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Physico-chemical studies on synthetic disordered Ni-Fe layered double hydroxides

机译:合成无序镍铁层状双氢氧化物的理化研究

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Layered double hydroxides (LDHs) possess positively charged brucite-like cationic layers (Jt = 0.3-0.5), with an-ions CO-14H2O intercalculated at the interlamellar space [1,2]. LDHs represent synthetic hydrotalcite-like compounds belonging to the anionic clay minerals and find extensive uses in antacid preparations, Zeigler-Natta catalyst supports, electrodes, magnetic materials, and selective oxidation catalysts for alcohol oxidations, epoxidations and polymerization etc. [3-6]. A number of iron-nickel hydroxide carbonates with reevesite-like structures are synthesized by coprecipitation with wide Ni-Fe mole ratios [7]. The oxide precursors from the Ni-Fe LDHs after calcinations were found to be metastable, and surface enrichment with Ni(II) and high oxygen to metal ratios were reported [8]. In our laboratory, NI(II)-Fe(III) LDHs with reevesite-like structures in 2:1 and 3:1 mole ratios were synthesized, which, upon controlled calcination, produced modified disordered Ni(II)-Fe(III) oxides to be used as catalysts for oxidation of alcohols. Measurements like magnetic susceptibility, specific surface area and pore volume variations with temperature on the calcined and normal LDHs were made in addition to the characterization analyses by X-ray diffraction (XRD), infrared (IR) spectroscopy and thermo-gravimetry (TG). Elucidation of the catalytic properties of the oxides on the oxidation of 2-methyl cyclohexanol through gas chromatography (GC) analyses of the products was undertaken. The results and discussion are outlined in this letter.
机译:层状双氢氧化物(LDHs)具有带正电的水镁石样阳离子层(Jt = 0.3-0.5),在层间空间中相互计算出阴离子CO-14H2O [1,2]。 LDHs代表属于阴离子粘土矿物的类合成水滑石化合物,可广泛用于抗酸制剂,Zeigler-Natta催化剂载体,电极,磁性材料以及用于乙醇氧化,环氧化和聚合等的选择性氧化催化剂。[3-6] 。通过共沉淀法以宽的Ni-Fe摩尔比合成了许多具有网状结构的铁-镍氢氧化物碳酸盐[7]。发现煅烧后的Ni-Fe LDHs的氧化物前体是亚稳态的,据报道表面富集了Ni(II)和高的氧金属比[8]。在我们的实验室中,合成了摩尔比为2:1和3:1的具有网状结构的NI(II)-Fe(III)LDHs,通过控制煅烧,可生产出改性的无序Ni(II)-Fe(III)用作醇氧化催化剂的氧化物。除了通过X射线衍射(XRD),红外(IR)光谱和热重分析(TG)进行表征分析外,还对煅烧和普通LDH进行了磁化率,比表面积和孔体积随温度变化的测量。通过产物的气相色谱法(GC)分析阐明了氧化物对2-甲基环己醇氧化的催化性能。这封信概述了结果和讨论。

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