Cyano-Bridged Heteropolynuclear Ni(II), Cu(II) and Cd(II) Complexes, [M(deten)2Ni(μ-CN)2(CN)2] n

Three new complexes [M(deten)₂Ni(μ-CN)₂(CN)₂] _n (M = Ni, Cu and Cd, deten = N,N-diethylethylenediamine) have been synthesized and characterized by chemical, thermal analysis, FT-IR and Raman spectroscopies. The crystal structure of the Cd complex has been determined by X-ray single crystal diffraction. Structural study reveals that the Ni²⁺ and Cd²⁺ ions are located on inversion centers, and adopt slightly distorted square-planar and octahedral geometries, respectively. In the crystal structure, the intermolecular N–H⋯N hydrogen bonds link the polymeric chains into a two dimensional network. Vibrational spectral data indicate the presence of two ν(C≡N) for complexes can be assigned to the terminal and bridging cyanides. The decomposition reaction take places in the temperature range 30–1000 °C in the static air atmosphere.     

Coordination of cobalt(III), nickel(II), copper(II), palladium(II) and platinum(II) with N-ethyl-N′-(4′-methylthiazol-2′-yl)thiourea (HL)

Coordination complexes of formula [ML₂], [CoL₃], [Pd(HL)Cl₂], [CuLCl(H₂O)] and [CuL₂(H₂O)₂] {L=anion of N-ethyl-N^′-(4^′-methylthiazol-2′-yl)thiourea; M=Pt^II, Pd^II or Ni^II} were prepared and characterized by elemental analyses, magnetic susceptibilities, and by IR, NMR, electronic and mass spectral measurements.     

叔胺萃取分离钴(II)、铁(II)

研究了不必预先氧化二价铁,直接用叔胺从氯化物溶液中萃取分离钴(II)、铁(II)的新方法. 考察了不同改性剂对叔胺萃取钴(II)、铁(II)的影响以及各种因素对钴(II)、铁(II)萃取、洗涤及反萃的影响. 提出了用叔胺萃取分离钴(II)、铁(II)的最佳工艺参数.     

防霉涂料(II)

4.5.2 颜料分散、润湿剂[1,5]带有颜料的分散系统的分散机理是相当复杂的，但多数研究者在概念上具有如下的一致看法：分散过程首先是展色剂对颜料的浸润改良，即通过降低展色剂和颜料粉体界面的张力，增大浸润速度，借助于颜料的附聚或过度絮凝状态，除去主要存在于颜料表面的空气层。接着，经机械研磨，使颗粒达到原级粒子状态，最后，要防止这种已经分离的粒子重新相互结合，并保持稳定的分散状态。润湿分散剂的作用就是能吸附在上述的展色剂－颜料界面上，使之更迅速地形成更稳定的分散系统。水性防霉涂料用颜料分散剂一般是表面活性剂…     

电渗析与萃取耦合技术分离Ni(II)与Co(II)

为实现混合溶液中Ni(II)与Co(II)的分离,设计了电渗析与萃取耦合的集成分离技术,借助自行设计的设备,在选P507为萃取剂后,考察了电流密度、酸用量、体积流量、萃取剂皂化率、原料与萃取剂摩尔比、萃取方式等对分离效果的影响.结果表明:在实验范围内,电流密度3.8 mA/cm2,酸用量为理论用量的1.3倍,体积流量60 L/h、皂化率60%,原料与萃取剂摩尔比1:1.7为优取的操作条件;料液循环重复萃取,能显著提高分离效果.由此表明,电渗析与萃取耦合的分离技术,可分离混合体系中的Ni(II)、Co(II),且无需溶剂参与.     

COBALT–NICKEL SEPARATION: THE EXTRACTION OF COBALT(II) AND NICKEL(II) WITH BIS(2-ETHYLHEXYL) PHOSPHINIC ACID (PIA-8) IN TOLUENE

The extraction behaviour of cobalt(II) and nickel(II) from sulfate solutions with bis(2-ethylhexyl) phosphinic acid (PIA-8) in toluene has been studied. Quantitative extraction of Co(II) was observed at pH 5.0–5.9 while that of Ni(II) at pH 6.8–7.0 with 0.03 M PIA-8 in toluene. The difference in pH_0.5 for Co(II) and Ni(II) was 1.9. The stoichiometry of the extracted species were determined by slope analysis method. The extraction reaction proceeds by cation exchange mechanism and the extracted species were Co · R₂(HR)₂ and Ni · R₂ · 2(HR)₂. Temperature dependance of the extraction equilibrium constants were determined to estimate the apparent thermodynamic functions (ΔG, ΔS and ΔH). The method was used for separation of cobalt(II) and nickel(II). Cobalt(II) was separated from nickel even at 1:20 (Co:Ni) ratio. The separation of cobalt(II) from nickel(II) was favoured with the increase in temperature.     

Pd(II)-Cu(II)催化氧化净化PH3的动力学实验

传统的净化方法难以实现低成本、高效、选择性净化含磷化氢尾气,这限制了含磷化氢尾气的资源化技术的实现.文章利用自主筛选的催化剂,在实验室进行了Pd2 浓度、Cu2 浓度、反应温度、混和气氧体积分数、磷化氢质量浓度、混合气流速等因素对Pd(II)-Cu(II)水溶液净化含磷化氢气体影响的研究.实验结果表明,Pd(II)-Cu(II)催化剂在低温(22-73 ℃)、常压下(100 kPa)对质量浓度为850 mg/m3磷化氢气体净化效率可高达100%.并且催化剂稳定性随催化氧化反应温度的升高而降低,随被净化混和气中氧体积分数、吸收液中Pd2 浓度及Cu2 浓度增大而增强;催化氧化净化效率随混和气中磷化氢质量浓度升高而降低,随被净化的混和气流速降低而升高.     

First 3D heterotrimetallic Mn(II)–Cu(II)–K(I) polymer and three 3D Cu(II)/Mn(II) open network based on pyridine-2,3,5,6-tetracarboxylic acid

Four novel 3D coordination polymers, {[K₃Cu₂(H_0.5pdtc)₂ (H₂O)₆]·(H₂O)₂}_n (1), {[trans-K₂Mn₃(pdtc)₂ (H₂O)₁₁]·H₂O}_n (2), {[trans-K₂Mn₃(pdtc)₂ (H₂O)₁₀]·H₂O}_n (3) and {[cis-K₂Cu₂Mn(pdtc)₂ (H₂O)₁₀]·H₂O}_n (4), were synthesized by the self-assembly of potassium pyridine-2,3,5,6-tetracarboxylate (K₄pdtc) with metal salts. All of them contain infinite 1D stepwise chain. Notably, 2–4 have 2D network structures depending on the trans- and cis- hexacoordinated Mn(II) acting as connecters between the chains. Then, they further assemble into 3D or twin-plane structures by K(I) ions. 4 is the first Cu/Mn/K heterotrimetallic complex with H₄pdtc. The (H₂O)₆ clusters in 1 arranged stepwise along the complex chains owing to the host chains' template effect. The variable–temperature magnetic measurements reveal that weak antiferromagnetic interactions exist in complexes 1 and 4.     

Heteronuclear Cu(II)–Mn(II)–Cu(II) Complex Constructed from Metallo-Ligand Through Carboxylate Oxygens: Coexistence of Water Hexamers

A heteronuclear complex of [Mn(H₂O)₄(CuL)₂]₂·4H₂O 1 (H₂L = 2-hydrogen benzaldehydeneglycylglycine) has been synthesized and characterized by IR spectra, TGA, and single crystal X-ray diffraction analysis. The molecule consists of one $\text{Mn}{(\text{H}_{2}\text{O})_{4}}^{2+}$ Mn(H₂O) ₄ ²⁺ group and two symmetric groups [CuL]^? which are connected by carboxylate oxygen atoms. A discrete water hexamer composed of a planar tetrameric water ring and two pendent water molecules acts as a ‘glue’ to assemble adjacent [CuL]^? into a two-dimensional structure.     

A very labile monomeric 1,5-cyclooctadiene complex of W(II) and its transformation to dimeric [(μ-Cl)2W2(GeCl3)2(CO)6(NCMe)2]

The photochemical oxidative addition of 1 equiv. of GeCl₄ to [W(CO)₄(η²,η²-1,5-C₈H₁₂)] affords the very labile seven-coordinate complex of tungsten(II) [WCl(GeCl₃)(CO)₃(η²,η²-1,5-C₈H₁₂)] (1). The structure of compound 1 has been established by IR and ¹H NMR spectroscopic methods. A very labile 1,5-cyclooctadiene ligand of 1 in dichloromethane/acetonitrile solution leaves the coordination sphere of tungsten to give a dimeric seven-coordinate compound of tungsten(II) [(μ-Cl)₂W₂(GeCl₃)₂(CO)₆(NCMe)₂] (2). The crystal structure of a new dimeric compound containing W–Ge bonds (2) was determined by X-ray diffraction studies.     

A cyanohydridoborato–vanadium(II) complex,trans-[V(NCBH3)2(thf)4]

[V(NCBH₃)₂(thf)₄], the first cyanohydroborato complex of an early transition metal, has been generated in the system [V(CO)₆]⁻/I₂/tolane/Na[NCBH₃] in THF. The crystal structure reveals an ideal trans configuration (point group D_2h) with about linear CNBH₃⁻ units, and without intermolecular (hydrogen bonding) interactions.     

Adsorption Behavior of Cadmium(II) and Lead(II) on Mesoporous Silicate MCM‐41

Abstract

This investigation examines metal ion adsorption on mesoporous silicate, MCM‐41, synthesized from sodium silicate solution and cethyltrimethylammonium bromide (CTAB). MCM‐41 has potential as an adsorbent material, with a regular hexagonal pore structure, large specific surface area, and large pore volume. The MCM‐41 synthesized for this investigation is characterized using powder X‐ray diffraction and nitrogen adsorption and desorption isotherms data. The adsorption behavior for cadmium(II) and lead(II) onto MCM‐41 was studied by contacting the mesoporous silicate with an aqueous solution of metal salts and acetylacetone. Both Cd²⁺ and Pb²⁺ were found to quantitatively adsorb onto MCM‐41. The results of this study suggest that MCM‐41 may have applications in the recovery of toxic metals from waste waters.     

Hydrothermal synthesis and characterisation of lead(II) benzene-1,3,5-tricarboxylate [Pb3BTC2]·H2O: a lead(II) carboxylate polymer

The coordination polymer of formula [Pb₃BTC₂]·H₂O (BTC=1,3,5-benzenetricarboxylate) contains 2 different BTC trianions, 3 different Pb cations and 3 different carboxylate coordination modes.     

Syntheses and Characterization of New Nano-porous Soft Copper(II) Metal–organic Framework and Nano-porous Two-dimensional Manganese(II) and Zinc(II) Coordination Polymers with 4,4′-Bipyridine and 2-Sulfobenzoic Acid

Three new Cu(II), Mn(II), and Zn(II) coordination polymers with 4,4′-bipyridine (4,4′-bipy) and 2-sulfobenzoic acid (2-H₂sb) ligands, [M(4,4′-bipy)(2-sb)(H₂O)]_n, have been synthesized and characterized by IR spectroscopy and elemental analyses. The structures were determined by single-crystal X-ray crystallography. The structural studies show that the metal atoms have six-coordinate geometry with a distorted octahedral environment constructed with 4,4′-bipy and 2-sb²⁻ linkers stacked over each other to generate a two-dimension motif. Self-assembly of these compounds in the solid state is likely caused by coordination and hydrogen-bonds. While polymers containing Zn(II) and Mn(II) have analogous structures, the Cu(II)-containing nano-porous soft metal–organic framework presents a different structure.     

Novel Polymeric Metal Complexes of 2,7-Bis[2-(2′-Pyridyl) Benzimidazole]- 9,9′-Dioctylfluorene with Cu(II)and Zn(II): Synthesis and Luminescence Properties

Abstract  A novel ligand, 2,7-bis[2-(2′-Pyridyl)benzimidazole]- 9,9′-dioctylfluorene (BPDOF) and its polymeric complexes with copper(II) and zinc(II) were successfully synthesized and characterized by ¹H NMR, FT-IR, elemental analysis, UV-vis, conductivity measurements and gel permeation chromatography. The UV–vis absorption, fluorescence spectra, and thermal properties of these complexes were investigated at room temperature. The experimental results show that polymeric metal complexes BPDOF-Cu(II) and BPDOF-Zn(II) emit purple/green luminescence at 430 and 509 nm in DMF solution and emit green luminescence at 495 and 527 nm in the solid state. Thermal properties measurement and analysis show that they have good thermal stabilities. Graphical Abstract  Synthesis route: 2,7-bis[2-(2′-Pyridyl) benzimidazole]- 9,9′-dioctylfluorene (BPDOF) was synthesized using 2-(2′-Pyridyl)benzimidazole and 2,7-dibromo-9,9′-dioctylfluorene by Ullmann condensation. Polymeric metal complexes of the corresponding were synthesized with CuCl₂ · 2H₂O, ZnCl₂.      

Ruthenium(II) acetylacetonato–sulfoxide complexes

The water-soluble Ru^II acetylacetonato–sulfoxide complexes, cis-Ru(acac)₂(DMSO)₂ (1) and Ru(acac)₂(meso-BESE) (2), were synthesized (BESE=1,2-bis(ethylsulfinyl)ethane=EtS(O)(CH₂)₂S(O)Et). Both complexes were characterized by ¹H and ¹³C{¹H} NMR, UV–Vis, and IR spectroscopies, as well as MS, elemental analysis, solution conductivity, and cyclic voltammetry, while the molecular structure of 2 was determined also by X-ray crystallography. All sulfoxide ligands are S-bonded. The complexes were tested against human breast cancer cells (MDA-MB-435S) using an in vitro MTT assay, a colorimetric determination of cell viability; IC₅₀ values of >2000 and 1500 ± 100 μM were determined for 1 and 2, respectively, while cisplatin exhibits an IC₅₀ value of 30 ± 5 μM.     

Hydrothermal Synthesis of Cd(II), Mn(II) and Ni(II) Coordination Polymers Derived from Benzopenone-2,4′-carboxylate and N-door Ligands

Three new coordination polymers [Cd(L)(4,4′-bipy)_0.5]_n (1), {[Mn(L)(bpp)]·H₂O}_n (2) and [Ni(L)(2,2′-bipy)(H₂O)₂]_n(3) [H₂L = Benzopenone-2,4′-dicarboxylic acid, 4,4′-bipy = 4,4′-bipy ridine, bpp = 1,3-di(4-pyridyl) propane and 2,2′-bipy = 2,2′-bipyridine] have been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction. Single-crystal X-ray analyses revealed that the H₂L ligand acts as a bridge, exhibiting three coordination modes to link metal ion: bidentate chelating, bis-monodentate, monodentate. Compound 1 has 3-connected metal–organic framework with the (6³) topology notation; Compounds 2 and 3 are one-dimensional chain structures. The luminescent properties for compound 1 was investigated.     

Synthesis,structure and properties of a new copper (II) complex, [Cu2(4,4′-bpy)5(H2O)4](ClO4)4(4,4′-bpy)(DMF)2(H2O)2

A new copper (II) complex with formula [Cu₂(4,4′-bpy)₅(H₂O)₄](ClO₄)₄(4,4′-bpy)(DMF)₂(H₂O)₂ has been synthesized by reaction of 4,4′-bpyridine (4,4′-bpy) with Cu(ClO₄)₂. While strong hydrogen bonds play central roles in the formation of the 3D structure, the combined influence of the weak interactions such as C–H?O bonds, anion?π and C–H?π interactions are also evident in the structure. The preliminary investigation on the thermal property of the complex is presented.     

Removal efficiency of Pb(II), Zn(II), Cd(II) and Cu(II) from aqueous solution and natural water by ketoenol–pyrazole receptor functionalized silica hybrid adsorbent

In this study, we reported an efficient, alternative, and low-cost adsorbent for the efficient removal of Pb(II), Zn(II), Cd(II) and Cu(II) from water. The new hybrid material has been prepared by immobilizing a conjugated system (2Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxybut-2-en-1-one on silica gel previously doped with 3-aminopropyltrimethoxysilane. The formed surface (SiNPz) was perfectly analyzed. Adsorption studies have demonstrated the ability to highlight the surface designed for efficient removal of above toxic metals from aqueous solutions using FAAS. The new material was used for the extraction of metals from natural water and showed efficiency results for toxic heavy metals.