Sreekumar, K; Raja, T; Kiran, B P; Sugunan, S; Rao, B S(Elsevier, 1999)
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Abstract:
The reaction of aniline with methanol was carried out over Zn1-xNixFe2O4 (x= 0, 0.2, 0.5, 0.8 and 1) type systems in a
fixed-bed down-flow reactor. It was observed that systems possessing low ``x'' values are highly selective and active for mono
N-alkylation of aniline leading to N-methyl aniline. Selectivity for N-methyl aniline over ZnFe2O4 was more than 99% under
the optimized reaction conditions. Even at methanol to aniline molar ratio of 2, the yield of N-methyl aniline was nearly
55.5%, whereas its yield exceeded 67% at the molar ratio of 7. The Lewis acid sites of the catalysts are mainly responsible for
the good catalytic performance. Cation distribution in the spinel lattice influences their acido-basic properties, and hence,
these factors have been considered as helpful to evaluate the activity and stability of the systems.
Girish Kumar,K; Chowdary, K P R; Devala Rao, G(Indian Journal Of Pharmaceutical Sciences, January 8, 1999)
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Abstract:
Two simple and sensitive spectrophotometric methods (A and B)in the visible region have been developed for the determination of nimesulide in bulk and in dosage forms.Method A is based on the reaction of reduced nimesulide with nitrous acid followed by its coupling with phloroglucinol to yield an yellow colored azo dye with an absorption maximum of 400 nm and method B is based on the reaction of reduced nimesulide with p-dimethylamino benzaldehyde(PDAB) to form an yellow colored chromogen wiht an absorption maximum of 415 nm.When pharmaceutical preparations (Tablets and suspension) were analysed, the results obtained by the proposed methods are in good agreement with the labelled amounts and are comparable with the results obtained by a reported method.recovery in both the method is 98-101 %.
Sugunan, S; Seena, C R K(Indian Journal of Chemistry, September , 1999)
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Abstract:
The surface acidity/ basicity of TiO2 (rutile) and its sulphate modified
form have been determined by titration method using Hammett
indicators after activation at different temperatures. The electron
donating properties of these oxides are also studied from the adsorption
of electron acceptors of different electron affinity values. The
data have been correlated with the catalytic activity of these oxides
towards esterification of acetic acid using n-butanol, reduction of
cyclohexanone in isopropanol and oxidation of cyclohexanol in benzophenone.
Catalytic activity for esterification and oxidation reaction
parallels the acidity while that for reduction reaction parallels
the basicity of these oxides.
Sugunan, S; Bindhu, Jacob; Binoy,Jose(Indian Journal of Chemistry, October , 1999)
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Abstract:
The results of a detailed study of the propionylation of anisole over various medium and large pore zeolites such as H-ZSM-5, H-beta, H-Na-beta. H-mordenite. H-Y and H-RE- Y are presented and discussed. In addition, homogenous catalysts and amorphous Si02-Al2O3 are also included for comparison, The catalyst and process parameters are optimised to enhance the conversion of propionyl chloride(PC) and selectivity to 4-methoxypropiophenone(4-MOPP).
Sugunan, S; Bindhu, Jacob(Indian Journal of Chemistry, October , 1999)
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Abstract:
The acidity of the various rare-earth exchanged zeolite-Y
catalysts has been examined by titration method using Hammett
indicators and is correlated with the catalytic activity of the
samples in the benzylation of 0-xylene.
Sugunan, S; Seena, Kumaree C R(Indian Journal of Chemistry, November , 1999)
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Abstract:
The changes in surface acidity/basicity and catalytic activity of cerium oxide due to surface modification by sulphate ion have been
investigated. Electron donor properties of both the modified and unmodified oxides have been studied using electron acceptors of
various electron affinity values, viz. 7,7,8,8-tetracyanoquinodimethane, 2,3,5,6-tetrachloro--l, 4-benzoquinone. p-dinitrobenzene and
m-dinitrobenzene in order to find out whether the increase in acidity on suphation is due to the generation of new acidic sites or they are
formed at the expense of some of the basic sites. The surface acidity/basicity has been determined using a set of Hammett indicators.
The data have been correlated with the catalytic activity of the oxides for esterification of acetic acid using l-butanol, reduction of
cyclohexanone with 2- propanol and oxidation of cyclohexanol using benzophenone.
Jyothi, T M; Rao, B S; Sugunan, S; Sreekumar, K(Indian Journal of Chemistry, December , 1999)
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Abstract:
Alkylation of phenol with methanol has been carried out over
Sn-La and Sn-Sm mixed oxides of varying compositions at 623 K
in a vapour phase flow reactor. It is found that the product
selectivity is greatly influenced by the acid-base properties of the
catalysts. Ortho-cresol formation is favoured over catalysts with
weak acid sites whereas formation of 2,6-xylenol occurs in the
presence of stronger acid sites. The cyclohexanol decomposition
reaction and titrimetric method using Hammett indicators have
been employed to elucidate the acid-base properties of the
catalysts.
Description:
Indian Journal of Chemistry
Vol. 38A, December 1999, pp. 1253-1255
Sreekumar, K; Jyothi, T M; Talawar, M B; Kiran, B P; Rao, B S(Elsevier, 2000)
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Abstract:
A series of ferrites having the general formula Zn1-xCoxFe2O4 (x=0, 0.2, 0.5, 0.8 and 1.0)were prepared by soft
chemical route. The materials were characterized by adopting various physico-chemical methods. The reaction of aniline
with methanol was studied in a fixed-bed reactor system as a potential source for the production of various methyl anilines.
It was observed that systems possessing low ‘ x’ values are highly selective and active for N-monoalkylation of aniline
leading to N-methylaniline. Reaction parameters were properly varied to optimize the reaction conditions for obtaining
N-methylaniline selectively and in better yield. Among the systems Zn0.8Co0.2Fe2O4 is remarkable due to its very high
activity and excellent stability. Under the optimized conditions N-methylaniline selectivity exceeded 98%. Even at a
methanol to aniline molar ratio of 2, the yield of N-methylaniline was nearly 50%, whereas its yield exceeded 71% at the
molar ratio of 5. ZnFe2O4, though executed better conversion than Zn0.8Co0.2Fe2O4 in the initial period of the run,
deactivates quickly as the reaction proceeds. The Lewis acidity of the catalysts is mainly responsible for the good
performance. Cation distribution in the spinel lattice influences their acido-basic properties and, hence, these factors have
been considered as helpful parameters to evaluate the activity of the systems.
Sreekumar, K; Thomas, Mathew; Mirajkar, S P; Sugunan, S; Rao, B S(Elsevier, 2000)
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Abstract:
The catalyst compositions of the Zn1−xCOxFe2O4 (x= 0, 0.2, 0.5, 0.8 and 1.0) spiel series possessing ‘x’ values, x less than or equal to 0.5, are
unique for selective N-monomethylation of aniline using methanol as the alkylating agent. Since dimethyl carbonate (DMC)
is another potential non-toxic alkylating agent, alkylation of aniline was investigated over various Zn–Co ferrites using DMC
as the alkylating agent. The merits and demerits of the two alkylating agents are compared. Catalytic activity followed a
similar trend with respect to the composition of the ferrospinel systems. DMC is active at comparatively low temperature,
where methanol shows only mild activity. However, on the selectivity basis, DMC as an alkylating agent could not compete
with methanol, since the former gave appreciable amounts of N,N-dimethylaniline (NNDMA) even at low temperature where
methanol gave nearly 99% N-methylaniline (NMA) selectivity. As in the case of methanol, DMC also did not give any
C-alkylated products.
Jyothi, T M; Sugunan, S; Rao, B S(Catalysis Letters, 2000)
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Abstract:
A comparative study on the anisole methylation with methanol over lanthanum-promoted Sn02 catalyst and its sulfate-doped analogue
is presented. A maximum 2.6-xylenol selectivity of 82% was achieved at 400 degreeC under optimized conditions at an anisole
conversion of 65% over lanthanum-promoted Sn02 catalyst. The sulfate modification resulted in the dealkylation of anisole to phenol
followed by several unselective side reactions due to the creation of strong acid sites. The activity of lanthanum-modified tin oxide
catalysts in the selective formation of 2.6-xylenol is ascribed to the presence of weak Lewis acid sites and comparatively stronger basic
sites.
Sugunan, S; Nisha, K; Rekha, R; Rahna, K S; Suja, H; Deepa, C S(Indian Journal of Chemistry, July , 2000)
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Abstract:
The pillared montmorillonite has been prepared by exchanging
Na+ in the interlayer of montmorillonite with Al hydroxy cation followed
by calcination. Pillared clays are also prepared after exchanging
Na' ions with Ce, La, Sm-ions and then pillarcd with aluminium
oxides, The surface characterisation of the prepared catalysts has been
done using XRD and surface area measurements. To probe the acidic
property of the system, temperature programmed desorption (TPD)
of NH, has been done. Toluene alkylation by benzyl chloride has
been carried out for the evaluation of catalytic activity. The most
active system is found to be mixed Al/Zr pillarcd montrnorillonite.
Mohammed Yusuff, K K; Sridevi, Nadimpall; Jelaja, Padmavathy(Kluwer Academic Publishers, July 20, 2000)
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Abstract:
The nature of the diperiodatocuprate(III) (DPC) species present in aqueous alkaline medium has been investigated
by a kinetic and mechanistic study on the oxidation of iodide by DPC. The reaction kinetics were studied over the
1.0 ´ 10)3±0.1 mol dm)3 alkali range. The reaction order with respect to DPC, as well as iodide, was found to be
unity when [DPC] [I)]. In the 1.0 ´ 10)3±1.0 ´ 10)2 mol dm)3 alkali region, the rate decreased with increase in
the alkali concentration and a plot of the pseudo-®rst order rate constant, k versus 1/[OH)] was linear. Above
5.0 ´ 10)2 mol dm)3, a plot of k versus [OH)] was also linear with a non-zero intercept. An increase in ionic
strength of the reaction mixtures showed no e ect on k at low alkali concentrations, whereas at high concentrations
an increase in ionic strength leads to an increase in k. A plot of 1/k versus [periodate] was linear with an intercept in
both alkali ranges. Iodine was found to accelerate the reaction at the three di erent alkali concentrations employed.
The observed results indicated the following equilibria for DPC.
Ferrospinels of nickel, cobalt and copper and their sulphated analogues were prepared by the room temperature coprecipitation
route to yield samples with high surface areas. The intrinsic acidity among the ferrites was found to decrease in
the order: cobalt> nickel> copper. Sulphation caused an increase in the number of weak and medium strong acid sites,
whereas the strong acid sites were left unaffected. Electron donor studies revealed that copper ferrite has both the highest
proportion of strong sites and the lowest proportion of weak basic sites. All the ferrite samples proved to be good catalysts
for the benzoy lation of toluene with benzoyl chloride. copper and cobalt ferrites being much more active than nickel ferrite.
The catalytic activity for benzoylation was not much influenced by sulphation, but it increased remarkably with calcination
temperature of the catalyst. Surface Lewis acid sites, provided by the octahedral cations on the spinel surface, are suggested
to be responsible for the catalytic activity for the benzoylation reaction.
Sugunan, S; Renuka, N K(Indian Journal of Chemistry, February , 2001)
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Abstract:
Vapour phase methylation of phenol is carried out over La2O3 supported vanadia systems of various composition. The structural features and physico chemical characterisation of the catalysts are investigated. Orthovanadates are formed in addition to surface vanadyl species on the metal oxide support. No V2O5 crystallites are detected. The acid base properties of the oxides are studied by Hammett indicator method and decomposition of cyclohexanol.The data are correlated with the catalytic activity and selectivity of the products. Ring alkylation is found to be predominant over these catalysts.
Girish Kumar,K; Devala Rao, G; Chowdary, K P R(Indian Journal Of Pharmaceutical Sciences, February 7, 2001)
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Abstract:
Two simple and sensitive spectrophotometric methods(A and B) in the visible region have been developed for the determination of cefotaxime sodium (DFTS) in bulk and in dosage forms. Method A is based on the reaction of CFTS with nitrous acid under alkaline conditions to form a stable violet colored chromogen with absorption maximum of 560 nm and method B is based on the reaction of CFTS with1,10-phenanthroline and ferric chloride to form a red colored chromogen with the absorption maximum of 520 mm.The color obeyed Beer’s law in the concentration range of 100-500 µg/ml for method A and 1.6-16 µg/ml for method B, respectively.When pharmaceutical preparations containing CFTS were analysed, the results obtained by the proposed methods are in good agreement with the labeled amounts and are comparable with the results obtained using a UV spectrophotometric method.
Mohammed Yusuff, K K; Ahmed Yasir,Vakayil; Mohan Das,P N(Elsevier, International Journal of Inorganic Materials, August 12, 2001)
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Abstract:
Highly crystalline, ultra fine TiO (anatase) having high surface area has been prepared by thermal hydrolysis of titanyl sulphate 2
solution and characterized using B.E.T surface area measurements, XRD and chemical analysis. The dependence of surface area on
concentration of staffing solution, temperature of hydrolysis, duration of boiling and calcination temperature were also studied. As the
boiling temperature, duration of boiling and calcination temperature increased, the surface area of TiO formed decreased significantly. 2
On increasing calcination temperature, the crystallite size of TiO also increased and gradually the phase transformation to rutile took 2
place. The onset and completion temperatures of rutilation were 700 and 10008C, respectively