions of the extractant films with the aqueous phase. The metal extractants used in this study were: the anti-isomer of 5,8-diethyl-7-hydroxy-6-dodecanone oxime (DEDO, the active extractant in LIX63, Henkel), and the anti-isomer of 2-hydroxy-5-nonylbenzophenone oxime (HBPO, the active extractant in LIX65N, Henkel). Both equilibrium and dynamic film properties of single component and mixed monolayers were examined. The effects of aqueous phase copper ion on the equilibrium properties of these extractant monolayers were also investigated.     

Novel Gas-assisted Three-liquid-phase Extraction System for Simultaneous Separation and Concentration of Anthraquinones in Herbal Extract

abstract Gas-assisted three-liquid-phase extraction (GATE), which has the advantages of both three-liquid-phase extrac-tion and solvent sublation, is a novel separation technique for separation and con...