Indian Journal of Chemical Technology

 

VOLUME 8

NUMBER 5

SEPTEMBER 2001

CONTENTS

 

Papers

 

 

Reverse osmosis transport models evaluation: a new approach

335

 

Samir Y Vaidya, Amit V Simaria & Z V P Murthy

 

 

 

 

 

Magnetic fluid effect on fingero-imbibition phenomenon in secondary recovery process in transport phenomenon

344

 

Rajesh C Shah

 

 

 

 

 

Kinetic and mechanistic studies of saponification of industrially important distearates, dilaurates of glycol, propylene glycol, glycerol and glyceryl oleostearates

348

 

B Madhava Rao, K Gajanan & K Vijaya Mohan

 

 

 

 

 

Epoxy/Resole blends – A study of its degradation kinetics

357

 

Shailesh K Shukla & Deepak Srivastava

 

 

 

 

 

Catalytic esterification of benzyl alcohol with acetic acid by zeolites and their modified forms

362

 

K R Sharath, Sreenivasan Vijayashree & N Nagaraju

 

 

 

 

 

Beckmann rearrangement of cyclohexanone oxime over modified molecular sieves

368

 

K V V S B S R Murthy, M Chandrakala, S J Kulkarni and K V Raghavan

 

 

 

 

 

Synthesis of crosslinked methacrylic acid-co-N,N΄-methylene bis acrylamide sorbents for recovery of heavy metal ions from dilute solutions

371

 

H Hari Prasad, Ashrima Senger, Kavita Chauhan, Kirti M Popat
& Ptitpal Singh Anand

 

 

 

 

 

Synthesis, characterization and evaluation of heated rubber seed  oil and rubber seed-oil modified alkyd resins as binders in  surface coatings

378

 

A I Aigbodion, C K S Pillai, I O Bakare & L E Yahaya

 

 

 

 

 

Extraction of ethanol from aqueous solution by solvent extraction- liquid-liquid equilibrium of ethanol-water-1-butanol, ethanol- water-1-pentanol and ethanol-water-1-hexanol systems

385

 

M A Rahman, M S Rahman & M N Nabi

 

 

 

 

 

Effect of condensation product on bright zinc electrodeposition  from sulphate bath

390

 

Y Arthoba Naik, T V Venkatesha & P Vasudeva Nayak

 

 

 

 

 

Study on multilayer ethylcellulose matrices for controlled release of benzoic acid

396

 

Reena Singhal, A K Nagpal & G N Mathur

 

 

 

 

 

Effect of thermal treatment on photoelectrochemical and corrosion behaviour of CdSe

402

 

Md Rashid Tanveer & Umme Farva

 

 

Plain and ion pair thin layer chromatography of some herbicides  and related compounds on admixture of silica gel G and  barium sulphate in a single solvent system

408

 

Aditya K Misra, Sonu Pachauree & Upasana Gupta

 

 

 

 

 

Recycling of hydrocarbon from textile printing

413

 

Joseph Zacharia

 

 

 

 

 

Characteristics of air-borne dust emitted by opencast coal mining  in Jharia Coalfield

417

 

M K Ghosh & S R Majee

 

 

 

 

 

Notes

 

 

Synthesis of sulphur containing compounds over molecular sieve catalysts

425

 

G Kamalakar, P Srinivasu, M Ramakrishna Prasad, S J Kulkarni  & K V Raghavan

 

 

 

 

 

Educator

 

 

The rise and fall of the salitre (sodium nitrate) industry Jaime Wisniak & Ingrid Garcés

427

 

 

 

 

 

 

 


Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 335-343

 

Reverse osmosis transport models evaluation: A new approach

Samir Y Vaidya, Amit V Simaria & Z V P Murthy*

Department of Chemical Engineering, Dharmsinh Desai Institute of Technology (Deemed University),
P.B.No. 35, College Road, Nadiad 387 001, India

Received 8 February 2001; revised 12 June 2001; accepted 2 July 2001

Various transport models have been developed to describe the transport phenomena through reverse osmosis membrane. Such models give relationship amongst the operating variables, such as rejection, flux and driving force and membrane parameters that may include the physical properties of membrane. Knowing membrane parameters, one can predict the performance of membrane with minimum number of experiments, and can be extended to whole range of operating parameters without performing experiments. The available models are based on two concepts. One is on the basis of irreversible thermodynamics, and the others on the transport mechanisms. At present, the membrane transport models are used with the experimental data to estimate the parameters involved assuming that the mass transfer coefficient is available in the literature. The disadvantages of the same were reported recently in the literature. In the present paper an attempt has been made to evaluate the various models available in combination with the film theory .The experimental data obtained on the membrane is used to estimate the membrane parameters and mass transfer coefficient simultaneously, which will have more relevance than the existing methods. With this combined method, the models are compared.

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 344-347

Magnetic fluid effect on fingero-imbibition phenomenon in secondary recovery process in transport phenomenon

Rajesh C Shah

Department of Applied Sciences, VVP Engineering College, Kalavad Road, Rajkot 360 005, India

Received 4 October 2000; revised 12 March 2001; accepted 22 March 2001

Fingero-imbibition phenomenon through homogeneous porous media with magnetic fluid effect has been discussed numerically under some suitable set of initial and boundary conditions. This type of problem arises particularly in petroleum technology, geophysics, hydrogeology, etc.

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 7, September 2001, pp.348-356

 

Kinetic and mechanistic studies of saponification of industrially important distearates, dilaurates of glycol, propylene glycol,glycerol and glyceryl oleostearates

B Madhava Rao*, K Gajanan & K Vijaya Mohan

Department of Chemistry, Visvesvaraya Regional College of Engineering, Nagpur 440 011, India

Received 25 August 2000; revised 16 March 2001; accepted 26 March 2001

Kinetic and mechanistic studies of saponification of  seven structurally related and industrially important diesters have been investigated.  Time ratio method and Swain's standard data for series first order reactions have been utilized for the evaluation of rate data and thermodynamic parameters viz. DE¹,-DH¹, DG¹,DS¹  and log A for both the steps which involve the competitive and consecutive saponification reactions which also indicate the first step of saponification processes is quite faster than the second step and further more the laurates are more saponifiable  than stearates and oleostearate  in 72% alcohol-water moiety and in general these processes are much faster in acetone-water, dioxane-water, DMSO-water and DMF-water systems than in alcohol-water system.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 357-361

 

Epoxy/Resole blends—A study of its degradation kinetics

Shailesh K. Shuklaa & Deepak Srivastavaa*

aDepartment of Plastic Technology, H.B. Technological Institute, Kanpur 208 002, India

Received 10 July 2000; revised 15 March 2001; accepted 25 March 2001

The degradation kinetics of blends of resole with epoxy resin, having different weight ratios, has been studied by dynamic thermogravimetric analysis in nitrogen atmosphere at a heating rate of 150C/min. These blends were prepared by physical mixing and were cured with 40% polyamide (based on blend resin and polyamide). The degradation of each sample followed 0.67th order degradation kinetics, which was calculated by Coats and Redfern equation using best-fit analysis. This was further confirmed by linear regression analysis. The validity of data was checked by t-test statistical analysis. From this value of reaction order, activation energy (E) and pre-exponential factor (Z) were calculated. It was found that the activation energy increased while pre-exponential factor decreased as the resole content in the blend decreased from 100 to zero weight percent.

 

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 362-367

 

Catalytic esterification of benzyl alcohol with acetic acid by zeolites and their modified forms

K R Sharath, Sreenivasan Vijayashree & N Nagaraju*

Department of Chemistry, St. Joseph's College P.G. Centre, 46, Langford Road, Bangalore 560 027, India

Received 26 June 2000; revised 12 April 2001; accepted 23 May 2001

An attempt has been made to synthesise benzyl acetate from benzyl alcohol and acetic acid using Na-b, Na-Y, and Na-ZSM5 zeolites and their ion exchanged forms as catalysts. All the catalysts are characterised for their surface acidity, surface area and crystallinity by n-butyl amine titration method, BET and XRD respectively. The esterification reaction has been carried out in liquid phase taking the reactants in different acid to alcohol molar ratios (1:1, 1:2, 2:1). The amount of the ester formed has been estimated indirectly by titrating the unreacted acid with a standard base. The selectivity was found to be 100% with reasonably good yield (44-83%). The catalysts are also checked for their reusability.

 

 

Indian Journal of  Chemical Technology

Vol. 8, September 2001, pp.368-370

 

Beckmann rearrangement of cyclohexanone oxime over modified molecular sieves

K V V S B S R Murthy, M Chandrakala, S J Kulkarni* & K V Raghavan

Catalysis Group , Indian Institute of Chemical Technology, Hyderabad 500 007, India

Received 5 September 2000; revised 15 January 2001; accepted 24 January 2001

The vapour phase Beckmann rearrangement of cyclohexanone oxime to e-Caprolactum over silicoaluminophosphate (MSAPO-5, MSAPO-11) and MZSM-5 has been carried out. The yields of e-Caprolactum were 72.0 and 81.5% at 96.0 and 100% conversion over ZnSAPO-11 and TiSAPO-11 molecular sieves, respectively.

 

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 371-377

 

Synthesis of crosslinked methacrylic acid-co-N,N¢-methylene bis acrylamide sorbents for recovery of heavy metal ions from dilute solutions

 

H Hari Prasad, Ashrima Senger, Kavita Chauhan, Kirit M Popat & Pritpal Singh Anand*

Separation Technology Discipline, Central Salt & Marine Chemicals Research Institute, Bhavnagar 364 002, India

Received 19 February 2001; revised 4 June 2001; accepted 26 June 2001

Several crosslinked porous copolymers of methacrylic acid-N,N¢-methylene bis acrylamide were synthesized by suspension polymerisation using benzoylperoxide as the initiator. They were characterized for physico-chemical properties like, surface area, porosity and scientific weight capacity. The sorbents were further studied for adsorption of nickel and copper ions from spiked metal ion solutions in static and dynamic conditions. Concentration ratios of 1:60 and 1:30 have been achieved for nickel and copper ions respectively.

 

 

Indian Journal of Chemical Technology

Vol.8, September 2001, pp. 378-384

 

Synthesis, characterisation and evaluation of heated rubber seed oil and rubber seed oil-modified alkyd resins as binders in surface coatings

A I Aigbodiona*, C K S Pillaib, I O Bakarea & L E Yahayac

aEnd–Use Division, Rubber Research Institute of Nigeria, PMB 1049 Benin City, Nigeria

bPolymer Section, Regional Research Laboratory,Thiruvanathapuram 695 019, India

cDepartment of Chemistry, University of Benin, Benin City, Nigeria

Received 18 September 2000; revised 29 May 2001; accepted 15 June 2001

Rubber seed oil (RSO) heated at 300 ± 5 °C for six hours and RSO-modified alkyd resins were evaluated as binders for surface coatings. During heating of rubber seed oil, the bulk viscosity varied exponentially with time. GPC analysis showed that RSO consists of a very high molecular weight fraction that is uncommon in vegetable oil in addition to free fatty acid, mono– di–, tri-glycerides and oligomeric tryglycerides. Values of n and w of 7393 and 13076 respectively were found for RSO. Heated rubber seed oil (HRSO) gave n of 475 and w of 599; while RSO-modified alkyd samples of oil contents of 40% (I), 50% (II) and 60% (III) gave n of 3234, 1379 and 3304 respectively; and w of 6186, 2147 and 8406 respectively. HRSO is narrowest in size distribution compared to RSO and all the alkyd samples as indicated by their polydispersity indices. RSO was found to be semi–drying as the film remained tacky after long period (about 48h) of exposure. Heating enhanced its drying ability. The HRSO films exhibited reasonable pencil hardness and excellent resistance to acid and salt solution but poor resistance to alkali solution compared to the alkyd samples. The drying ability and chemical resistance of HRSO and RSO-modified alkyd were greatly enhanced by modification with cashewnut shell liquid-formaldehyde resin (10% w/w).

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 385-389

Extraction of ethanol from aqueous solution by solvent extraction-liquid-liquid equilibrium of ethanol-water-1-butanol, ethanol-water-1-pentanol and ethanol-water-1-hexanol systems

M A Rahman, M S Rahman* & M N Nabi

Department of Applied Chemistry & Chemical Technology, University of Rajshahi, Rajashahi, Bangladesh

Received 25 August 2000; revised 30 May 2001; accepted 12 June 2001

Solubility and liquid-liquid equilibrium data are presented for ethanol-water-1-butanol, ethanol-water-1-pentanol and ethanol-water-1-hexanol ternary systems at room temperature (30 ± 0.5)°C. From the above data binodal curves, tie lines and distribution curves have been determined with an aim to extract ethanol from the aqueous solution. Hand’s method has been used to correlate tie lines and to calculate co-ordinates of plait points. The heterogeneous region of 1-hexanol at room temperature has appeared to be broader than those of 1-pentanol and 1-butanol systems. The solubility of ethanol in these systems increases with decreasing number of carbon atoms in the chain of solvents giving higher values of distribution coefficient and consequent by lowering the separation factor. The distribution coefficients are greater than 1 and the separation factors are considerably greater than 2 for all the solvents studied. All the solvents are found to be suitable for extraction of ethanol from the aqueous solution.

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001. pp.390-395

Effect of condensation product on bright zinc electrodeposition from sulphate bath

Y Arthoba Naik, T V Venkatesha* & P Vasudeva Nayak

Department of Studies in Chemistry, Kuvempu University, Shankaraghatta577 451, India

Received 18 August 2000; revised 19  March 2001; accepted 29 March 2001

Zinc electroplating is carried out in presence of condensation product formed between dl-Alanine and Glutaraldehyde. The bath constituents are optimized through Hull cell experiments. Operating parameters such as pH, temperature, current density are also optimized. Current efficiency and throwing power are measured. Polarization study reveals high shift of potential towards negative direction in the presence of addition agents. Corrosion resistance test indicated good protection of steel by the coating. IR spectrum of the deposit shows the inclusion of the compound. SEM photomicrographs show fine grained deposit in the presence of addition agent. The consumption of brightener in the lab scale is 8 mL for 1000 amp-hour.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp.396-401

Study on multilayer ethylcellulose matrices for controlled release of benzoic acid

Reena Singhala*, A K Nagpala & G N Mathurb

a Department of Plastic Technology, H B T I , Kanpur  208 002, India

b D M S R D E , G T Road, Kanpur, India

Received 18 February 2000; revised 12 June 2001; accepted 28 June 2001

Matrix devices based on ethyl cellulose (EC) for controlled release (CR) applications were investigated for zero order release. These matrices were prepared by solvent casting and contained three or five layers arranged in symmetrical fashion with benzoic acid (BA) loaded only in inner layers; while the outermost layers were kept free from BA. It was found that three layer matrices maintain high release rates inspite of outer barrier layer and heavy initial release (burst effect) was significantly reduced; but linear release profile was not obtained. In five layer matrices four type of drug distribution profiles were tested and it was found that descending staircase type concentration gradient gave linear release profile, with enhanced release duration and reduced burst effect.

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 402-407

Effect of thermal treatment on photoelectrochemical and corrosion
behaviour of CdSe

 

Md Rashid Tanveer* & Umme Farva

Department of Chemistry, St. Andrew’s P.G. College, Gorakhpur 273 001, India

Received 25 April 2000; revised 4 June 2001; accepted 26 June 2001

Titanium based CdSe films of variable composition were prepared and subjected to thermal treatment. The formation of CdSe has been investigated using cyclic voltammetry. The swiftness of fall in current during deposition of CdSe films is expressed in terms of relaxation time under different conditions. Photoelectrochemical studies showed the alteration in the nature of semiconductivity on thermal treatment. Impedance measurements were carried out for the examination of corrosion characteristics.

 

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp.408-412

 

Plain and ion pair thin layer chromatography of some herbicides and
related compounds on admixture of silica gel G and barium sulphate in a single solvent system

Aditya K Misra*, Sonu Pachauree & Upasana Gupta

Department of Chemistry, NMSN Dass (PG) College, Badaun 243 601, India

Received 27 December 2000; revised 23 April 2001; accepted 7 May 2001

Some carboxylic acid herbicides and  related compounds such as - p-chlorophenoxyacetic acid, benzoic acid, cinnamic acid, b-naphthoxy acetic acid, a-naphthoxy acetic acid, b-naphthalene acetic acid, indole 3-acetic acid, indole propionic acid and gallic acid have been separated on silica gel G-barium sulphate coatings in different ratio using acetone as mobile phase. The ion pair thin layer chromatography (IPTLC) has shown the better possibilities of separating ternary mixtures of a herbicides and related compounds in comparison to the normal phase TLC.

 

 

Indian Journal of Chemical Technology

Vol. 8, September  2001. pp. 413-416

 

Recycling of hydrocarbon from textile printing

Joseph Zacharia*

The Bombay Textile Research Association, L.B.S. Marg, Ghatkopar (West), Mumbai 400 086, India

Received 24 July 2000; revised 15 March 2001; aceepted 24 March 2001

In India and in many developing countries hydrocarbons are still being used for pigment printing. In India, over 136 million litres of kerosene/mineral turpentine or solvent naphtha are used in pigment printing and also in reactive colour printing. After printing, the hydrocarbons vapours from the fabric is evaporated to the atmosphere during drying and curing. Due to inherent risk of explosion at the printing machine dryer, more air is pumped into the printing machine dryer to maintain the hydrocarbon vapour level below 0.5%. Thus the conventional vapour recovery systems are not suited for the recovery of this thin vapour. After several years of R&D activities for the first time in India, a hydrocarbon vapour recovery plant for textile printing has been developed. Subsequently, the plant has been setup and is been in continuous operation in a printing unit near Mumbai. The recovery efficiency is above 70%. This results in minimising air pollution and to save hydrocarbon which otherwise would have gone to the atmosphere. The recovered hydrocarbon is reused for printing.

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 417-424

 

Characteristics of air-borne dust emitted by
opencast coal mining in Jharia Coalfield

M K Ghose* & S R Majee

Centre of Mining Environment,Indian School of Mines,Dhanbad 826 004, India

Received 31st July 2000; revised 19 June 2001; accepted 20 June 2001

Opencast coal mining creates more air pollution problems in respect of dust and the fines contain coal particles, benzene soluble matters, etc.An investigation was conducted to evaluate the characteristics of the air-borne dust due to opencast coal mining. The study area has been described and the sources of air pollution were identified.Approach for the selection of air monitoring stations to assess the level of air pollution due to coal mining activities at different areas have been described. Suspended patriculate matter (SPM) concentration was found to be very high in work zone and surrounding locations.The status of air pollution in respect of diurnal and seasonal variations have been discussed. The SPM was subjected to particle size analysis by using different techniques. It was observed that the particulates were more respirable in nature and the median diameter was around 20 m. Dispersion of these finer particles was causing pollution problem at longer distances. Work zone was found to be more deteriorated in respect SPM, respirable particulate matter (RPM) and benzene soluble matters. Variations of weight percentages for different size ranges have been discussed on the basis of mining activities. Benzene soluble and anion fractions in SPM were found to be high in comparison to other areas.The characteristics of the air-bone dust have been discussed in respect of human health hazard and air quality standards.

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 425-426

 

Synthesis of sulphur containing compounds over molecular sieve catalysts

G Kamalakar, P Srinivasu, M Ramakrishna Prasad,
S J Kulkarni* & K V Raghavan

Catalysis Group, Indian Institute of Chemcal Technology,
Hyderabad 500 007, India

Received 9 August 2000; revised 27 February 2001;
accepted 27 March 2001

Cyclization of aliphatic butane1,4-diol in presence of hydrogen sulphide gas was carried out in the vapour phase. The catalysts used for this reaction are modified and unmodified ZSM-5 and HY molecular sieves. The effect of variation of catalyst and reaction temperature are studied for this reaction. A probable reaction mechanism for the formation of butane dithiol, which is used as protecting agent in the organic synthesis was proposed.

 

 

Indian Journal of Chemical Technology

Vol. 8, September 2001, pp. 427-438

The rise and fall of the salitre (sodium nitrate) industry

Jaime Wisniaka & Ingrid Garcésb

aDepartment of Chemical Engineering, Ben-Gurion University of the Negev, Beer-Sheva, Israel 84105

bDepartamento de Ingeniería Química, Universidad de Antofagasta, Antofagasta, Chile

 

The nitrate fields in Chile are exceptional for their mineral content and unknown origin and serve as an excellent example how a chemical technology can arise to create a very large and almost exclusive market, to be sent then almost into oblivion by competing technologies. The income from sodium nitrate export provided for many years almost 50% of the income of the Chilean government and a large part of the world needs for fertilizers. Development of the Haber-Bosch process for ammonia synthesis resulted in the crash of the dream and a serious economic crisis for Chile.

 

 

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