Mass transfer and chemical reaction on a distillation plate

A multistage distillation column in which mass transfer and a reversible chemical reaction occurred simultaneously, has been investigated to formulate a technique by which this process can be analysed or predicted. A transesterification reaction between ethyl alcohol and butyl acetate, catalysed by concentrated sulphuric acid, was selected for the investigation and all the components were analysed on a gas liquid chromatograph. The transesterification reaction kinetics have been studied in a batch reactor for catalyst concentrations of 0.1 - 1.0 weight percent and temperatures between 21.4 and 85.0 °C. The reaction was found to be second order and dependent on the catalyst concentration at a given temperature. The vapour liquid equilibrium data for six binary, four ternary and one quaternary systems are measured at atmospheric pressure using a modified Cathala dynamic equilibrium still. The systems with the exception of ethyl alcohol - butyl alcohol mixtures, were found to be non-ideal. Multicomponent vapour liquid equilibrium compositions were predicted by a computer programme which utilised the Van Laar constants obtained from the binary data sets. Good agreement was obtained between the predicted and experimental quaternary equilibrium vapour compositions. Continuous transesterification experiments were carried out in a six stage sieve plate distillation column. The column was 3" in internal diameter and of unit construction in glass. The plates were 8" apart and had a free area of 7.7%. Both the liquid and vapour streams were analysed. The component conversion was dependent on the boilup rate and the reflux ratio. Because of the presence of the reaction, the concentration of one of the lighter components increased below the feed plate. In the same region a highly developed foam was formed due to the presence of the catalyst. The experimental results were analysed by the solution of a series of simultaneous enthalpy and mass equations. Good agreement was obtained between the experimental and calculated results.

A small scale Multi-effect Distillation (MED) unit for rural micro enterprises:part I-design and fabrication

Removal of dissolved salts and toxic chemicals in water, especially at a few parts per million (ppm) levels is one of the most difficult problems. There are several methods used for water purification. The choice of the method depends mainly on the level of feed water salinity, source of energy and type of contaminants present. Distillation is an age old method which can remove all types of dissolved impurities from contaminated water. In multiple effect distillation (MED) latent heat of steam is recycled several times to produce many units of distilled water with one unit of primary steam input. This is already being used in large capacity plants for treating sea water. But the challenge lies in designing a system for small scale operations that can treat a few cubic meters of water per day, especially suitable for rural communities where the available water is brackish. A small scale MED unit with an extendable number of effects has been designed and analyzed for optimum yield in terms of total distillate produced. © 2010 Elsevier B.V.

Solvent extraction of phosphoric acid

This work investigated the purification of phosphoric acid using a suitable organic solvent, followed by re-extraction of the acid from the solvent using water. The work consisted of practical batch and continuous studies and the economics and design of a full scale plant, based on the experimental data. A comprehensive literature survey on the purification of wet process phosphoric acid by organic solvents is presented and the literature describing the design and operation of mixer-settlers has also been reviewed. In batch studies, the equilibrium and distribution curves for the systems water-phosphoric acid-solvent for Benzaldehyde, Cyclohexanol and Methylisobutylketone (MIBK) were determined together with hydrodynamic characteristics for both pure and impure systems. The settling time increased with acid concentration, but power input had no effect. Drop size was found to reduce with acid concentration and power input. For the continuous studies a novel horizontal mixer~settler cascade was designed, constructed and operated using pure and impure acid with MIBK as the solvent. The cascade incorporates three air turbine agitated, cylindrical 900 ml mixers, and three cylindrical 200 ml settlers with air-lift solvent interstage transfer. Mean drop size in the fully baffled mixer was correlated. Drop size distributions were log-normal and size decreased with acid concentration and power input and increased with dispersed phase hold-up. Phase inversion studies showed that the width of the ambivalent region depended upon rotor speed, hold-up and acid concentration. Settler characteristics were investigated by measuring wedge length. Distribution coefficients of impurities and acid were also investigated. The following optimum extraction conditions were found: initial acid concentration 63%, phase ratio of solvent to acid 1:1 (v/v), impeller speed recommended 900 r.p.m. In the washing step the maximum phase ratio of solvent to water was 8:1 (v/v). Work on phosphoric acid concentration involved constructing distillation equipment consisting of a 10& spherical still. A 100 T/d scale detailed process design including capital cost, operating cost and profitability was also completed. A profit model for phosphoric acid extraction was developed and maximised. Recommendations are made for both the application of the results to a practical design and for extensions of the study.

Gas distribution in shallow large diameter packed beds

It is important to maintain a uniform distribution of gas and liquid in large diameter packed columns to maintain mass transfer efficiency on scaling up. This work presents measurements and methods of evaluating maldistributed gas flow in packed columns. Little or no previous work has been done in this field. A gas maldistribution number, F, was defined, based on point to point velocity variations in the gas emerging from the top of packed beds. f has a minimum value for a uniformly distributed flow and much larger values for maldistributed flows. A method of testing the quality of vapour distributors is proposed, based on "the variation of f with packed height. A good gas distributor requires a short packed depth to give a good gas distribution. Measurements of gas maldistribution have shown that the principle of dynamic similarity is satisfied if two geometrically similar beds are operated at the same Reynold's number. The validity of f as a good measure of gas maldistribution, and the principle of dynamic similarity are tested statistically by Multi-Factor Analysis of the variance, and visually by the response "surfaces technique. Pressure distribution has been measured in a model of a large diameter packed bed, and shown to be associated with the velocity of the gas in a tangential feed pipe. Two simplified theoretical models are proposed to describe the flow of gases through packed beds and to support the principle of dynamic similarity. These models explain why the packed bed itself causes the flow of gas to become more uniformly distributed. A 1.2m. diameter scaled-down model was constructed geometrically similar to a 7.3m. diameter vacuum crude distillation column. The previously known internal cylinder gas distributor was tested. Three new distributors suitable for use in a large diameter column were developed and tested, these are: Internal Cylinder with Slots and Cross Baffles, Internal Cylinder with Guides in the Annulus, Internal Cylinder with Internal Cross Baffles - It has been shown that this is an excellent distributor.

The use of flow control devices to improve the flow pattern and throughput of sieve trays

Compared to packings trays are more cost effective column internals because they create a large interfacial area for mass transfer by the interaction of the vapour on the liquid. The tray supports a mass of froth or spray which on most trays (including the most widely used sieve trays) is not in any way controlled. The two important results of the gas/liquid interaction are the tray efficiency and the tray throughput or capacity. After many years of practical experience, both may be predicted by empirical correlations, despite the lack of understanding. It is known that the tray efficiency is in part determined by the liquid flow pattern and the throughput by the liquid froth height which in turn depends on the liquid hold-up and vapour velocity. This thesis describes experimental work on sieve trays in an air-water simulator, 2.44 m in diameter. The liquid flow pattern, for flow rates similar to those used in commercial scale distillation, was observed experimentally by direct observation; by water-cooling, to simulate mass transfer; use of potassium permanganate dye to observe areas of longer residence time; and by height of clear liquid measurements across the tray and in the downcomer using manometers. This work presents experiments designed to evaluate flow control devices proposed to improve the gas liquid interaction and hence improve the tray efficiency and throughput. These are (a) the use of intermediate weirs to redirect liquid to the sides of the tray so as to remove slow moving/stagnant liquid and (b) the use of vapour-directing slots designed to use the vapour to cause liquid to be directed towards the outlet weir thus reducing the liquid hold-up at a given rate i.e. increased throughput. This method also has the advantage of removing slow moving/stagnant liquid. In the experiments using intermediate weirs, which were placed in the centre of the tray. it was found that in general the effect of an intermediate weir depends on the depth of liquid downstream of the weir. If the weir is deeper than the downstream depth it will cause the upstream liquid to be deeper than the downstream liquid. If the weir is not as deep as deep as the downstream depth it may have little or no effect on the upstream depth. An intermediate weir placed at an angle to the direction of flow of liquid increases the liquid towards the sides of the tray without causing an increase in liquid hold-up/ froth height. The maximum proportion of liquid caused to flow sideways by the weir is between 5% and 10%. Experimental work using vapour-directing slots on a rectangular sieve tray has shown that the horizontal momentum that is imparted to the liquid is dependent upon the size of the slot. If too much momentum is transferred to the liquid it causes hydraulic jumps to occur at the mouth of the slot coupled with liquid being entrained, The use of slots also helps to eliminate the hydraulic gradient across sieve trays and provides a more uniform froth height on the tray. By comparing the results obtained of the tray and point efficiencies, it is shown that a slotted tray reduces both values by approximately 10%. This reduction is due to the fact that with a slotted tray the liquid has a reduced residence time Ion the tray coupled also with the fact that large size bubbles are passing through the slots. The effectiveness of using vapour-directing slots on a full circular tray was investigated by using dye to completely colour the biphase. The removal of the dye by clear liquid entering the tray was monitored using an overhead camera. Results obtained show that the slots are successful in their aim of reducing slow moving liquid from the sides of the tray, The net effect of this is an increase in tray efficiency. Measurements of slot vapour-velocity found it to be approximately equal to the hole velocity.

The synthesis of novel biodegradable polyesters and copolyesters from anhydrosulfites

This thesis was concerned primarily with the synthesis and the ring-opening polymerisation of anhydrosulfites (1,3,2-dioxa-thiolan-4-one-2-oxides), and secondly with the copolymerisation of anhydrosulfites with -caprolactone. The polyesters and copolyesters synthesised are of considerable interest in medical applications and also for use as environmental friendly packaging. A range of anhydrosulfites were prepared according to an established method. Aliphatic anhydrosulfites were obtained with a level of purity satisfactory for polymerisation whereas aromatic anhydrosulfites decomposed during distillation and purification by chromatographic techniques. Aliphatic anhydrosulfites with a substituent, such as methyl, isopropyl, n-butyl and isobutyl were studied by NMR spectroscopy. Analysis of these spectra revealed that the five-membered anhydrosulfite ring was puckered and that when the substituent was bulky, rotations about the alkyl chains were restricted. A wide range of anionic initiators may be used to initiate anhydrosulfites. Lithium alkyls turned out to be more successful than alkali metal alkoxides and amides. The molecular weights were found to depend on the basicity of the initiator, the monomer-to-initiator ratio, the nature of the solvent and the polymerisation temperature. The molecular weight M0 of poly(L-lactic acid) ranged from (0.5 to 6)x104. Highly crystalline and purely isotactic poly(lactic acid) was synthesised from L-lactic acid anhydrosulfite (L-LAAS) whereas DL-LAAS led to an amorphous polymer with randomly distributed D-and L-lactic units. This indicated that this polymerisation was not stereoselective. However, the bulkiness of the substituent in the anhydrosulfites molecule was found to influence the stereoselectivity of the polymerisation, thus polyesters with isobutyl or n-butyl pendant group were preferentially isotactic. Block-copolymers of ε-caprolactone and several anhydrosulfites were successfully produced. Block-copolymers of LAAS with ε-caprolactone were also synthesised, but the incorporation of caprolactone units was rather small. In contrast, random copolymerisation of LAAS and ε-caprolactone led to polymers with blocky structures similar to those obtained in the block-copolymerisation of LAAS with  ε-caprolactone.

Real-time process plant fault diagnosis

Operators can become confused while diagnosing faults in process plant while in operation. This may prevent remedial actions being taken before hazardous consequences can occur. The work in this thesis proposes a method to aid plant operators in systematically finding the causes of any fault in the process plant. A computer aided fault diagnosis package has been developed for use on the widely available IBM PC compatible microcomputer. The program displays a coloured diagram of a fault tree on the VDU of the microcomputer, so that the operator can see the link between the fault and its causes. The consequences of the fault and the causes of the fault are also shown to provide a warning of what may happen if the fault is not remedied. The cause and effect data needed by the package are obtained from a hazard and operability (HAZOP) study on the process plant. The result of the HAZOP study is recorded as cause and symptom equations which are translated into a data structure and stored in the computer as a file for the package to access. Probability values are assigned to the events that constitute the basic causes of any deviation. From these probability values, the a priori probabilities of occurrence of other events are evaluated. A top-down recursive algorithm, called TDRA, for evaluating the probability of every event in a fault tree has been developed. From the a priori probabilities, the conditional probabilities of the causes of the fault are then evaluated using Bayes' conditional probability theorem. The posteriori probability values could then be used by the operators to check in an orderly manner the cause of the fault. The package has been tested using the results of a HAZOP study on a pilot distillation plant. The results from the test show how easy it is to trace the chain of events that leads to the primary cause of a fault. This method could be applied in a real process environment.

The separation of hydrogen and carbon monoxide using polymer membranes

This work studies the development of polymer membranes for the separation of hydrogen and carbon monoxide from a syngas produced by the partial oxidation of natural gas. The CO product is then used for the large scale manufacture of acetic acid by reaction with methanol. A method of economic evaluation has been developed for the process as a whole and a comparison is made between separation of the H2/CO mixture by a membrane system and the conventional method of cryogenic distillation. Costs are based on bids obtained from suppliers for several different specifications for the purity of the CO fed to the acetic acid reactor. When the purity of the CO is set at that obtained by cryogenic distillation it is shown that the membrane separator offers only a marginal cost advantage. Cost parameters for the membrane separation systems have been defined in terms of effective selectivity and cost permeability. These new parameters, obtained from an analysis of the bids, are then used in a procedure which defines the optimum degree of separation and recovery of carbon monoxide for a minimum cost of manufacture of acetic acid. It is shown that a significant cost reduction is achieved with a membrane separator at the optimum process conditions. A method of "targeting" the properties of new membranes has been developed. This involves defining the properties for new (hypothetical -yet to be developed) membranes such that their use for the hydrogen/carbon monoxide separation will produce a reduced cost of acetic acid manufacture. The use of the targeting method is illustrated in the development of new membranes for the separation of hydrogen and carbon monoxide. The selection of polymeric materials for new membranes is based on molecular design methods which predict the polymer properties from the molecular groups making up the polymer molecule. Two approaches have been used. One method develops the analogy between gas solubility in liquids and that in polymers. The UNIFAC group contribution method is then used to predict gas solubility in liquids. In the second method the polymer Permachor number, developed by Salame, has been correlated with hydrogen and carbon monoxide permeabilities. These correlations are used to predict the permeabilities of gases through polymers. Materials have been tested for hydrogen and carbon monoxide permeabilities and improvements in expected economic performance have been achieved.

Flow patterns on sieve trays

Studies into gas-liquid flow patterns were carried out on commercial scale sieve trays where the ratio of froth depth to flow path length is typical of that found in practice. Experiments were conducted on a 2.44 m diameter air-water distillation simulator, in which flow patterns were investigated by direct observation, using directional flow pointers; by water cooling, to simulate mass transfer; and by height of clear liquid measurements across the tray. The flow rates used are typical of those found in practice. The approach adopted was to investigate the effect of the gas flow on the liquid flow by comparing water only flow patterns across an unperforated tray with air-water flow patterns on perforated trays. Initial gas-liquid contacting experiments on the 6.35 mm hole tray showed that, under certain conditions, the gas flow pattern beneath the test tray can have a significant effect on the tray liquid flow pattern such that gas-driven liquid circulation was produced. This was found to be a function of this particular air-water simulator design, and as far as is known this is the first time that this phenomenon has been observed. Consequently non-uniform gas flow effects were removed by modification of the gas distribution system. By eliminating gas circulation effects, the effect of the gas flow on the separation of liquid flow was similar to that obtained on the 1.0 mm hole tray (Hine, 1990). That is, flow separation occurred at the ends of the inlet downcomer which produced large circulating zones along the tray segments both on the non-perforated and perforated trays. The air when forced through the liquid, inhibited circulating flow such that it only occurred at high water inlet velocities. With the 6.35 mm hole tray, the growth and velocity of circulating flow was reduced at high superficial air velocities, and in the experiments to simulate distillation, liquid was in forward flow over most of the tray.

Omnigen:providing electricity, food preparation, cold storage and pure water using a variety of local fuels

We describe a polygeneration system that can run on neat plant oils, such as Jatropha and Pongamia, or standard diesel fuel. A prototype has been constructed using a compression ignition engine of 9.9 kW shaft output. It consumes 3 L/h of fuel and will produce 40 kg/h of ice by means of an adsorption refrigerator powered from the engine jacket heat. Steaming of rice, deep and shallow frying, and other types of food preparation heated by the exhaust gas have been demonstrated. In addition, the feasibility of producing distilled water by means of multiple-effect distillation powered by the engine waste heat is shown. Overall plant efficiency and potential savings in greenhouse gas emissions are discussed. © 2012 Elsevier Ltd.

Trigeneration using biomass energy for sustainable development

Purpose: The paper aims to design and prove the concept of micro-industry using trigeneration fuelled by biomass, for sustainable development in rural NW India. Design/methodology/approach: This is being tested at village Malunga, near Jodhpur in Rajasthan. The system components comprise burning of waste biomass for steam generation and its use for power generation, cooling system for fruit ripening and the use of steam for producing distilled water. Site was selected taking into account the local economic and social needs, biomass resources available from agricultural activities, and the presence of a NGO which is competent to facilitate running of the enterprise. The trigeneration system was designed to integrate off-the-shelf equipment for power generation using boilers of approximate total capacity 1 tonne of fuel per hour, and a back-pressure steam turbo-generator (200 kW). Cooling is provided by a vapour absorption machine (VAM). Findings: The financial analysis indicates a payback time of less than two years. Nevertheless, this is sensitive to market fluctuations and availabilities of raw materials. Originality/value: Although comparable trigeneration systems already exist in large food processing industries and in space heating and cooling applications, they have not previously been used for rural micro-industry. The small-scale (1-2 m3/h output) multiple effect distillation (3 effect plus condenser) unit has not previously been deployed at field level. © Emerald Group Publishing Limited.

Chemometric modelling to relate antioxidants, neutral lipid fatty acids and flavour components in chicken breast

Relationships among quality factors in retailed free-range, corn-fed, organic, and conventional chicken breasts (9) were modeled using chemometric approaches. Use of principal component analysis (PCA) to neutral lipid composition data explained the majority (93%) of variability (variance) in fatty acid contents in 2 significant multivariate factors. PCA explained 88 and 75% variance in 3 factors for, respectively, flame ionization detection (FID) and nitrogen phosphorus (NPD) components in chromatographic flavor data from cooked chicken after simultaneous distillation extraction. Relationships to tissue antioxidant contents were modeled. Partial least square regression (PLS2), interrelating total data matrices, provided no useful models. By using single antioxidants as Y variables in PLS (1), good models (r2 values > 0.9) were obtained for alpha-tocopherol, glutathione, catalase, glutathione peroxidase, and reductase and FID flavor components and among the variables total mono and polyunsaturated fatty acids and subsets of FID, and saturated fatty acid and NPD components. Alpha-tocopherol had a modest (r2 = 0.63) relationship with neutral lipid n-3 fatty acid content. Such factors thus relate to flavor development and quality in chicken breast meat.

A micro industry with closed energy and water cycles for sustainable rural development

Sustainable development requires combining economic viability with energy and environment conservation and ensuring social benefits. It is conceptualized that for designing a micro industry for sustainable rural industrialization, all these aspects should be integrated right up front. The concept includes; (a) utilization of local produce for value addition in a cluster of villages and enhancing income of the target population; (b) use of renewable energy and total utilization of energy generated by co and trigeneration (combining electric power production with heat utilization for heating and cooling); (c) conservation of water and complete recycling of effluents; (d) total utilization of all wastes for achieving closure towards a zero waste system. Enhanced economic viability and sustainability is achieved by integration of appropriate technologies into the industrial complex. To prove the concept, a model Micro Industrial Complex (MIC) has been set up in a semi arid desert region in Rajasthan, India at village Malunga in Jodhpur district. A biomass powered boiler and steam turbine system is used to generate 100-200 KVA of electric power and high energy steam for heating and cooling processes downstream. The unique feature of the equipment is a 100-150 kW back-pressure steam turbine, utilizing 3-4 tph (tonnes per hour) steam, developed by M/s IB Turbo. The biomass boiler raises steam at about 20 barg 3 tph, which is passed through a turbine to yield about 150 kW of electrical power. The steam let out at a back pressure of 1-3 barg has high exergy and this is passed on as thermal energy (about 2 MW), for use in various applications depending on the local produce and resources. The biomass fuel requirement for the boiler is 0.5-0.75 tph depending on its calorific value. In the current model, the electricity produced is used for running an oil expeller to extract castor oil and the castor cake is used as fuel in the boiler. The steam is used in a Multi Effect Distillation (MED) unit for drinking water production and in a Vapour Absorption Machine (VAM) for cooling, for banana ripening application. Additional steam is available for extraction of herbs such as mint and processing local vegetables. In this paper, we discuss the financial and economic viability of the system and show how the energy, water and materials are completely recycled and how the benefits are directed to the weaker sections of the community.

A cost-effective steam-driven RO plant for brackish groundwater

Desalination is a costly means of providing freshwater. Most desalination plants use either reverse osmosis (RO) or thermal distillation. Both processes have drawbacks: RO is efficient but uses expensive electrical energy; thermal distillation is inefficient but uses less expensive thermal energy. This work aims to provide an efficient RO plant that uses thermal energy. A steam-Rankine cycle has been designed to drive mechanically a batch-RO system that achieves high recovery, without the high energy penalty typically incurred in a continuous-RO system. The steam may be generated by solar panels, biomass boilers, or as an industrial by-product. A novel mechanical arrangement has been designed for low cost, and a steam-jacketed arrangement has been designed for isothermal expansion and improved thermodynamic efficiency. Based on detailed heat transfer and cost calculations, a gain output ratio of 69-162 is predicted, enabling water to be treated at a cost of 71 Indian Rupees/m3 at small scale. Costs will reduce with scale-up. Plants may be designed for a wide range of outputs, from 5 m3/day, up to commercial versions producing 300 m3/day of clean water from brackish groundwater.

Liquid desiccant dehumidification and regeneration process to meet cooling and freshwater needs of desert greenhouses

Agriculture accounts for ~70% of freshwater usage worldwide. Seawater desalination alone cannot meet the growing needs for irrigation and food production, particularly in hot, desert environments. Greenhouse cultivation of high-value crops uses just a fraction of freshwater per unit of food produced when compared with open field cultivation. However, desert greenhouse producers face three main challenges: freshwater supply, plant nutrient supply, and cooling of the greenhouse. The common practice of evaporative cooling for greenhouses consumes large amounts of fresh water. In Saudi Arabia, the most common greenhouse cooling schemes are fresh water-based evaporative cooling, often using fossil groundwater or energy-intensive desalinated water, and traditional refrigeration-based direct expansion cooling, largely powered by the burning of fossil fuels. The coastal deserts have ambient conditions that are seasonally too humid to support adequate evaporative cooling, necessitating additional energy consumption in the dehumidification process of refrigeration-based cooling. This project evaluates the use of a combined-system liquid desiccant dehumidifier and membrane distillation unit that can meet the dual needs of cooling and freshwater supply for a greenhouse in a hot and humid environment.