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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2017 ·Vol. 314 ·期 1 ·59-67 · IF 1.282

Highly selective extraction of Pd(II) with 5-octyloxymethyl-7-bromo-8-quinolinol from acidic solution

Liu Zhanxiang,Dong Yang,Liao Jiali,Li Xingliang,Yang Jijun,Yang Yuanyou,Luo Shunzhong,Liu Ning

A novel extractant, 5-octyloxymethyl-7-bromo-8-quinolinol (HBrO 8 Q), was employed to extract Pd(II) from low-acidity aqueous solution. The extraction behaviors indicated that HBrO 8 Q had high extraction efficiency and selectivity for Pd(II) under the experimental conditions, and the stoichiometry of Pd(II) with HBrO 8 Q was found to be 1:1 by means of mole ratio method and Job’s method. The thermodynamic study indicated that the extraction process was endothermic and spontaneous. Additionally, complete back extraction of palladium could be achieved by using acidic thiourea solution.

研究领域: 化学 · 环境科学
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Journal of the Iranian Chemical Society · 2023 ·Vol. 20 ·期 11 ·2861-2870 · IF 2.4

Three-dimensional self-assembled reduced graphene oxide composite as a promising adsorbent for the collection of palladium (II) and platinum (IV) in a low concentration

Chen Lei,Li Yuan-Long,Li Rong-Xin,Shu Qi-Jiang,Yang Tao

A three-dimensional reduced graphene oxide aerogel modified by sulfamic acid and ethylenediamine was prepared via one-step reduction self-assembly under atmospheric pressure within 90 °C heating constantly. The adsorption efficiency of palladium (II) was ~ 97.0% at pH 11 within 50 min by the prepared composite. While the composite exhibited adsorption for platinum (IV) at acid condition, giving a rising to an adsorption efficiency was 61.7% at pH 5. Only 25.8% adsorption efficiency of platinum (IV) was found at pH 11, and 17.0% adsorption efficiency of palladium (II) was obtained at pH 5. The adsorption capacity of the composite for palladium (II) was 80 μg mg −1 above, and the adsorption capacity of the composite for platinum (IV) was ~ 160 μg mg −1 . The obtained palladium (II) and platinum (IV) can be eluted by urea and surfactant from the surface of the composite, respectively. Understanding the mechanism of the adsorption/desorption between palladium (II)/platinum (IV) and the composite, explored a promising way for recycling and enrichment of noble metal at a low concentration.

研究领域: 材料科学 · 环境科学
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ACS Applied Materials & Interfaces · 2020 · IF 8.758

The Immobilization of Pd(II) on Porous Organic Polymers for Semihydrogenation of Terminal Alkynes

Jianguo Liu,Nan Wang,Jianan Liu,Ming Li,Ying Xu,Chenguang Wang,Yanzhi Wang,Haoquan Zheng,Longlong Ma

Highly selective catalytic hydrogenation of alkynes to alkenes is a highly important reaction owing to its industrial and commercial application. Specifically, semihydrogenation of terminal alkynes has been more challenging than internal alkenes even using Lindlar catalysts. Also, the high reduction degree state metal-supported catalysts like Pd0/C, Pt0/C, and Ru0/C have been well-known to be used widely in hydrogenation due to their super activity. However, charcoal can absorb a large amount of water; Pd/C with 50% water is convenient on a large-scale synthesis. Charcoal generally bears oxygen groups on its surface, which are responsible for low selectivity and undesired products. Even typically, only 10–60% of the Pd metal atoms are exposed, they still suffer from poor stability in acids owing to leaching. Herein, we intend to design active and stable metal catalysts with features as the following to avoid leaching: having strong interaction with the support and coordinatively unsaturated metal sites or low valence state metals physically isolated from the acid environment. Herein, a highly efficient semihydrogenation of terminal alkynes to produce alkenes has been realized using a heterogeneous Pd(II)/POP-GIEC catalyst, imine-linked, crystalline, and porous organic polymer supporter modified by coordination of Pd(OAc)2 to its walls under mild conditions. Surprisingly, for the first time, modified POP-supported low reduction degree PdII catalysts were synthesized efficiently, and they were successfully used in semihydrogenation of terminal alkynes. The substrate scope was studied and included both unfunctionalized as well as functionalized substituents on the para, ortho, and meta position of aromatic alkynes. The substrate having a substituent with the functionality of fluoro protected at the meta position was semihydrogenated with a high alkyne conversion of 100% and olefin selectivity (up to 99%).

CAS / MDL: 64-17-5 67-68-5 123-91-1
研究领域: 催化化学 · 材料科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2019 · IF 5.107

Stable, regenerable and 3D macroporous Pd (II)-imprinted membranes for efficient treatment of electroplating wastewater

Jian Lu,Yingying Qin,Chao Yu,Xinyu Lin,Minjia Meng,Yongsheng Yan,Hougang Fan,Yilin Wu,Chunxiang Li

Pd (II) from release-unbridled electroplating wastewater is causing great challenges, which is unfavourable either to human health or resource reutilization. Ion-imprinted membranes (IIMs) have recently drawn attentions for selective separation of specific ions from analogues. In this context, we have developed a facile strategy for fabrication of Pd (II)-imprinted membranes (Pd-IIMs) for the selective separation of Pd (II). The enhanced flux was obtained by three-dimensional macroporous structure on polydimethylsiloxane (PDMS). Then the Pd-IIMs were synthesized by a modification-imprinting strategy based on PDMS substrates. With the existence of Co (II), Cu (II), Cd (II) and Ni (II), the as-obtained Pd-IIMs showed superior adsorptive selectivity (3.32–5.06) and perm-selectivity (2.34–4.04) towards Pd (II), as well as the satisfactory regeneration performance (more than 92% of the initial rebinding capacities after 5 cycles of adsorption/desorption). Moreover, the as-prepared Pd-IIMs also displayed stability on separation factors even under ultrasonic treatment. Notably, the overused Pd-IIMs after applications for selective separation of Pd (II) showed a satisfactory performance for the treatment of methylene blue (99.87%), which displayed potentials for the “further applications”. The Pd-IIMs and preparation   strategy developed in this work have shown a positive opportunity for the efficient treatment of electroplating wastewater and organic dyes.

研究领域: 环境科学 · 材料科学 · 化学工程
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ADVANCED SYNTHESIS & CATALYSIS · 2017 ·Vol. 359 ·期 3 ·454-466 · IF 5.646

Ligand-Free C–C Coupling Reactions Promoted by Hexagonal Boron Nitride-Supported Palladium(II) Catalyst in Water

Xu Cheng,Weijian Li,Ruifang Nie,Xiaojun Ma,Rui Sang,Li Guo,Yong Wu

A micron-scale palladium(II) material has been successfully prepared using Schiff base-modified hexagonal boron nitride as a support and used for the first time as an efficient and recyclable catalyst in organic synthesis. The morphology, composition, metal loading and thermal stability of the catalyst were studied using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), infrared spectroscopy (FT-IR), inductively coupled plasma (ICP) and thermogravimetric (TG) analyses. Then, the micron material was tested in various C–C cross-coupling reactions and exhibited excellent catalytic activities in the Suzuki and Heck reactions. Moreover, the catalyst could be easily recovered by simple filtration and reused at least ten times without significant loss of its catalytic activity. In general, this work demonstrates the possibility of using Schiff-base@hexagonal boron nitride as an efficient support for heterogeneous catalysts.

研究领域: 有机化学 · 催化材料科学
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MICROCHEMICAL JOURNAL · 2021 · IF 4.821

Simultaneous determination of proton pump inhibitors by high performance liquid chromatography with resonance Rayleigh scattering: A study of mechanism, performance and application

Zhongying Zhang,Ranxi Ni,Piao Chen,Xiaolan Zhu,Zilong Zhang,Jingdong Peng

In the present study, a convenient, selective and sensitive method of high performance liquid chromatography combined with resonance Rayleigh scattering (HPLC-RRS) for the detection of proton pump inhibitors (PPIs) was proposed based on enhancing the volume and hydrophobicity of PPIs by introducing Eosin Y (EY) and Pd(II). In order to investigate the interaction and the mechanism of signal enhancement, the complexes were characterized by ultraviolet–visible spectrum (UV), dynamic light scattering (DLS), RRS, scanning electron microscope (SEM) and the calculation of the density functional theory (DFT). The results indicated that PPIs, Pd(II) and EY formed ionic associations at 1:1:2 due to electrostatic attraction, which increased the volume and hydrophobicity of the system, resulting in the enhancement of RRS signals. Under the optimized experimental conditions, a linear relationship was found between RRS intensity and the concentration of PPIs within 0.02–25.00 μg mL −1 . The limits of detection were 10.1, 5.6, 7.5 and 8.3 ng mL −1 for rabeprazole, omeprazole, pantoprazole, and lansoprazole, respectively. In addition, the established simple, reliable and cheap method was validated and applied for the human serum samples, which indicated broad application prospects in drugs.

CAS / MDL: 75-05-8 67-56-1
研究领域: 分析化学 · 药物分析
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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2020 ·Vol. 326 ·期 2 ·1323-1331 · IF 1.137

Adsorption and separation behavior of palladium(II) on a silica-based hybrid donor adsorbent from simulated high-level liquid waste

Wu Hao,Kubota Masahiko,Osawa Naoki,Kim Seong-Yun

Adsorption and separation performances of a microporous silica-based (DAMIA-EH + TOA)/SiO 2 -P adsorbent towards Pd(II) were systematically investigated under the effect of contact time, temperature, concentration of nitric acid, chromatography etc. in a simulated high-level liquid waste containing 14 kinds of representative co-existing metal ions. Successful recovery of around 97.95% Pd(II) was achieved under the elution with 0.01 M Tu (pH = 2) solution in column experiment.

CAS / MDL: 7697-37-2
研究领域: 化学工程 · 环境科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2016 · IF 3.299

Extraction of palladium (II) by a silicone ionic liquid-based microemulsion system from chloride medium

Yan Zheng,Liying Fang,Yan Yan,Shujie Lin,Zhaohui Liu,Yanzhao Yang

The silicone ionic liquid, 1-methyl-3-[tri-(trimethylsiloxy)]silylpropyl-imidazolium chloride ([Si 4 mim]Cl), was first used for the construction of the W/O microemulsion system and the [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system was applied for palladium extraction for the first time. The stability of [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system was characterized by the Turbiscan Lab. For the Pd (II) extraction by the [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system, primary parameters (namely, the vibration time, the [Si 4 mim]Cl concentration, the phase ratio and the additives) affecting the palladium extraction was investigated to optimize the process. Under the optimum conditions, the extraction percentage of Pd (II) is up to 98%. Afterwards, the ionic-exchange mechanism of Pd (II) extraction by the [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system was confirmed by the Job Method and analyzed by FT-IR spectra. The stripping of Pd (II) from the microemulsion phase was also studied using the NaCl solutions, indicating a high stripping efficiency. At last, the selectivity of the [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system to Pd (II) from other metals (Cu (II), Co (II), Ni (II), Fe (III), Al (III) Zn (II), Ce (III), Li (I), Mg (II) and Sn (IV)) was demonstrated to be quite high. The results of our work indicate that the [Si 4 mim]Cl/ n -heptane/ n -hexanol/NaCl microemulsion system is a promising approach for Pd (II) extraction.

CAS / MDL: 616-47-7
研究领域: 化学工程 · 材料科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2021 · IF 7.312

Highly efficient extraction of palladium(II) in nitric acid solution by a phenanthroline-derived diamide ligand

Qian Xiao,Lianjun Song,Xueyu Wang,Haowei Xu,Lanlan He,Qiuju Li,Songdong Ding

The solvent extraction of Pd 2+ in nitric acid solution by a phenanthroline-derived diamide ligand of N,N′ -diethyl- N,N′ -ditolyl-2,9-diamide-1,10-phenanthroline (Et-Tol-DAPhen) and the complexation between them were described. By using meta -nitrobenzotrifluoride (F-3) as a diluent, Et-Tol-DAPhen ligand extracted Pd 2+ with strong extractability and excellent selectivity in comparison with traditional amine extractants Aliquat 336 nitrate and tri- n -octylamine. Job's method and mole ratio method suggested the formation of a 1:1 complex of Pd 2+ with Et-Tol-DAPhen. The extraction was a spontaneous and exothermic process of decreased entropy. Furthermore, the analyses of Fourier transform infrared spectra (FT-IR), UV-vis titration, and single-crystal X-ray diffraction revealed that the composition of the extracted species was [Et-Tol-DAPhen·Pd(NO 3 ) 2 ]. Based on the results of solvent extraction and complexation study, a neutral complexation extraction model was proposed. Meanwhile, the stability constant for the complexation of Pd 2+ with Et-Tol-DAPhen was also presented.

研究领域: 化学 · 环境科学
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HYDROMETALLURGY · 2022 · IF 4.217

Separation of Pd(II) and Pt(IV) in concentrated hydrochloric acid using thin-layer oil membrane and comparison with conventional extraction

Dechao Xiao,Haitao Zhou,Kaihui Cui,Kun Huang

This study proposes a new thin-layer oil membrane (TOM) extraction strategy for enhanced mutual separation of Pd(II) and Pt(IV) chlorocomplex anions in concentrated aqueous hydrochloric acid solutions using di- n -butyl sulfoxide (DBSO) as an extractant. It was discovered that Pd(II) could be preferentially extracted even in concentrated hydrochloric acid solutions. The separation coefficient between Pd(II) and Pt(IV) considerably increased than that between them during conventional extraction using a separating funnel. A new extractor was designed to perform TOM extraction by spreading a thin layer of organic extractant liquid membrane on the surface of aqueous feed solutions under laminar flow . A simplified TOM extraction model and controlled experiments were used to investigate the effect of H + and Cl − ion concentrations on the mutual separation between Pd(II) and Pt(IV). Molecular dynamics (MD) simulations were used to understand the microscopic separation mechanisms at the molecular level. Experimental results revealed that the competitive distribution of H + and Cl − ions in the boundary layer along the normal vertical direction of the organic-aqueous interface are crucial in enhancing the separation between Pd(II) and Pt(IV). The competitive adsorption and enrichment of Cl − ions at the interface prevent DBSO molecules from being protonated by H + ions, which is beneficial for the substituted coordination of DBSO molecules with PdCl 4 2− . However, the ionic association of protonated DBSO molecules with PtCl 6 2− remains dominant at the interface. As a result, even in concentrated hydrochloric acid solutions, the difference in mass transfer between PdCl 4 2− and PtCl 6 2− toward the interface was intensified.

研究领域: 化学工程 · 材料科学
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2015 · IF 2.353

Resonance light scattering determination of 6-mercaptopurine coupled with HPLC technique

Ai Ping Li,Jing Dong Peng,MingQiong Zhou,Jin Zhang

A simple, fast, costless, sensitive and selective method of resonance light scattering coupled with HPLC was established for the determination of 6-mercaptopurine in human urine sample. In a Britton–Robinson buffer solution of pH   5.5, the formation of coordination complex between 6-mercaptopurine and metal palladium (II) led to enhance the RLS intensity of the system. The RLS signal was detected by fluorescence detector at λ ex   =   λ em   =   315   nm. The analytical parameters were provided by the coupled system, the linear of 6-mercaptopurine response from 0.0615 to 2.40   μg   L −   1 and the limit of detection (S/N   =   3) was 0.05   μg   L −   1 . The presented method has been applied to determine 6-mercaptopurine in human urine samples which obtained satisfactory results. Moreover, the reaction mechanism and possible reasons for enhancement of RLS were fully discussed.

CAS / MDL: 73-24-5 50-44-2
研究领域: 分析化学 · 药物分析 · 医学检验
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HYDROMETALLURGY · 2023 · IF 4.7

Accelerated kinetics of Pd(II) solvent extraction using functionalized 1-methyl-2-(nonylthio)-1H-imidazole and its comparison with dialkylsulfide to separate Pd(II) and Pt(IV)

Shaoping Feng,Kun Huang

Dialkylsulfide is considered as the most promising extractant for separating Pd(II) and Pt(IV) in industrial processes. However, the slow kinetics for Pd(II) extraction limits its extensive application. The development of new extractants with faster kinetics, high extraction efficiency, and exceptional Pd(II) separation selectivity has been a persisting goal over the past few decades. In this study, a new functionalized extractant, 1-methyl-2-(nonylthio)-1H-imidazole (MNI) containing both N and S atoms, was synthesized and employed to separate Pd(II) from mixed hydrochloric acid solutions with different initial Pd(II)/Pt(IV) concentration ratios. Experimental results revealed that MNI not only has a high selectivity for Pd(II) over Pt(IV) but also has faster kinetics for Pd(II) extraction than diisopentylsulfide (S201) under similar extraction conditions. In contrast to traditional dialkylsulfide extractants, MNI coordinates with Pd(II) ions via the N(5) atom in its imidazole ring to form Pd(MNI) 2 Cl 2 complexes, instead of using the S atom as with dialkylsulfide. The extraction mechanism involving the coordination between Pd(II) and MNI was demonstrated using the slope analysis method and ultraviolet (UV), Fourier-transform infrared (FT-IR), 1 H NMR, and 13 C NMR spectroscopic methods. The fast extraction kinetics between MNI and Pd(II) was possibly attributed to the high charge density of the N(5) atom in the imidazole ring, whereas the outstanding separation selectivity for Pd(II) was due to the strong affinity of the N(5) atom. The facile synthesis, high saturation capacity, excellent Pd(II) selectivity, and remarkable reusability endow MNI with potential applications in Pd(II) recovery from leach solutions of waste automotive catalysts and other secondary resources.

CAS / MDL: 693-58-3 60-56-0
研究领域: 化学工程 · 材料科学
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