Zeolite Encapsulated Complexes Of Fe,Co,Ni,Cu And Pd:Synthesis , Characterization And Catalysis-2003

This thesis deals with the synthesis, characterization and catalysis activity studies of some zeolite encapsulated complexes. Encapsulation inside the zeolite cages makes the catalysts more stable. Further, the framework prevents the complexes from dimerising. Catalysis by metal complexes encapsulated in the cavities of zeolites and other molecular sieves has many features of homogeneous, heterogenous and enzymatic catalysis. Serious attempts has been made to gain product selectivity in catalysis .The catalytic activity shown by the encapsulated complexes can be correlated to the structure of the active site inside the zeolite pore. It deals with the studies on the partial oxidation of benzyl alcohol to benzaldehyde. The oxidatio was carried out using hydrogen peroxide as oxidant in presence of PdYDMG and CuYSPP as catalysts. The product (benzaldehyde) was detected using TLC and confirmed using GC.The catalytic activity of the complexes was tested for oxidation under various conditions. The operating conditions like the amount of the catalyst, reaction time, oxidant to substrate ratio, reaction temprature, and solvents have been optimized. No further oxidation products were obtained on continuing the reaction for four hours beyond the optimum time. Maximum conversion was obtained at room temperature and the percentage conversion decreased with increase in temperature. Activity was found to be dependent on the solvent used. With increasing awareness about the dangers of environmental degradation, research in chemistry is getting increasing geared to the development of “green chemistry,” by designing environmentally friendly products and processes that bring down the generation and use of hazardous substances.

A PVC Plasticized Sensor for Ni(II) Ion Based on a Simple Ethylenediamine Derivative

new PVC membrane ion selective electrode which is highly selective towards Ni(II) ions was constructed using a Schiff base containing a binaphthyl moiety as the ionophore. The sensor exhibited a good Nernstian response for nickel ions over the concentration range 1.0 × 10–1 – 5.0 × 10–6 M with a lower limit of detection of 1.3 × 10–6 M. It has a fast response time and can be used for a period of 4 months with a good reproducibility. The sensor is suitable for use in aqueous solutions in a wide pH range of 3.6 – 7.4 and works satisfactorily in the presence of 25% (v/v) methanol or ethanol. The sensor shows high selectivity to nickel ions over a wide variety of cations. It has been successfully used as an indicator electrode in the potentiometric titration of nickel ions against EDTA and also for the direct determination of nickel content in real samples: effluent samples, chocolates and hydrogenated oils.

Zeolite-encapsulated Co(II), Ni(II) and Cu(II) complexes as catalysts for partial oxidation of benzyl alcohol and ethylbenzene

Co(II), Ni(II) and Cu(II) complexes of dimethylglyoxime and N,N-ethylenebis(7-methylsalicylideneamine) have been synthesized in situ in Y zeolite by the reaction of ion-exchanged metal ions with the flexible ligand molecules that had diffused into the cavities. The hybrid materials obtained have been characterized by elemental analysis, SEM, XRD, surface area, pore volume, magnetic moment, FTIR, UV-Vis and EPR techniques. Analysis of data indicates the formation of complexes in the pores without affecting the zeolite framework structure, the absence of any extraneous species and the geometry of encapsulated complexes. The catalytic activities for hydrogen peroxide decomposition and oxidation of benzyl alcohol and ethylbenzene of zeolite complexes are reported. Zeolite Cu(II) complexes were found to be more active than the corresponding Co(II) and Ni(II) complexes for oxidation reactions. The catalytic properties of the complexes are influenced by their geometry and by the steric environment of the active sites. Zeolite complexes are stable enough to be reused and are suitable to be utilized as partial oxidation catalysts.

Ni(II) and Ru(II) Schiff base complexes as catalysts for the reduction of benzene

Two new complexes, [MII(L)(Cl)(H2O)2]·H2O (where M=Ni or Ru and L = heterocyclic Schiff base, 3- hydroxyquinoxaline-2-carboxalidene-4-aminoantipyrine), have been synthesized and characterized by elemental analysis, FT-IR, UV–vis diffuse reflectance spectroscopy, FAB-MASS, TG–DTA, AAS, cyclic voltammetry, conductance and magnetic susceptibility measurements. The complexes have a distorted octahedral structure andwere found to be effective catalysts for the hydrogenation of benzene. The influence of several reaction parameters such as reaction time, temperature, hydrogen pressure, concentration of the catalyst and concentration of benzenewas tested. A turnover frequency of 5372 h−1 has been found in the case of ruthenium complex for the reduction of benzene at 80 ◦C with 3.64×10−6 mol catalyst, 0.34 mol benzene and at a hydrogen pressure of 50 bar. In the case of the nickel complex, a turnover frequency of 1718 h−1 has been found for the same reaction with 3.95×10−6 mol catalyst under similar experimental conditions. The nickel complex shows more selectivity for the formation of cyclohexene while the ruthenium complex is more selective for the formation of cyclohexane

Fabrication of thin films and nano columnar structures of Fe-Ni amorphous alloys and modification of its surface properties by thermal annealing and swift heavy ion irradiation for tailoring the magnetic properties

Department of Physics, Cochin University of Science and Technology

Study of cyclohexanol decomposition reaction over the ferrospinels, A1−xCuxFe2O4 (A=Ni or Co and x=0, 0.3, 0.5, 0.7 and 1), prepared by ‘soft’ chemical methods

Preparation of simple and mixed ferrospinels of nickel, cobalt and copper and their sulphated analogues by the room temperature coprecipitation method yielded fine particles with high surface areas. Study of the vapour phase decomposition of cyclohexanol at 300 °C over all the ferrospinel systems showed very good conversions yielding cyclohexene by dehydration and/or cyclohexanone by dehydrogenation, as the major products. Sulphation very much enhanced the dehydration activity over all the samples. A good correlation was obtained between the dehydration activities of the simple ferrites and their weak plus medium strength acidities (usually of the Brφnsted type) determined independently by the n-butylamine adsorption and ammonia-TPD methods. Mixed ferrites containing copper showed a general decrease in acidities and a drastic decrease in dehydration activities. There was no general correlation between the basicity parameters obtained by electron donor studies and the ratio of dehydrogenation to dehydration activities. There was a leap in the dehydrogenation activities in the case of all the ferrospinel samples containing copper. Along with the basic properties, the redox properties of copper ion have been invoked to account for this added activity.

A marine actinomycete nocardiopsis mccb 110 as source of novel drugs to manage vibriosis

Aquaculture is a form of agriculture that involves the propagation, cultivation and marketing of aquatic plants and animals in a controlled environment (Swann, 1992). After growing steadily, particularly in the last four decades, aquaculture is for the first time set to contribute half of the fish consumed by the human population worldwide. Given the projected population growth over the next two decades, it is estimated that at least an additional 40 million tonnes of aquatic food will be required by 2030 to maintain the current per capita consumption (FAO, 2006). Capture fisheries and aquaculture supplied the world with about 110 million tonnes of food fish in 2006. Of this total, aquaculture accounted for 47 percent (FAO, 2009). Globally, penaeid shrimp culture ranks sixth in terms of quantity and second in terms of value amongst all taxonomic groups of aquatic animals cultivated (FAO, 2006). In places where warm-water aquaculture was possible black tiger shrimp, Penaeus monodon became the preferred variety of shrimp cultivar owing to its fast growth, seed availability and importantly due to high prices it fetches (Pechmanee, 1997). World shrimp production is dominated by P.monodon, which accounted for more than 50 % of the production in 1999 (FAO, 2000). In the last few years the whiteleg shrimp, Litopenaeus vannamei, has replaced P.monodon in many countries. Indian shrimp culture is dominated by P.monodon with the East Coast accounting for 70% of the production (Hein, 2002). Intensive culture, apart from other problems, results in enhanced susceptibility of the cultured species to diseases (Jory, 1997), which in fact have become the biggest constraint in shrimp aquaculture (FAO, 2003).

Synthesis, spectral and structural studies of novel binuclear Ni(II) complex of salicylaldehyde 3-azacyclothiosemicarbazone

A novel binuclear Ni(II) complex of salicylaldehyde 3-azacyclothiosemicarbazone (H2L) has been synthesized and characterized by elemental analysis, IR and UV–Vis spectroscopy. The single crystal X-ray structure of the complex shows that bridging occurs through thiolato sulfur and phenolic oxygen atoms. Nickel centers in the complex have square planar and octahedral geometries

Ni filled flexible multi-walled carbon nanotube–polystyrene composite films as efficient microwave absorbers

In this letter, we report flexible, non corrosive, and light weight nickel nanoparticle@multi-walled carbon nanotube–polystyrene (Ni@MWCNT/PS) composite films as microwave absorbing material in the frequency range of S band (2-4 GHz). Dielectric permittivity and magnetic permeability of composites having 0.5 and 1.5 wt. % filler amount were measured using the cavity perturbation technique. Reflection loss maxima of 33 dB (at 2.7 GHz) and 24 dB (at 2.7 GHz) were achieved for 0.5 and 1.5 wt. % Ni@MWCNT/PS composite films of 6 and 4 mm thickness, respectively, suggesting that low concentrations of filler provide significant electromagnetic interference shielding

On the Growth Mechanism of Nickel and Cobalt Nanowires and Comparison of Their Magnetic Properties

Magnetic nanowires (NWs) are ideal materials for the fabrication of various multifunctional nanostructures which can be manipulated by an external magnetic fi eld. Highly crystalline and textured nanowires of nickel (Ni NWs) and cobalt (Co NWs) with high aspect ratio (~330) and high coercivity have been synthesized by electrodeposition using nickel sulphate hexahydrate (NiSO4·6H2O) and cobalt sulphate heptahydrate (CoSO4·7H2O) respectively on nanoporous alumina membranes. They exhibit a preferential growth along〈110〉. A general mobility assisted growth mechanism for the formation of Ni and Co NWs is proposed. The role of the hydration layer on the resulting one-dimensional geometry in the case of potentiostatic electrodeposition is verified. A very high interwire interaction resulting from magnetostatic dipolar interactions between the nanowires is observed. An unusual low-temperature magnetisation switching for fi eld parallel to the wire axis is evident from the peculiar high fi eld M(T) curve

Structural, topographical and magnetic evolution of RF-sputtered Fe-Ni alloy based thin films with thermal annealing

Metglas 2826 MB having a nominal composition of Fe40Ni38Mo4B18 is an excellent soft magnetic material and finds application in sensors and memory heads. However, the thin-film forms of Fe40Ni38Mo4B18 are seldom studied, although they are important in micro-electro-mechanical systems/nano-electromechanical systems devices. The stoichiometry of the film plays a vital role in determining the structural and magnetic properties of Fe40Ni38Mo4B18 thin films: retaining the composition in thin films is a challenge. Thin films of 52 nm thickness were fabricated by RF sputtering technique on silicon substrate from a target of nominal composition of Fe40Ni38Mo4B18. The films were annealed at temperatures of 400 °C and 600 °C. The micro-structural studies of films using glancing x-ray diffractometer (GXRD) and transmission electron microscope (TEM) revealed that pristine films are crystalline with (FeNiMo)23B6 phase. Atomic force microscope (AFM) images were subjected to power spectral density analysis to understand the probable surface evolution mechanism during sputtering and annealing. X-ray photoelectron spectroscopy (XPS) was employed to determine the film composition. The sluggish growth of crystallites with annealing is attributed to the presence of molybdenum in the thin film. The observed changes in magnetic properties were correlated with annealing induced structural, compositional and morphological changes

Vibrational spectroscopic studies of Guanidinium metal (MII) sulphate hexahydrates [MII = Co, Fe, Ni]

The Raman and FTIR spectra of [C(NH2)3]2M(SO4)2 ·6H2O (withM= Co, Fe, Ni) were recorded and analysed. The observed spectral bands are assigned in terms of vibrations of guanidinium ions, sulphate groups and water molecules. The analysis shows that the sulphate tetrahedra are distorted from their free state symmetry Td to C1. This is attributed to the presence of hydrogen bonds from water molecules. The order of distortion of the metal oxygen octahedra influenced the distortion of the sulphate tetrahedra. The appearance of 1– 3 modes of water molecules above 3300 cm−1 indicates the presence of weak hydrogen bonds