季铵盐(Aliquat 336)萃取对氨基苯磺酸的特性研究

利用季铵盐(Aliquat 336)为反应剂,在较宽的pH值条件下,研究了对氨基苯磺酸稀溶液的萃取相平衡特性;测定了反应剂浓度、稀释剂种类、盐的存在以及溶液pH值对反应萃取平衡分配系数的影响;提出了反应剂与对氨基苯磺酸负离子的阴离子交换反应机理,建立了平衡分配系数D值的表达式。结果表明,极性稀释剂不利于对氨基苯磺酸的萃取,惰性稀释剂能提供较大的萃取平衡分配系数,其顺序为:苯>四氯化碳>氯仿>正辛醇;盐的存在会降低Aliquat 336的萃取效率;与三烷基胺(Alamine 336)相比,Aliquat 336具有更宽的pH值适用范围。     

Aliquat 336萃取醋酸的平衡特性

选择Aliquat 336为萃取剂 ,氯仿、正辛醇和煤油为稀释剂 ,醋酸稀溶液为分离溶质 ,研究了稀释剂种类、反应剂浓度、水相 pH值、溶质在水相的浓度等因素对醋酸萃取分配系数的影响 ,分析了Aliquat 336萃取醋酸的机理 ,并在此基础上建立了描述萃取平衡的数学模型 .结果表明 :萃取结果基本符合反应剂与稀释剂的简单加和 ;稀释剂对萃取效果的影响显著 ,随Aliquat 336浓度的增大 ,氯仿和煤油为稀释剂时的萃取能力较正辛醇增加得快 ;随 pH值的变化D存在一个最大值 ,该值只与反应剂在有机相中的浓度有关 .Aliquat 336萃取醋酸存在阴离子交换和化学缔合两种机制 ,表观的阴离子交换反应平衡常数K₁在有稀释剂的条件下比纯反应剂时有所增大 ,其中氯仿的影响相对较大 ,表观的化学缔合反应平衡常数K₂ 在有稀释剂的条件下表现为 ,惰性稀释剂煤油对K₂ 的影响不明显 ,氯仿具有强化的作用 ,而正辛醇具有削弱Aliquat 336与醋酸化学缔合的能力 .     

膜萃取去除水中对氨基苯磺酸的研究

以特定混合物 (2 0 %TOA 30 %辛醇 50 %煤油 ) -对氨基苯磺酸 -水为实验体系 ,应用中空纤维膜萃取技术处理含对氨基苯磺酸的水溶液。研究了两相流速、溶液pH、初始浓度对传质性能的影响。结果表明 ,传质由水相侧阻力控制 ,在相比(有机相 /水相 )较小的情况下 ,可使初始质量浓度为 1 0 0 0mg/L的溶液降至 30mg/L ,证明了中空纤维萃取去除水中对氨基苯磺酸的高效性。     

季铵萃取分离钴、镍的生产性实验

在萃取分离钴、镍的基础上,根据串级模拟计算结果合理安排工艺流程,进行了与生产规模相当的生产性实验. 结果表明季铵氯化物萃取分离钴、镍的工艺可行, 稳定可靠, 经济合理. 对氯离子浓度较低的料液, 季铵比叔胺更优越, 特别适合从高镍低钴的低浓度氯化物介质中萃取分离钴、镍.     

三烷基胺(7301)络合萃取对氨基苯磺酸稀溶液

利用三烷基胺 (730 1 )为络合剂 ,在较宽的 pH值条件下实验测定了对氨基苯磺酸稀溶液的萃取相平衡分配系数 ;分析了络合剂浓度、稀释剂种类以及溶液 pH值对络合萃取相平衡分配系数的影响 ;讨论了络合剂萃取对氨基苯磺酸偶极离子的质子转移过程 ,提出了平衡分配系数D值的表达式 .     

对氨基苯磺酸催化合成阿司匹林

以水杨酸与乙酸酐为反应原料,采用对氨基苯磺酸为催化剂,合成了阿司匹林,分别讨论了反应原料摩尔比、催化剂对氨基苯磺酸的用量、反应时间和反应体系的温度对产物阿斯匹林收率的影响。结果表明：当水杨酸与乙酸酐摩尔比为1：3．5,催化剂对氨基苯磺酸用量为0．4g,反应时间为6min,反应温度为80—85℃时,阿斯匹林的收率可达到62．33％。     

对氨基苯磺酸催化合成水杨酸正丁酯

以正丁醇与水杨酸为原料,采用对氨基苯磺酸为催化剂,通过酯化反应合成了水杨酸正丁酯。考察了酸醇物质的量比、催化剂用量、反应时间对水杨酸正丁酯化收率的影响。结果表明,在回流条件下,当水杨酸的加入量0.20 mol,正丁醇的加入量0.32 mol,即酸与醇物质的量比为1∶1.6,催化剂对氨基苯磺酸用量为0.70 g(相当于5%的酸),反应4.0 h时,水杨酸正丁酯收率可达到72.90%。     

甲基橙萃取分光光度法分析季铵酯类农药

研究了季铵酯类农药的甲基橙萃取分光光度分析法，它灵敏、简便，快速，在２５ｍｌ中农药含量１０￣７０μｇ范围内符合光吸收定律，其摩尔吸光系数ε为３．１×１０＾４ｌ·ｃｍ＾－１·ｍｏｌ＾－１。     

对氨基苯磺酸的微波合成

采用微波加热方法,用苯胺与浓硫酸反应生成对氨基苯磺酸。实验中分别从微波输出功率、微波辐射时间和投料比三个因素进行实验条件探讨,得出最佳的微波合成条件为:苯胺与浓硫酸两者的物质的量之比为1∶3,微波辐射功率为130W,微波加热时间12min。与传统加热方法合成对氨基苯磺酸对比后可知,微波辐射下反应速率至少是常规反应速率的30倍。     

Extraction of protactinium from acid media using Aliquat 336

Solvent extraction studies on protactinium were carried out from hydrofluoric acid, hydrochloric acid, and a mixture of hydrochloric and hydrofluoric acids using Aliquat 336 and ²³¹Pa. The extraction of protactinium from hydrofluoric acid (0.025–10 M) decreased with increasing acid concentration and was less than 10% above 5 M. The extraction from hydrochloric acid (0.5–8 M) started only above 4 M and increased with increasing acid concentration. The extraction of protactinium from a mixture containing hydrochloric acid (0.5–8 M) and 0.03 M hydrofluoric acid decreased with increasing acid concentration reached to a minimum at about 2 M and then increased with increasing acid concentration. At low acidity, extraction of protactinium from hydrofluoric acid was higher compared to hydrochloric acid and the mixture of hydrochloric and hydrofluoric acids. Nitric acid (10 M) and hydrofluoric acid (10 M) were suitable for quantitative recovery of protactinium from organic phase. The extraction of ²³¹Pa from real thorium lean raffinate of thorium–uranium extraction process was studied using optimized extraction conditions.     

Zirconium and Hafnium Separation,Part 1. Liquid/Liquid Extraction in Hydrochloric Acid Aqueous Solution with Aliquat 336

Abstract

The extraction of zirconium and hafnium from aqueous HCl solutions by means of Aliquat 336 in organic diluents was systematically studied. The following three aspects were discussed: the extraction dependence on HCl, the Aliquat 336 concentrations, and the nature of diluents. Both of the metals were stripped with deionized water and the influence of phase ratio on the efficiency of the stripping has been investigated. The stoichiometry of the extracted Zr and Hf species from single metal ion were studied and a possible extraction mechanism for the Zr‐Hf mixture is discussed in the light of the results obtained.     

Equilibrium and kinetic studies of the extraction of chelated copper(II) anions with Aliquat 336

The equilibrium and kinetics of solvent extraction of Cu²⁺ from aqueous solutions containing equimolar EDTA with Aliquat 336 in n‐decanol and kerosene at 298 K were investigated. The concentrations of Cu²⁺ (8–50 mol m^?3), Cl^? (5–60 mol m^?3), and Aliquat 336 (20–100 mol m^?3) were varied. A semi‐empirical model with three parameters was proposed to describe the equilibrium behavior, in which the non‐idealities in both aqueous and organic phases were considered. Over the ranges studied, the model agreed reasonably well with the experimental data (standard deviation, 15%). The forward and backward reaction rate constants were determined as (5.31 ± 0.16)×10^?6 m^9/4 mol^?3/4 s^?1 and (2.62 ± 0.09)×10^?7 s^?1, respectively, at 298 K. An interfacial reaction mechanism was proposed, which revealed that the reaction between the chelated anions and trimeric amine molecules at the interface was rate limiting. The derived rate laws were consistent with the experimental results. © 2002 Society of Chemical Industry     

Extraction of toluene and n-heptane mixture using ionic liquid Aliquat 336 and mathematical modeling for solvent selection

Liquid–liquid equilibrium data for the system consisting of toluene, n-heptane and Aliquat 336 ionic liquid was obtained at 303.15 K and atmospheric pressure. The values of distribution coefficient and selectivity were evaluated. Mathematical model relating distribution coefficient and dispersion, dipolar interaction and hydrogen bonding has been developed. Hansen’s solubility parameters were used to determine the parameters. The model was applied for various ionic liquids as solvents. The model predicted the trends similar to the trend reported in the literature. Thus model can predict better solvent for the given extraction application. This methodology has great potential to act as a knowledge-based framework to aid development of new tailor-made solvents. This will save cost and time in experimentation and analysis.     

Extraction and separation of Pt(IV)/Rh(III) from acidic chloride solutions using Aliquat 336

Extraction and separation of Pt(IV)/Rh(III) from chloride solutions using Aliquat 336 (Quaternary ammonium salt made by the methylation of mixed tri octyl/decyl amine) diluted in kerosene as an extractant/synergist alone and mixed with organophosphorous extractants as synergists/extractants were carried out from an aqueous feed containing 0.0005 mol L⁻¹ Pt(IV)/Rh(III).Variation of hydrochloric acid concentration of aqueous phase from 0.005 to 10.0 mol L⁻¹ increased the percentage extraction of platinum up to 5.0 mol L⁻¹ there after it decreases. Whereas in the case of rhodium, from 0.005 to 1.0 mol L⁻¹ acid range the percentage extraction was decreased from 1.0 to 10.0 mol L⁻¹ acid range is favorable for extraction. Platinum(IV)/rhodium(III) separation factor of 279.2 was obtained at 1.0 mol L⁻¹ HCl concentration with 0.005 mol L⁻¹ Aliquat 336 and separation factor of 612.3 was obtained at 3.0 mol L⁻¹ HCl concentration with 0.01 mol L⁻¹ Aliquat 336. The present study optimized the various experimental parameters like phase contact time, effect of extractant, salts, temperature, loading capacity of extractant, stripping studies with various mineral acids/bases, recycling and reusing capacity of extractant up to ten cycles.     

Parametric optimization of green synergistic reactive extraction of lactic acid using trioctylamine,Aliquat336, and butan-2-ol in sunflower oil by response surface methodology

A novel green synergistic reactive extraction technique for the removal of lactic acid (LA) from aqueous solution was explored. Response surface methodology (RSM) was applied to optimize the process variables for LA synergistic reactive extraction using a mixture of trioctylamine and Aliquat336 as extractants. During this present investigation, 2-butanol and sunflower oil were used as organic and green diluent. Systematic investigation has been carried out to obtain the optimum process conditions viz. initial LA concentration, pH of aqueous solution, extractant ratio, extractant concentration, solvent ratio, phase ratio, temperature, stirring speed, and contact time for maximizing the LA distribution coefficient (K_D) and extraction efficiency (%, η). The highest experimentally achievable LA distribution coefficient (K_D) and extraction efficiency (%) at optimized process conditions were found to be in close agreement with those predicted by numerical optimization using RSM. Thus, the results of present finding have been shown a great ability of sunflower oil as an economic and environmentally friendly green solvent for LA extraction.     

Simple Method for High-Density Impregnation of Aliquat 336 onto Porous Sheet and Binding Performance of Resulting Sheet for Palladium Ions

Aliquat 336 was impregnated onto the polymer chain grafted onto a 2.0-mm-thick porous sheet with a porosity of 75% and a pore size of 1.2 µm via the graft polymerization of glycidyl methacrylate and the subsequent reaction of the epoxy group with mercaptoundecanoic acid. In a 2:1 ethanol/4M NaOH (v/v) mixture, Aliquat 336 was impregnated at a density of 0.85 mmol/g, which was comparable to that of conventional Aliquat-336-impregnated polymeric beads. The dynamic binding capacity for palladium was 0.60 mmol/g when 100 mg-Pd/L palladium chloride solution was forced to permeate at a space velocity of 3700 h^?1.     

Adsorption of rhenium and rhodium in nitric acid solution by Amberlite XAD-4 impregnated with Aliquat 336

An Extractant Impregnated Resin (EIR) was prepared by impregnation of Aliquat 336 into Amberlite XAD-4 for tentative separation of rhenium from rhodium in nitric acid solution. An optimum loading ratio of the XAD-4 resin for Aliquat 336 was found to be about 0.4 (g Aliquat 336/g resin). The prepared EIR showed high preference for rhenium over rhodium and adsorption isotherms for rhenium were described well by Langmuir equation in both the single and multi-component systems. Maximum adsorption capacities obtained by modeling the isotherms of rhenium were 2.01 and 1.97 meq/g for the single and the multi-component systems, respectively. On the other hand, only little adsorption of rhodium ions was observed. The homogeneous model fitted the kinetic data quite well and the obtained effective diffusivities of rhenium and rhodium ions were on the order of 10^-7 and 10^-6 cm² min^-1, respectively.