Replacement of precious
metal catalysts in the Guerbet upgrade
of ethanol to n-butanol with first-row metal complex
catalysts is highly appreciated due to their economic and environmental
friendliness. The manganese pincer complexes of the type [(RPNP)MnBr(CO)2] (R =
i
Pr, Cy,
t
Bu, Ph or Ad) are found to be excellent catalysts
for upgrading ethanol to n-butanol. Under suitable
reaction conditions and with an appropriate base, about 34% yield
of n-butanol can be obtained in high selectivity.
A detailed account on the effect of the temperature, solvent, nature,
and proportion of base used and the stereoelectronic effects of the
ligand substituents on the catalytic activity of the catalysts as
well as the plausible deactivation pathways is presented.
The steric properties of various
nitrogen substituents on amidines
were tuned in order to obtain group 4 mono- and bis(amidinate) dimethylamido
or chloride complexes. The amidinate dimethylamido and chloride complexes
were prepared, and their solid-state as well as their solution-state
structures were studied. After the activation by MAO, these complexes
were tested in the polymerization of propylene and ethylene. A noticeable
influence of the amidine carbon and nitrogen substituents on the activity
of the catalyst and properties of the obtained polymer was observed.
Further, a plausible mechanism for the ethylene polymerization process
is presented taking into account a combination of ESR-C60 and MALDI-TOF experiments, shedding light on the nature of the catalytic
species.
Here we demonstrate the selective bulk scale synthesis of delaminated graphene sheets by a proper choice of magnetic field modulating an electric-arc. An ultra-high purity glassy graphite anode was sublimated in an argon atmosphere. Carbon nanotubes (CNTs), as well as graphene sheets were found inside the deposit formed on the cathode. Both the high purity CNTs as well as graphene sheets, with minimal structural defects, were synthesized separately by varying the strength and orientation of the external magnetic field generated by arrays of permanent magnets. The as-synthesized carbonaceous samples were characterized with the help of transmission electron microscopy, selected area electron diffraction (SAED), Raman spectroscopy (RS) and thermogravimetry for optimizing the highest selective production of delaminated graphenes. This optimization was done by varying the strength and orientation of the external magnetic field.The as-synthesized graphene sheets exhibited relatively high degree of graphitization and low structural defect density as confirmed by RS. They were found to exhibit higher oxidation temperature (767°C) than that of the carbon nanocrystalline (690°C) particles as inferred from the thermogravimatric analysis. Moreover, they were found to form 'scroll-like CNTs' at their edges on account of their surface energy minimization. This was confirmed by the SAED analysis. With this new technique, we could successfully synthesize delaminated graphenes at a rate of few g/h.
New transition metal complexes of quinoxaline-thiosemicarbazone ligands were prepared and characterised by spectroanalytical techniques. The ligands L 1 H 2 and L 2 H 2 were obtained by the reaction of quinoxaline-2.3(1,4H)-dione with methyl and phenyl thiosemicarbazide, respectively. All the complexes are found to be monomeric in nature and have tetrahedral geometry. The copper complexes have shown redox responses in the applied voltage range, whereas the ligands and other complexes are electrochemically innocent. The ligands, copper and zinc complexes are explored for antidiabetic activity in the diabetes-induced Wister rats. Evaluation of antidiabetic activity was done by blood-glucose test and oral glucose tolerance test; few compounds have exhibited significant antidiabetic activity and posses low toxicity with a high safety profile.
The paper reports the deterministic effects of a focusing electric field in improving the purity and yield of the arc-generated carbon nanotubes (CNTs). The method utilizes a focusing electrostatic field, which was superimposed on the arc symmetrically. The focusing voltage was varied from 0 to 1200 V at steps of 200 V and a number of cathode deposits, thus generated, were collected and thoroughly analysed in their totality with the help of weight balance, Raman spectroscopy, transmission electron microscopy and thermogravimetry. With the optimally configured focusing electric field, the arc generator is found to utilize nearly 85% of the consumed anode material, for converting into cathode deposit consisting of CNTs, as compared with about 35% in the conventional arc plasma method. The sample prepared under optimized conditions exhibited high oxidation temperature (851 °C) in the thermogravimetric analysis, negligible D band intensity along with a reduced G band line-width (14 cm−1) in the Raman spectrum, confirming the presence of high purity CNTs with a high relative yield.
The cationic zinc adduct {[HB(3,5-(CF3)2Pz)3]Zn(NCMe)2}ClO4 catalyzes the functionalization of tertiary, secondary, and primary C-H bonds of alkanes via carbene insertion. Ethyl diazoacetate serves as the :CHCO2Et carbene precursor. The counteranion, supporting ligand, and coordinating solvents affect the catalytic activity. An in situ generated {[HB(3,5-(CF3)2Pz)3]Zn}(+) species containing a bulkier {B[3,5-(CF3)2C6H3]4}(-) anion gives the best results among the zinc catalysts used.
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