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JOM · 2018 ·Vol. 70 ·期 12 ·2837-2845 · IF 2.145

Extraction Separation of Sc(III) and Fe(III) from a Strongly Acidic and Highly Concentrated Ferric Solution by D2EHPA/TBP

Zhang Weiguang,Zhang Ting-An,Lv Guozhi,Zhou Weihua,Cao Xuejiao,Zhu Hangyu

The solvent extraction and separation process of Sc(III) and Fe(III) from a strongly acidic and highly concentrated ferric solution using mixtures of di(2-ethylhexyl) phosphate (D2EHPA) and tri-n-butyl phosphate (TBP) in sulfonated kerosene was studied. The effects of various parameters, including D2EHPA concentration, dosage of TBP, and phase ratio, were investigated for the extraction process. The results indicated that the extraction rate of Sc(III) was 99.72% with 1.09% Fe(III) co-extracted after two stages of counter-current extraction under optimal conditions. Moreover, saturation capacity and slope analysis were used to determine the reaction mechanism. Sc(III) is extracted in the form of HSc(SO 4 ) 2 ·4HL. Further separation of Sc(III) and Fe(III) was realized in a scrubbing and stripping process. First, 98.67% of the co-extracted iron in the loaded organic phase was scrubbed with a dilute HCl solution by a three-stage counter-current scrubbing. Then, 85.00% of Sc(III) can be stripped efficiently with a 2-mol/L NaOH solution saturated in 1-mol/L NaCl by three-stage cross-current stripping.

CAS / MDL: 12060-08-1
研究领域: 化学工程 · 分析化学 · 环境科学
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CHEMICAL ENGINEERING SCIENCE · 2017 · IF 2.895

Modeling multiple chemical equilibrium in chiral extraction of metoprolol enantiomers from single-stage extraction to fractional extraction

Panliang Zhang,Shichuan Wang,Kewen Tang,Weifeng Xu,Fan He,Yunren Qiu

Enantioselective extraction of metoprolol (MT) enantiomers with di-cyclohexyl (D)-tartrate (DT) and boric acid (BA) as chiral extractant was performed. The process involving multiple chemical equilibrium is very complicated and the process optimization is difficult. On the basis of an interfacial reaction mechanism, a single-stage extraction model was established. The operation conditions of pH and DT to BA ratio were obtained through simulation and optimization of the equilibrium of the two phase extraction system. Based on the single-stage extraction model and the law of mass conservation, a fractional extraction model was established to simulate and optimize the fractional extraction process. To pursue a high productivity and reduce the required stages, a high feed to aqueous phase ratio (F/W = 1) and an asymmetric separation mode were applied. By asymmetric separation where the optical purity of the product in extract phase and raffiniate phase is not equal, enantiomeric excess ( ee ) value for the eutomer of MT can reach up to 98.64% and yield can reach up to 64.68% with 20 extraction stages.

CAS / MDL: 87-69-4
研究领域: 化学工程 · 制药工程
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INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH · 2023 · IF 4.2

Continuous Counter-Current Multistage Microextraction in a Novel Tube-In-Tube Microextractor

Junxin Chen,Caijin Zhou,Bingqi Xie,Jisong Zhang

Counter-current operation has been widely applied to enhance the extraction efficiency for systems with low distribution coefficients, which was hindered in microextraction because viscous force and surface tension dominate over gravity and inertial force. In this study, a novel design of a tube-in-tube microextractor relying on a poly tetra fluoroethylene membrane to construct a stable interface was proposed to conduct continuous counter-current extraction. Extraction kinetics for two systems with different distribution coefficients, membranes with different pore radii, and three flow rate ratios were measured as a function of residence time. For the system that toluene was used to extract 0.06 wt % phenol in water, 4.1 stages of extraction efficiency were achieved at a residence time of 9.8 min. A challenging case study (50 wt % acetone–water–toluene) was subsequently conducted to prove the high applicability for emulsion systems of this special microextractor. Lastly, a mathematical model was established and the predicted results of three flow rate ratios are in good agreement with experimental results.

CAS / MDL: 108-95-2
研究领域: 化学工程 · 分析化学
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MOLECULES · 2019 ·Vol. 24 ·期 3 ·442 · IF 3.06

Comparison of the Partition Efficiencies of Multiple Phenolic Compounds Contained in Propolis in Different Modes of Acetonitrile–Water-Based Homogenous Liquid–Liquid Extraction

Wenbin Chen,Xijuan Tu,Dehui Wu,Zhaosheng Gao,Siyuan Wu,Shaokang Huang

Homogeneous liquid–liquid extraction (HLLE) has attracted considerable interest in the sample preparation of multi-analyte analysis. In this study, HLLEs of multiple phenolic compounds in propolis, a polyphenol-enriched resinous substance collected by honeybees, were performed for improving the understanding of the differences in partition efficiencies in four acetonitrile–water-based HLLE methods, including salting-out assisted liquid–liquid extraction (SALLE), sugaring-out assisted liquid–liquid extraction (SULLE), hydrophobic-solvent assisted liquid–liquid extraction (HSLLE), and subzero-temperature assisted liquid–liquid extraction (STLLE). Phenolic compounds were separated in reversed-phase HPLC, and the partition efficiencies in different experimental conditions were evaluated. Results showed that less-polar phenolic compounds (kaempferol and caffeic acid phenethyl ester) were highly efficiently partitioned into the upper acetonitrile (ACN) phase in all four HLLE methods. For more-polar phenolic compounds (caffeic acid,p-coumaric acid, isoferulic acid, dimethoxycinnamic acid, and cinnamic acid), increasing the concentration of ACN in the ACN–H2O mixture could dramatically improve the partition efficiency. Moreover, results indicated that NaCl-based SALLE, HSLLE, and STLLE with ACN concentrations of 50:50 (ACN:H2O,v/v) could be used for the selective extraction of low-polarity phenolic compounds. MgSO4-based SALLE in the 50:50 ACN–H2O mixture (ACN:H2O,v/v) and the NaCl-based SALLE, SULLE, and STLLE with ACN concentrations of 70:30 (ACN:H2O,v/v) could be used as general extraction methods for multiple phenolic compounds.Keywords:salting-out assisted liquid–liquid extraction;sugaring-out assisted liquid–liquid extraction;hydrophobic-solvent assisted liquid–liquid extraction;subzero-temperature assisted liquid–liquid extraction;phenolic compounds

研究领域: 分析化学 · 植物化学
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Journal of Environmental Chemical Engineering · 2024 · IF 7.4

Uranium extraction by a bifunctional extractant dialkyl (2-(hydroxyamino)-2-oxoethyl) phosphonate

Mengjia Hu,Jingjing Xiao,Hongqing Wang,Chen Yao,Yaxin Wu,Zhihong Xiao,Changzhu Li

In this paper, a novel bifunctional molecule dialkyl (2-(hydroxyamino)-2-oxoethyl) phosphonate (DAHAOEP) containing both phosphoryl and hydroxamic groups was designed and synthesized, and used as a uranium extractant. The extraction properties of DAHAOEP were focused. Dihexyl (2-(hydroxyamino)-2-oxoethyl) phosphonate (DHHAOEP) was shown to have a better extraction effect on uranyl ions than dibutyl (2-(hydroxyamino)-2-oxoethyl) phosphonate (DBHAOEP) and diethyl (2-(hydroxyamino)-2-oxoethyl) phosphonate (DEHAOEP). Under the optimal extraction conditions, the extraction efficiency of DHHAOEP on uranyl ions could reach up to 98 %. Extraction saturation capacity, reusability and selectivity results indicated that the saturation capacity of DHHAOEP continuous extraction can reach 596 % after 10 times of extraction, DHHAOEP had been recycled more than 5 times, and exhibited a superior selectivity for uranyl ions. Slope method showed that DHHAOEP mainly coordinated with uranyl ions in a 1:2 coordination, i.e., monomolecular bidentate coordination M 2 L. FTIR and XPS analysis further confirmed that DHHAOEP combined with uranyl ions through it’s -C(=O)-NHOH and P = O groups to form a five-membered ring and P-O-U configuration, respectively.

研究领域: 化学 · 环境科学
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JOURNAL OF CHROMATOGRAPHY A · 2012 · IF 4.531

Dispersive microextraction based on water-coated Fe3O4 followed by gas chromatography–mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils

Qin Zhao,Fang Wei,Neng Xiao,Qiong-Wei Yu,Bi-Feng Yuan,Yu-Qi Feng

In the present work, we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction (LPME) and magnetic solid-phase extraction (MSPE). In this method, trace amount of water directly absorbed on bare Fe 3 O 4 to form water-coated Fe 3 O 4 (W-Fe 3 O 4 ) and rapid extraction can be achieved while W-Fe 3 O 4 dispersed in the sample solution. The analyte adsorbed W-Fe 3 O 4 can be easily collected and isolated from sample solution by application of a magnet. It was worth noting that in the proposed method water was used as extractant and Fe 3 O 4 served as the supporter and retriever of water. The performance of the method was evaluated by extraction of 3-monochloropropane-1,2-diol (3-MCPD) from edible oils. The extracted 3-MCPD was then derived by a silylanization reagent (1-trimethylsilylimidazole) before gas chromatography–mass spectrometry (GC–MS) analysis. Several parameters that affected the extraction and derivatization efficiency were investigated. Our results showed that the limit of detection for 3-MCPD was 1.1   ng/g. The recoveries in spiked oil samples were in the range of 70.0–104.9% with the RSDs less than 5.6% (intra-day) and 6.4% (inter-day). Taken together, the simple, rapid and cost-effective method developed in current study, offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples.

研究领域: 分析化学 · 食品科学
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Analytical Methods · 2014 ·Vol. 7 ·期 2 ·560-565 · IF 1.938

Centrifugal microextraction tube-cloud point extraction coupled with gas chromatography for simultaneous determination of six phthalate esters in mineral water

Yun-Kai Lv,Wei Zhang,Meng-Meng Guo,Fang-Fang Zhao,Xiao-Xue Du

A home-made centrifugal microextraction tube (CMET) was developed and applied to cloud point extraction coupled with microwave-assisted back extraction and gas chromatographic separation of six phthalate esters (PAEs) from mineral water. All phthalate esters were entrapped in the micelles of the non-ionic surfactant Triton X-114 and removed from the bulk phase by centrifugation. The obtained surfactant-rich phase was treated with water-immiscible solvents, and the target analytes were back extracted by short-term microwave application and determined by GC-FID directly. The whole process was finished in the CMET. The proposed method demonstrated good performance concerning linearity (R2 = 0.9977-0.9998), precision (2.3–5.7%), the limits of detection and quantitation (LOD, 11.5-19.3 μg L−1; LOQ, 37.0-63.3 μg L−1), spiked recoveries (89.1–96.3%) and enrichment factor (71-85). The proposed method was successfully applied for the determination of trace amount of phthalate esters in mineral water. DBP and BBP were found in actual mineral water samples.

研究领域: 分析化学 · 环境毒理学 · 食品安全 · 分子监测 · 样品前处理
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Chemical Engineering and Processing-Process Intensification · 2022 · IF 4.264

Back extraction combined with magnetic solid phase extraction based on bubble column for separation and purification of juglone from Juglans mandshurica Maxim. coproducts

Mengfei Tian,Xianming Meng,Naveed Ahmad,Chunying Li,Zhanyu Yuan,Zidan Luo,Yu Zhang,Chunyu Liang,Chunjian Zhao

Juglone was first preliminary purified by back extraction (BE) which also completed the sustainability of microemulsion as a solvent for extraction of juglone in J. mandshurica Maxim. branches. Then, magnetic solid phase extraction (MSPE) based on bubble column (BC) was proposed to further purify the juglone, GO/ND/Fe 3 O 4 as adsorbent, which broke through the limitation that MSPE is only suitable for trace enrichment. Thus, a BE combined with MSPE based on BC (BE-MSPE/BC) technology to separate and purify juglone from J. mandshurica Maxim. was developed. Under the optimal conditions (optimal adsorption conditions: 0.5 h of adsorption time, 30 mg/mL of solid-liquid ratio, 5.5 of pH, 60 L/min of air flow; optimal desorption conditions: 0.4 h of desorption time, methanol of desorption agent, 100% of desorbent volume fraction, 8 of pH, 40 mg/mL of solid-liquid ratio, 80 L/min of air flow rate), the recovery yield and purity of juglone obtained by BE-MSPE/BC were 80.57% and 72.38%, respectively. BE-MSPE/BC, as a green separation and purification technology that can easily achieve large-scale and sustainable production, is expected to be an alternative method to separate and purify active components in biomass materials and products.

CAS / MDL: 481-39-0
研究领域: 植物化学 · 分析化学 · 环境科学
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MINERALS ENGINEERING · 2023 · IF 4.8

Novel octanethioic acid alkyl amide extractants: Synthesis, their highly selective separation for palladium, and the extraction mechanism from chloride media

Junlian Wang,Lu Liu,Guodong Xu,Fan Li

Highly selective extraction of Pd from leaching liquor of spent auto-catalysts is a research hotspot in recent years. In this study, three novel octanethioic acid alkyl amide extractants (alkyl = butyl TA-804, hexyl TA-806 and 2-ethylhexyl TA-826) were designed, synthesized and characterized by 1 H NMR, FT-IR and ESI-HRMS. The effect of contact time, extractant concentration, HCl concentration and diluents on Pd selective extraction and separation by these three extractants were investigated. The stripping behaviors of the loaded Pd in the organic phase were examined. The McCabe-Thiele diagrams of Pd extraction and stripping were drawn. The extraction mechanism was studied through methods of stoichiometry calculation, slope analysis, FT-IR and ESI-HRMS. In the end, the Pd separation from simulated leaching liquor of spent auto-catalysts by TA-804, TA-806 and TA-826 was carried out. The results show TA-826 has much slow Pd extraction kinetics than TA-804 and TA-806. They all have highly efficient extraction and separation performance for Pd from chloride media at acidities of [HCl] ≤ 3 mol/L. When the HCl concentration is ≥4 mol/L, Fe and Pt begin to be extracted. At any acidities, Rh, Zn, Al, La, Zr, Co, Cu, Ni, Ce and Mg are not extracted. The studied octanethioic acid alkyl amides extract Pd from chloride media via complexation mechanism. Two extractant molecules quantitatively extract one Pd. The loaded Pd are easily and efficiently stripped by thiourea. They can efficiently extract and highly separate Pd from leaching liquor of spent auto-catalysts at acidity of 3 mol/L HCl.

CAS / MDL: 8008-20-6 124-07-2
研究领域: 化学工程 · 无机化学 · 材料科学
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JOURNAL OF HAZARDOUS MATERIALS · 2024 · IF 12.2

Efficient extraction of nickel from chloride system using a cleaner extractant: Taking the example of processing nickel-aluminum slag remaining from spent hydroprocessing catalysts

Yunhui Li,Yixiong Chen,Jialin Qing,Zuoying Cao,Shengxi Wu,Qinggang Li,Mingyu Wang,Wenjuan Guan,Guiqing Zhang

The efficient recovery of nickel from chloride systems has long presented a challenge in the field. While solvent extraction is a viable approach, conventional extractants have been associated with drawbacks such as a high requirement for chloride ions and substantial consumption of acids and alkalis. In response to these challenges, this investigation developed and synthesized a novel thiazole-based extractant, N, N-Bis(4-thiazolylmethyl)octylamine (NNBT), tailored for the selective extraction of nickel from chloride systems. Findings from the study indicate that the nitrogen atom situated on the benzylamine framework within NNBT can interact synergistically with the chelating thiazole ring, facilitating effective nickel extraction and notably reducing the need for chloride ions. Furthermore, the extractant can be regenerated using deionized water , thereby obviating the necessity for additional consumption of acids and alkalis. Following the validation of NNBT as an environmentally sustainable and efficient nickel extractant within the chloride ion system, it was successfully employed to selectively and effectively extract nickel from the nickel-aluminum slag of spent HDP catalyst. The extracted nickel and aluminum were subsequently processed into electroplated nickel chloride and polyaluminum chloride, respectively, meeting the national standards of China. These outcomes underscore the eco-friendliness and promise of NNBT for nickel extraction from chloride systems.

研究领域: 冶金工程 · 环境科学
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INORGANICA CHIMICA ACTA · 2025 · IF 3.2

Solvent extraction of TODGA in the presence of phase modifiers of TBP, n-octanol, and DHOA dissolved in n-dodecane: Thermodynamics, kinetics and aggregation studies

Xingyue Liu,Xuanhao Huang,Yiting Wang,Zhuang Wang,Qiao Yu,Hang Zhou,Rui Li,Songdong Ding

Tri- n -butyl phosphate (TBP), n -octanol and N,N -dihexyloctanamide (DHOA) are often used as phase modifiers to prevent the formation of the third phase during the extraction of trivalent lanthanides and actinides by N,N,N′,N′ -tetraoctyl diglycolamide (TODGA) in spent fuel reprocessing process. In this context, the effects of these three modifiers on the thermodynamic and kinetic behaviors of 0.20 mol·L −1 TODGA in n -dodecane toward Nd 3+ in nitric acid solution were studied and compared together for the first time. A systematic comparison of the effects of the three modifiers on the extraction distribution ratio, stripping percentage, loading capacity, aggregation and extraction kinetics was carried out with the aim of selecting a phase modifier for the TODGA-based process that would work optimally and to elucidate the impact of the modifiers in the TODGA extraction system. It is found that modifier reduces the capacity of TODGA to extract Nd 3+ in the order of DHOA > TBP >  n -octanol, slightly hinders the stripping of Nd 3+ , while significantly enhancing the loading capacity of TODGA. With increasing the modifier concentration, the limiting organic phase concentration (LOC) for Nd 3+ increases. At the modifier concentration below 0.30 mol·L −1 , n -octanol has the greatest promotion effect on the LOC value, while at that above 0.50 mol·L −1 , TBP has the best effect. Meanwhile, through the dynamic light scattering analysis for the loaded organic phase, it is also found that the particle size of the aggregates in organic phase decreases significantly upon the addition of modifier. Furthermore, the extraction kinetics studies in a Lewis cell indicate that the addition of modifier can prolong the time to reach extraction equilibrium, and decrease the extraction rate. Although the modifier also exerts some influence on the reaction order and extraction rate constant to some extent, it does not alter the underlying regime of the extraction reaction.

研究领域: 化学工程 · 核燃料循环与材料科学
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JOURNAL OF RARE EARTHS · 2021 · IF 3.712

Solvent extraction and separation of light rare earths from chloride media using HDEHP-P350 system

Wenjie Zhang,Dongxia Feng,Xian Xie,Xiong Tong,Yunpeng Du,Yang Cao

Solvent extraction is the most important method for rare earth extraction and separation. Currently, di(2-ethylhexyl) phosphoric acid (HDEHP) and 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HEH/EHP) are widely used in industrial production, but there are still obvious deficiencies that require further research to resolve. In this paper, the unsaponification extraction of light rare earth ions in a hydrochloric acid medium by di(2-ethylhexyl) phosphoric acid-di(1-methyl-heptyl) methyl phosphonate (HDEHP-P350) system was studied. The results show that the addition of P350 reduces the extraction capacity of HDEHP, and also greatly reduces the concentration of acidity required for the back-extraction. It still has a good separation factor for light rare earths without saponification , and the extractant is not easy to emulsify. With an aqueous phase of pH = 2.85, and HDEHP mole fraction X HDEHP  = 0.9 (compared with O/A = 2), the separation effect of light rare earth is the best, resulting in the separation coefficient β Ce/La  = 3.39, β Pr/Ce  = 1.67 and β Nd/Pr  = 1.45, respectively. The loaded light rare earth ions extracted by HDEHP-P350 can be easily stripped when 2 mol/L HCl is used as the stripping agent. Finally, the extraction mechanism is discussed using a slope method, and the final structure of the extracted complex is determined to be RECl[(DEHP) 2 ] 2 P350 (o) , based on a combination of infrared spectra and 1 H NMR and 31 P NMR analyses.

研究领域: 化学工程 · 材料科学
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