次氧化锌酸性浸出液中直接萃取铟

针对现行湿法炼锌综合回收铟过程中存在的铟分散损失严重和直收率低的问题,采用直接萃取法从次氧化锌酸性浸出液中回收铟,考察了萃取剂浓度、混合时间、硫酸浓度和萃取温度等因素对铟及主要金属离子萃取率及盐酸浓度和相比对铟反萃率的影响,绘制了萃取平衡等温线和反萃平衡等温线,进行了小型模拟实验和连续逆流萃取-反萃实验,重点考察主要金属离子在萃取和反萃过程中的分布与走向.结果表明,以10%P204为有机相,在相比(A/O)为2/1、逆流萃取级数为3级的条件下,浸出液中铟萃取率达99.9%,杂质铁、锌和镉的萃取率分别为1.5%,0.5%和1.1%.得到的负载有机相采用6 mol/L盐酸反萃,相比为1/5时4级反萃后,铟反萃率达100%,镉、锌和铁基本被全部反萃,反萃后的贫有机相可循环使用.     

萘磺酸类有机废水的络合萃取研究

采用络合萃取法对萘磺酸类有机废水进行预处理。选用了三烷基胺(7301)、三辛胺作萃取剂,用NaOH、KOH、NH3.H2O作反萃剂,分别进行萃取与反萃实验,确定了最优良的萃取与反萃体系。同时,研究了萃取剂与稀释剂比例、废水pH、油水比以及萃取温度对废水萃取效果的影响及反萃时碱液的最佳质量分数和油碱比。     

铜萃取剂Mac12萃取性能的研究

采用国产化工原料合成了Mac12铜萃取剂，用Mac12萃取剂进行了萃取剂用量、有机相与无机相相比、pH值试验、萃取动力学试验、萃取热力学试验、反萃动力学试验、反萃剂酸度试验，得到了较好的萃取效果，萃取率≥93％，反萃取率≥96％。     

PC-88A萃取镍离子的工艺条件探究与优化

研究了酸性萃取剂2-乙基己基磷酸单2-乙基己基酯(PC-88A)萃取镍离子的萃取条件,反萃相硫酸含量对反萃效率的影响,并进行了优化。结果表明,优化萃取条件为:萃取反应温度40℃,萃取剂的体积分数80%,原料液初始pH为6.5,萃取剂皂化率为10%,此时PC-88A对Ni(II)的萃取率高达98.0%。在此优化条件下获得的负载有机相,采用0.8 mol/L的硫酸进行反萃,反萃率达到93.6%。     

2-丁基-2-乙基-1,3-丙二醇从地下卤水中提硼的研究

研究了以2-丁基-2-乙基-1,3-丙二醇为萃取剂,三氯甲烷为稀释剂,从四川平落地下卤水中萃取提硼。通过萃取条件的考察和筛选,最终确定萃取剂浓度为1.0mol/L,相比为1∶1,萃取时间为10min,萃取级数为二级的最优萃硼条件,此时萃取率可达98.56%,萃取剂的饱和萃取容量达44.25g/L(以H3BO3计)。同时,探究了以氢氧化钠溶液作为反萃剂的最佳反萃条件:反萃剂浓度为0.3mol/L,反萃相比为1∶1,反萃时间为8min,反萃级数为二级,其反萃率达到95.49%。在最优萃取和反萃条件下,经两级萃取和两级反萃,硼酸的回收率达到94.87%。     

草酸强化三价铁离子的反萃性能

二(2-乙基己基)磷酸(P204)常作为溶液净化除铁的萃取剂，P204-磺化煤油体系中Fe³⁺与有机相形成络合能力较强的萃合物，使得Fe³⁺反萃比较困难，需采用较高浓度的酸作为反萃剂，但高浓度的酸会破坏有机分子的结构，影响萃取剂循环利用。针对P204-磺化煤油负铁有机相反萃困难的问题，提出利用草酸为反萃剂对负载1g/L铁的P204-磺化煤油有机相的反萃行为进行研究，考察了反萃转速、草酸浓度、反萃温度、反萃时间和相比对Fe³⁺反萃率的影响。结果表明：以反萃转速200r/min，草酸0.4mol/L，反萃时间10min，反萃温度40℃，反萃相比1∶1，采用二级逆流萃取方式，铁的反萃率可以达到99%以上；Fe³⁺反萃过程是吸热反应，其反应的焓变为81.58kJ/mol，反萃过程符合准一级反应动力学方程，对应活化能为49.5kJ/mol。进一步研究了反萃后P204-磺化煤油有机相对Fe³⁺的萃取性能。结果表明：经5次草酸反萃后的P204-磺化煤油有机相萃铁性能几乎不变，对比于高浓度的酸反萃，草酸反萃简化了反萃流程，降低了萃取剂的消耗。     

混合醇萃取剂从浓缩盐湖卤水中萃取提硼的实验研究

以2-乙基-1,3-己二醇和异丁醇按照一定体积比组成混合萃取剂、航空煤油为稀释剂,萃取某硫酸盐型盐湖浓缩卤水中的硼。对萃取剂浓度、浓缩卤水pH、萃取相比、萃取温度、萃取时间、饱和萃取容量和反萃剂浓度、反萃相比等进行了实验研究。结果表明:2-乙基-1,3-己二醇、异丁醇和航空煤油体积比为1∶2∶3,卤水pH为3,萃取相比为1∶1,温度为20℃,萃取时间为5 min;将得到的富硼有机相用0.25 mol/L氢氧化钠溶液进行反萃,反萃相比为1∶2、温度为30℃、反萃取时间为15 min。经三级萃取及反萃,卤水中硼质量浓度降为0.8 mg/L,硼萃取率为99.99%,反萃率为99.78%,硼回收率为99.77%,萃取效果好。     

从乳酸铵发酵液提取乳酸的技术研究

利用萃取和反萃技术从乳酸铵发酵液中提纯乳酸,研究了在发酵液复杂成分条件下乳酸的萃取工艺,优化了萃取和反萃的工艺条件,实现了复杂体系条件下乳酸的提纯.重点研究了发酵液酸化过滤、萃取反萃温度、萃取剂饱和容量及分配比、级数确定、脱油、脱色、浓缩及水洗等工艺.探讨了络合萃取法的优点,萃取技术提纯乳酸的可行性.     

转盘萃取塔在净化湿法磷酸中的应用

在改进型转盘萃取塔中,以磷酸三丁酯（TBP）为萃取剂,航空煤油为稀释剂,对不同浓度的湿法磷酸进行萃取净化,并以蒸馏水为反萃剂对萃取相进行反萃。研究结果表明：转盘萃取塔用于萃取净化湿法磷酸具有良好的适用性,在适宜的操作条件下能取得较好的萃取和反萃效果。实验转盘塔在运行过程中稳定性较好。在该萃取体系下,Ф50mm转盘萃取塔的理论级当量高度约为0．65m。     

络合萃取法回收废液中的6-APA

利用络合萃取法回收废液中的6-APA,考察了稀释剂种类、络合剂浓度、p H、相比等对萃取效果的影响。结果表明,在0.117 5 mol/L甲基三辛基氯化铵氯仿溶液为混合萃取剂,水相p H=6,萃取剂与水相体积比为0.4时,6-APA的萃取率最高可达56.96%。对反萃过程的研究表明,使用p H=1的盐酸反萃液,反萃相与萃取相体积比为0.4时,反萃率最高可达51.42%。三级萃取和反萃取后,总的萃取和反萃率可达95%以上,络合剂可循环再生使用7次以上而不影响萃取和反萃效果,大大降低了操作成本。经络合萃取处理后的废液中6-APA质量分数大大降低,实现了经济和环保效益的双赢。     

Extraction and separation of molybdenum(VI) from acidic media by fatty hydrazides

BACKGROUND: The increasing demand for molybdenum has encouraged the development of low‐cost and environmentally friendly extractants to recycle and recover this metal. In the present study, solvent extraction of Mo(VI) from acidic media using a mixture of fatty hydrazides synthesised from palm olein as the extractant was carried out. The effects of various parameters such as acid, diluent, contact time, extractant concentration, metal ion concentration and stripping agent and the separation of Mo(VI) from other metal ions such as Co(II), Ni(II), Al(III) and Mn(II) were investigated. RESULTS: It was found that the extraction of Mo(VI) into the organic phase involved the formation of 1:3 complexes. Mo(VI) was successfully separated from commonly associated metal ions such as Ni(II), Co(II), Al(III) and Mn(II). Mo(VI) stripping from the loaded organic phase was studied using different acidic and alkaline solutions and was found to be optimal with ammonium hydroxide solution. CONCLUSION: These results are useful for the development of a method to recover Mo(VI) from acidic media utilising fatty hydrazides as the extractant. Copyright © 2008 Society of Chemical Industry     

Liquid-Liquid Extraction Studies of Trivalent Yttrium from Phosphoric Acid Solutions Using TOPS 99 as an Extractant

Liquid-liquid extraction studies of trivalent yttrium (Y) from phosphoric acid solutions have been carried out with commercial organophosphoric acid based extractant TOPS 99 (Talcher Organo phosphorus solvent, an equivalent of di-2-ethylhexyl phosphoric acid). The parameters studied include equilibration time, acid concentration, extractant concentration, diluent, metal concentration, temperature, stripping, and regeneration of the extractant. Increase of phosphoric acid concentration in the range from 0.01 to 0.5 M on the extraction of trivalent Y with 6 × 10^?3 M TOPS 99 (Talcher Organo phosphorus solvent) decreases the percentage extraction, indicating the transfer of metal follows ion exchange type reaction. The plot of log D vs. equilibrium pH gave a straight line with a slope of 3.1 indicating the exchange of three moles of hydrogen ions for every mole of trivalent Y extracted into the organic phase. Stripping of metal from the loaded organic with mineral acids indicate sulphuric acid as the best stripping agent. The extraction behavior of associated elements clearly follows their ionic radii with a maximum separation factor of 414 for Lu-Tb.     

应用[Omim][BF_4]为萃取剂分离钒铬渣酸浸液中钒/铬的研究

离子液体是一种新型绿色溶剂,在重金属离子萃取分离方面较传统的有机物质有显著的优势,但其成本昂贵是制约其作为溶剂应用的重要瓶颈,将其作为重要萃取剂是其扩大应用的一种有效途径。研究了1-辛基-3-甲基咪唑四氟硼酸盐离子液体([Omim][BF_4])萃取分离V(Ⅴ)、Cr(Ⅲ)的影响因素,包括相比(O/A)、时间、温度及金属离子初始质量浓度。结果表明,[Omim][BF_4]对于钒铬渣酸浸液中的V(Ⅴ)具有较好的萃取选择性,而对于Cr(Ⅲ)的萃取能力较弱,可以用于钒铬分离,为钒铬渣的绿色资源化利用开辟了新的途径。     

Where is the Anion Extraction Going?

Reactive extraction processes represent efficient and smart technologies for separation and concentration of metal ions in solution, which are frequently used in industry. Despite the importance of anions in biology, medicine, environment and industry, practical examples of anion extraction are relatively limited compared to metal ion separation. Anion extraction processes are mainly based on the nonspecific ion pair formation with hydrophobic ammonium cations. In this case the phase transfer of anions is dominated by their lipophilicity. The reasons for this situation are closely connected with the specific features of anions in contrast to cations. Novel approaches for specific binding and selective transport of anionic components are based both on the better understanding of the biological role of anions and on the possibilities of supramolecular chemistry to create receptor architectures with complementary binding modes for anions. In the given review the authors discuss present research tendencies and application possibilities of new extractant types for separation and concentration of anionic species in solution.     

离子液体体系用于盐湖卤水提取锂

3种咪唑类离子液体:1-丁基-3-甲基咪唑六氟磷酸盐([C₄mim][PF₆])、1-己基-3-甲基咪唑六氟磷酸盐([C₆mim][PF₆])、1-辛基-3-甲基咪唑六氟磷酸盐([C₈mim][PF₆])被作为绿色溶剂用于盐湖卤水分离镁锂, 建立了以离子液体(ILs)、磷酸三丁酯(TBP)分别为萃取介质和萃取剂的盐湖卤水锂萃取体系, 并与使用传统有机溶剂磺化煤油和氯仿的萃取效果进行了对比。研究发现, 该离子液体体系较使用传统挥发性有机溶剂的萃取体系有更高的萃取率。锂的萃取率随离子液体中烷基碳原子数的减小而增加。详细考察了溶液pH、离子液体浓度、相比对萃取效率的影响, 获得了离子液体体系萃取的最优条件。在最佳萃取条件下, 3种离子液体体系对锂的单级萃取效率均高于80%, 分离系数最高达到100以上。机理研究表明:离子液体体系是以阳离子交换实现对锂的萃取, Li⁺与TBP形成[Li·2TBP]⁺络合物进入有机相。     

磁性流体固定床萃取分离低浓度金离子

采用一种全新的快速萃取方法--磁性流体固定床萃取分离技术,该方法是将磁性Fe₃O₄纳米颗粒表面包覆油酸,溶于有机溶剂中,加入萃取剂三苯基氧化膦TPPO,制成磁性萃取剂。借助于高梯度磁性分离装置,对目标离子进行萃取分离。萃取完成后通过原子吸收光谱仪测定萃取后金溶液中Au³⁺的浓度。通过对铁磁导线直径、初始金溶液pH值、萃取剂体积分数和协同萃取等影响因素的考察,得出了对Au³⁺浓度为19.128 mg·L^-1的氯金酸溶液进行萃取分离的最佳工艺：采用直径为2.34 mm的铁磁导线作为磁性填充介质时萃取率较其他优越。初始金溶液的pH值和萃取剂的体积分数对萃取率影响较大。在初始金溶液pH=1,萃取剂(TPPO)体积分数达到50%时萃取率最高。使用TPPO和TBP协同萃取也能提高萃取率。采用浓度为1 mol·L^-1的硫脲进行反萃实验,振荡10 min,反萃率在90%以上。     

Grouping separation of mixed rare earths from their coexisting aqueous solutions by liquid-column elution

A new approach was proposed for grouping separation of 14 lanthanide rare-earth ions from their coexisting mixed aqueous solutions, by performing liquid-column elution using the aqueous solution containing 14 lanthanide rare-earth ions as the stationary phase and the dispersed organic oil droplets containing P507 extractant as the mobile phase. It was revealed that 14 lanthanide rare-earth ions could be separated into four groups, according to the lanthanide tetrad effect, respectively eluting out from the liquid column at different time in a certain order. Various effects including the saponification degree of P507, the concentration of P507 in organic phase, the length and inner diameter of the extraction column on the performance of grouping separation of rare-earth ions were discussed. The changes of the mass transfer coefficients were also investigated. The separation efficiency of the four groups of rareearth elements(REEs) was evaluated based on the elution resolution, Rs, of the elution peaks of La(Ⅲ),Gd(Ⅲ), Ho(Ⅲ) and Lu(Ⅲ), the four representative elements respectively from each of the four groups of REEs. Experimental results demonstrated that the separation of REEs by liquid-column elution mainly depended on the competitive adsorption of different rare-earth groups onto the surface of ascending P507 oil droplets. The affinity of different rare-earth groups with P507 extractant and a limited adsorption capacity of P507 molecules at the surface of the oil droplets ascending in liquid column play the important role. The present work highlights a promising technique for grouping separation of multiple lanthanide elements co-existing complex systems.     

溶剂油萃取深度脱芳烃实验

随着环保要求的日益严格和清洁燃料的需求增加,低芳烃含量溶剂油亦需进一步脱芳烃。液液萃取脱芳技术因具有操作条件缓和、萃取剂可循环利用、可得到芳烃副产品等优势被广泛应用,但针对低芳烃含量的原料,萃取剂的研发是关键问题。本实验采用N,N-二甲基甲酰胺（DMF）+乙二醇复合萃取剂萃取分离低浓度芳烃溶剂油体系,从萃取剂对甲苯的选择性系数（S）和分配系数（K）两方面出发优化了脱芳萃取剂配方,确定乙二醇质量分数为15%的复合萃取剂适用于萃取分离芳烃质量分数小于15%的低芳烃原料。测定了常压、40℃时 DMF-甲苯-正庚烷和复合萃取剂-甲苯-正庚烷体系的液液相平衡数据,并用Othmer-Tobias 方程对实验数据进行关联。相平衡数据证实了复合萃取剂更适用于低芳烃原料油脱芳。将优化的复合萃取剂用于溶剂油脱芳烃,实验结果表明在萃取温度40℃、萃取时间5min、分相时间10min、单级剂油质量比0.5的操作条件下,经7级错流萃取,溶剂油的芳烃质量分数可从9.15%降至0.76%,具有一定的工业应用前景。     

Ionic Liquids as Extraction Solvents: Where do We Stand?

Abstract

The unique physicochemical properties of ionic liquids (ILs) and the relative ease with which these properties can be fine‐tuned by altering the cationic or anionic moieties comprising the IL have led to intense interest in their use as alternatives to conventional organic solvents in a wide range of synthetic, catalytic, and electrochemical applications. Recent work by a number of investigators has been directed at the application of ionic liquids in various separation processes, among them the liquid‐liquid extraction of metal ions. Although certain IL‐extractant combinations have been shown to yield metal ion extraction efficiencies far greater than those obtained with molecular organic solvents, other work suggests that the utility of ILs may be limited by solubilization losses and difficulty in recovering extracted metal ions. In this report, recent efforts to overcome these limitations are described, and progress both in achieving an improved understanding of the fundamental aspects of metal ion transfer into ILs and in devising viable IL‐based systems for metal ion separation is detailed. In addition, areas upon which future research efforts might profitably be focused are identified.     

离子液体-磷酸三丁酯体系分离盐湖卤水镁锂

将一种典型的室温离子液体(ionic liquids, ILs)1-辛基-3-甲基咪唑六氟磷酸盐作为替代溶剂用于盐湖卤水萃取锂。在该萃取体系中, 离子液体和磷酸三丁酯(TBP)分别用作萃取介质和萃取剂。详细考察了水相酸度、相比等因素对锂分离效率的影响。初步结果表明:与传统萃取体系相比, 该离子液体萃取体系能极大提高萃取效率。该体系最优条件包括: TBP/ILs=9/1(体积比), 相比O/A=2:1, 水相的pH萃取前不需要调节。在此条件下, 锂和镁的单级萃取效率分别为80.64%和5.30%。经过三级逆流萃取, 锂的萃取率高达99.42%。在温度为80℃, 反萃相比A/O为2的条件下, 锂和镁的单级反萃效率分别为98.78%和99.15%。反萃水相中的镁锂比(Mg/Li)降至3.03, 与初始值相比降低了93.41%。