Structured packing in air distillation

An economic analysis has been performed to establish when it is advantageous to use structured packing in air separation plant. A model of a low pressure cycle was developed to calculate the power saved when packing is used, and cost models were developed for the columns and cold box. The rate of return was calculated on the extra investment required for a packed plant based on the annual power saving. Structured packing was found to be economic only in larger plants, where economies of scale mean that the increased capital cost becomes less significant compared with the power saved. It was also found that different sized plants favour different packings. The analysis identified that the packing variable with the biggest impact on the economic balance was the efficiency and that increasing the efficiency of current packings could enhance their balance in air distillation. A new packing was therefore developed to have a higher efficiency than conventional ones. The vapour phase resistance was targeted for reduction, since most packing models predict this to be dominant. The final shape was chosen as the easiest and most economic to make. It has converging and diverging channels and was manufactured in two specific areas and with two block heights by Tianjin University Packing Factory. A 0.3 m diameter distillation column test rig was designed, built and commissioned with the standard Sulzer Mellapak 500YW. It was then used to test the new packing alongside some standard ones. Because the packings had different specific areas, correlations of published results were developed to allow a true comparison to be made. The test results show that, unexpectedly, the packings with 0.1 m high blocks have an efficiency about 8% greater than the standard 0.2 m blocks. The new shape as implemented in the 350Y packing shows an additional 7% greater efficiency, so it is 15% better than a standard packing with the same area. It has a better efficiency than the Mellapak 500YW and the higher capacity associated with its lower area. The new 500Y did not show a significant advantage.

Optimal packing for cascaded regenerative transmission based on phase sensitive amplifiers

We investigate the transmission performance of advanced modulation formats in nonlinear regenerative channels based on cascaded phase sensitive amplifiers. We identify the impact of amplitude and phase noise dynamics along the transmission line and show that after a cascade of regenerators, densely packed single ring PSK constellations outperform multi-ring constellations. The results of this study will greatly simplify the design of future nonlinear regenerative channels for ultra-high capacity transmission

Optimal packing for cascaded regenerative transmission based on phase sensitive amplifiers

We investigate the transmission performance of advanced modulation formats in nonlinear regenerative channels based on cascaded phase sensitive amplifiers. We identify the impact of amplitude and phase noise dynamics along the transmission line and show that after a cascade of regenerators, densely packed single ring PSK constellations outperform multi-ring constellations. The results of this study will greatly simplify the design of future nonlinear regenerative channels for ultra-high capacity transmission. © 2013 Optical Society of America.

Efficient packing for phase regenerative channels

We compare the performance of advanced modulation formats in cascaded phase regenerative systems and demonstrate the importance of constellation optimization to the transfer function characteristics of the regenerator. © 2013 IEEE.

Solubilisation of drugs within liposomal bilayers:alternatives to cholesterol as a membrane stabilising agent

Objectives The aim of this work was to investigate the effect of cholesterol on the bilayer loading of drugs and their subsequent release and to investigate fatty alcohols as an alternative bilayer stabiliser to cholesterol. Methods The loading and release rates of four low solubility drugs (diazepam, ibuprofen, midazolam and propofol) incorporated within the bilayer of multilamellar liposomes which contained a range of cholesterol (0–33 mol/mol%) or a fatty alcohol (tetradecanol, hexadecanol and octadecanol) were investigated. The molecular packing of these various systems was also investigated in Langmuir monolayer studies. Key findings Loading and release of drugs within the liposome bilayer was shown to be influenced by their cholesterol content: increasing cholesterol content was shown to reduce drug incorporation and inclusion of cholesterol in the bilayer changed the release profile of propofol from zero-order, for phosphatidyl choline only liposomes, to a first-order model when 11 to 33 total molar % of cholesterol was present in the formulation. At higher bilayer concentrations substitution of cholesterol with tetradecanol was shown to have less of a detrimental impact on bilayer drug loading. However, the presence of cholesterol within the liposome bilayer was shown to reduce drug release compared with fatty alcohols. Monolayer studies undertaken showed that effective mean area per molecule for a 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC) : cholesterol mixture deviated by 9% from the predicted area compared with 5% with a similar DSPC : tetradecanol mixture. This evidence, combined with cholesterol being a much more bulky structure, indicated that the condensing influence of tetradecanol was less compared with cholesterol, thus supporting the reduced impact of tetradecanol on drug loading and drug retention. Conclusions Liposomes can be effectively formulated using fatty alcohols as an alternative bilayer stabiliser to cholesterol. The general similarities in the characteristics of liposomes containing fatty alcohols or cholesterol suggest a common behavioural influence for both compounds within the bilayer.

Design and characterisation of novel blends of poly(lactic acid)

This thesis is concerned with the effect of polymer structure on miscibility of the three component blends based on poly(lactic acid) (PLA) with using blending techniques. The examination of novel PLA homologues (pre-synthesised poly(a-esters)), including a range of aliphatic and aromatic poly(a-esters) is an important aspect of the work. Because of their structural simplicity and similarity to PLA, they provide an ideal system to study the effect of polyester structures on the miscibility of PLA polymer blends. The miscibility behaviour of the PLA homologues is compared with other aliphatic polyesters (e.g. poly(e-caprolactone) (PCL), poly(hydroxybutyrate hydroxyvalerate) (P(HB-HV)), together with a series of cellulose-based polymers (e.g. cellulose acetate butyrate (CAB)). The work started with the exploration the technique used for preliminary observation of the miscibility of blends referred to as “a rapid screening method” and then the miscibility of binary blends was observed and characterised by percent transmittance together with the Coleman and Painter miscibility approach. However, it was observed that symmetrical structures (e.g. a1(dimethyl), a2(diethyl)) promote the well-packing which restrict their chains from intermingling into poly(L-lactide) (PLLA) chains and leads the blends to be immiscible, whereas, asymmetrical structures (e.g. a4(cyclohexyl)) behave to the contrary. a6(chloromethyl-methyl) should interact well with PLLA because of the polar group of chloride to form interactions, but it does not. It is difficult to disrupt the helical structure of PLLA. PLA were immiscible with PCL, P(HB-HV), or compatibiliser (e.g. G40, LLA-co-PCL), but miscible with CAB which is a hydrogen-bonded polymer. However, these binary blends provided a useful indication for the exploration the novel three component blends. In summary, the miscibility of the three-component blends are miscible even if only two polymers are miscible. This is the benefit for doing the three components blend in this thesis, which is not an attempt to produce a theoretical explanation for the miscibility of three components blend system.

Achieving internal process benchmarking:guidance from BASF

Purpose - The purpose of the work discussed in this paper is to understand, analyse and benchmark the "Packing and Filling" processes within BASF. A benchmarking project is described in detail which aimed to cover sites in different countries that supplied many different variants of finished goods in order to establish best practice and then to generate some options for their implementation. Design/methodology/approach - The project used an adaptation of accepted benchmarking methodology combined with other techniques (such as rich picture generation, and cluster analysis) to maximise the insight generated. Findings - The findings of the research showed that one of the main factors effecting the process was how third parties were used (e.g. extent and nature of out-sourcing, and its degree of centralisation). Research limitations/ implications - The exercise was challenged by the selection of suitably similar benchmarking candidates because the environment was complex and highly varied; the paper explains practical solutions for dealing with this challenge. Practical limitations - Strategic and tactical options are outlined at the end of the paper and will have applicability to other organisations and industries that are looking to find the answers to frequently asked questions about how to successfully implement an internal process benchmarking project in a large complex organisation that has high variety in end products and delivery methods. Originality/value - The methodology described in this paper is of a proprietary and unique nature. The paper is structured around some key questions commonly asked of benchmarking, and the answers are provided via a real in-depth case study from BASF that spans 4 sites in 3 countries using 15 different filling lines. © Emerald Group Publishing Limited.

Coalescence of secondary dispersions in fibrous beds

SUMMARY A study has been made of the coalescence of secondary dispersions in a fibrous bed. The literature pertaining to the formation, hydrodynamic behaviour and methods of separation of droplets less than one hundred micrometres in diameter has been reviewed with particular reference to fibrous bed coalescers. The main operating parameters were identified as inlet drop size distribution, phase ratio, superficial velocity and the thickness and voidage of the bed . A recirculatory rig with interchangeable fibrous bed pads was designed and operated with toluene-water dispersions generated by a combination of centrifugal pumps . Inlet drop sizes were analysed using a Coulter Counter and outlet drops were sized photographically. A novel technique, involving conductivity measur ements at different planes in the bed, was developed to measure hold up distribution. Single phase flow and two phase flow pressure drops were correlated by a Blake-Kozeny type equation. Exit drop size was independent of inlet drop size distribution and phase ratio but a function of superficialvelocity and packing thickness. Average bed hold up was independent of inlet drop size distribution and phase ratio, but decreased with increase in superficial velocity. Hold up was not evenly distributed in the bed, the highest value occurred at the inlet followed by a sharp -2 drop at approximately 1.2 x 10 m. Hold up remained constant throughout the rest of the bed until the exit plane, where it increased. From the results, a mechanism is postulated involving: (a) Capture of the inlet drops followed by interdrop coalescence until an equilibrium value is reached. (b) Equilibrium size droplets flowing as rivulets through the intermediate portion of the bed, and (c) Each rivulet forms droplets at the exit face, which detach by a 'drip point' mechanism.

Polymer fractionation by continuous chromatography

A review is given of general chromatographic theory, the factors affecting the performance of chromatographi c columns, and aspects of scale-up of the chromatographic process. The theory of gel permeation chromatography (g. p. c.) is received, and the results of an experimental study to optimize the performance of an analytical g.p.c. system are reported. The design and construction of a novel sequential continuous chromatographic refining unit (SCCR3), for continuous liquid-liquid chromatography applications, is described. Counter-current operation is simulated by sequencing a system of inlet and outlet port functions around a connected series of fixed, 5.1 cm internal diameter x 70 cm long, glass columns. The number of columns may be varied, and, during this research, a series of either twenty or ten columns was used. Operation of the unit for continuous fractionation of a dextran polymer (M. W. - 30,000) by g.p.c. is reported using 200-400 µm diameter porous silica beads (Spherosil XOB07S) as packing, and distilled water for the mobile phase. The effects of feed concentration, feed flow rate, and mobile and stationary phase flow rates have been investigated, by means of both product, and on-column, concentrations and molecular weight distributions. The ability to operate the unit successfully at on-column concentrations as high as 20% w/v dextran has been demonstrated, and removal of both high and low molecular weight ends of a polymer feed distribution, to produce products meeting commercial specifications, has been achieved. Equivalent throughputs have been as high as 2.8 tonnes per annum for ten columns, based on continuous operation for 8000 hours per annum. A concentration dependence of the equilibrium distribution coefficient, KD observed during continuous fractionation studies, is related to evidence in the literature and experimental results obtained on a small-scale batch column. Theoretical treatments of the counter-current chromatographic process are outlined, and a preliminary computer simulation of the SCCR3 unit t is presented.

Computational fluid dynamical studies of structured distillation packings

In recent years structured packings have become more widely used in the process industries because of their improved volumetric efficiency. Most structured packings consist of corrugated sheets placed in the vertical plane The corrugations provide a regular network of channels for vapour liquid contact. Until recently it has been necessary to develop new packings by trial and error, testing new shapes in the laboratory. The orderly repetitive nature of the channel network produced by a structured packing suggests it may be possible to develop improved structured packings by the application of computational fluid dynamics (CFD) to calculate the packing performance and evaluate changes in shape so as to reduce the need for laboratory testing. In this work the CFD package PHOENICS has been used to predict the flow patterns produced in the vapour phase as it passes through the channel network. A particular novelty of the approach is to set up a method of solving the Navier Stokes equations for any particular intersection of channels. The flow pattern of the streams leaving the intersection is then made the input to the downstream intersection. In this way the flow pattern within a section of packing can be calculated. The resulting heat or mass transfer performance can be calculated by other standard CFD procedures. The CFD predictions revealed a circulation developing within the channels which produce a loss in mass transfer efficiency The calculations explained and predicted a change in mass transfer efficiency with depth of the sheets. This effect was also shown experimentally. New shapes of packing were proposed to remove the circulation and these were evaluated using CFD. A new shape was chosen and manufactured. This was tested experimentally and found to have a higher mass transfer efficiency than the standard packing.

Gas distribution in shallow packed beds

Packed beds have many industrial applications and are increasingly used in the process industries due to their low pressure drop. With the introduction of more efficient packings, novel packing materials (i.e. adsorbents) and new applications (i.e. flue gas desulphurisation); the aspect ratio (height to diameter) of such beds is decreasing. Obtaining uniform gas distribution in such beds is of crucial importance in minimising operating costs and optimising plant performance. Since to some extent a packed bed acts as its own distributor the importance of obtaining uniform gas distribution has increased as aspect ratios (bed height to diameter) decrease. There is no rigorous design method for distributors due to a limited understanding of the fluid flow phenomena and in particular of the effect of the bed base / free fluid interface. This study is based on a combined theoretical and modelling approach. The starting point is the Ergun Equation which is used to determine the pressure drop over a bed where the flow is uni-directional. This equation has been applied in a vectorial form so it can be applied to maldistributed and multi-directional flows and has been realised in the Computational Fluid Dynamics code PHOENICS. The use of this equation and its application has been verified by modelling experimental measurements of maldistributed gas flows, where there is no free fluid / bed base interface. A novel, two-dimensional experiment has been designed to investigate the fluid mechanics of maldistributed gas flows in shallow packed beds. The flow through the outlet of the duct below the bed can be controlled, permitting a rigorous investigation. The results from this apparatus provide useful insights into the fluid mechanics of flow in and around a shallow packed bed and show the critical effect of the bed base. The PHOENICS/vectorial Ergun Equation model has been adapted to model this situation. The model has been improved by the inclusion of spatial voidage variations in the bed and the prescription of a novel bed base boundary condition. This boundary condition is based on the logarithmic law for velocities near walls without restricting the velocity at the bed base to zero and is applied within a turbulence model. The flow in a curved bed section, which is three-dimensional in nature, is examined experimentally. The effect of the walls and the changes in gas direction on the gas flow are shown to be particularly significant. As before, the relative amounts of gas flowing through the bed and duct outlet can be controlled. The model and improved understanding of the underlying physical phenomena form the basis for the development of new distributors and rigorous design methods for them.

Continous annular chromatography for the separation of carbohydrate mixtures

The continuous separation of beet molasses resulting in a sucrose rich product and a non-sugar waste product was carried out using a rotating annular chromatograph. The annulus was 12 mm wide and 1.4 m long and was packed with a sodium charged 5.5% cross-linked polystyrene ion exchange resin. Separation was achieved by the simultaneous mechanisms of ion exclusion, size exclusion and partition chromatography. The entire packed bed was slowly rotated while beet molasses was fed continuously through a stationary feed nozzle to the top of the bed. Each molasses constituent having a different relative affinity for the packing and the deionised water mobile phase describes a characteristic helical path as it progresses from the stationary feed point to the bottom of the rotating bed. Each solute then elutes from the annulus at a different angular distance from the feed and separation of the multicomponent mixture is thereby achieved. When a 35% w/w sucrose beet molasses feed was used the throughput achievable was 45.1 kg sucrose m~3 resin h"1. In addition to beet molasses separation other carbohydrate mixtures were separated. In particular the separation of glucose and fructose by Ligand exchange chromatography on a calcium charged ion exchange bed was carried out. The effects of flowrates, concentration, rotation rate, temperature and particle size on resolution and dilution of constituents in the mixtures to be separated were studied. A small test rig was designed and built to determine the cause of liquid maldistribution around the annulus. The problem was caused by the porous bed support media becoming clogged with fines being introduced by eluent flows and off the resin. An outer ring was constructed to house the bed support which could be quickly replaced with the onset of maldistribution. The computer simulation of the operation of the rotating annular chromatograph has been carried out successfully.

Mechanisms of secondary dispersions separation in particulate beds

The mechanisms by which drops of secondary liquid dispersion ie. <100μ m, are collected, coalesced and transferred have been studied in particulate beds of different sizes and heights of glass ballotini. The apparatus facilitated different coalescer cell arrangements. The liquid-liquid system was toluene/de-ionised water. The inlet drop size distribution was measured by microscopy and using the Malvern Particle Size analyser; the outlet dispersion was sized by photography. The effect of packed height and packing size upon critical velocity, pressure drop and coalescence efficiency have been investigated. Single and two phase flow pressure drops across the packing were correlated by modified Blake-Kozeny equations. Two phase pressure drop was correlated by two equations, one for large ballotini sizes (267μm - 367μm), the other for small ballotini sizes (93μm- 147.5μm). The packings were efficient coalescers up to critical velocities of 3 x 10-2 m/s to 5 x 10-2 m/s. The saturation was measured across the bed using relative permeability and a mathematical model developed which related this profile to measured pressure drops. Filter coefficients for the range of packing studied were found to be accurately predicted from a modified queueing drop model. 

The separation of secondary oil-water dispersions in particulate beds

The literature relating to haze formation, methods of separation, coalescence mechanisms, and models by which droplets <100 μm are collected, coalesced and transferred, have been reviewed with particular reference to particulate bed coalescers. The separation of secondary oil-water dispersions was studied experimentally using packed beds of monosized glass ballotini particles. The variables investigated were superficial velocity, bed depth, particle size, and the phase ratio and drop size distribution of inlet secondary dispersion. A modified pump loop was used to generate secondary dispersions of toluene or Clairsol 350 in water with phase ratios between 0.5-6.0 v/v%.Inlet drop size distributions were determined using a Malvern Particle Size Analyser;effluent, coalesced droplets were sized by photography. Single phase flow pressure drop data were correlated by means of a Carman-Kozeny type equation. Correlations were obtained relating single and two phase pressure drops, as (ΔP2/μc)/ΔP1/μd) = kp Ua Lb dcc dpd Cine A flow equation was derived to correlate the two phase pressure drop data as, ΔP2/(ρcU2) = 8.64*107 [dc/D]-0.27 [L/D]0.71 [dp/D]-0.17 [NRe]1.5 [e1]-0.14 [Cin]0.26  In a comparison between functions to characterise the inlet drop size distributions a modification of the Weibull function provided the best fit of experimental data. The general mean drop diameter was correlated by: q_p q_p p_q /β      Γ ((q-3/β) +1) d qp = d fr  .α        Γ ((P-3/β +1 The measured and predicted mean inlet drop diameters agreed within ±15%. Secondary dispersion separation depends largely upon drop capture within a bed. A theoretical analysis of drop capture mechanisms in this work indicated that indirect interception and London-van der Waal's mechanisms predominate. Mathematical models of dispersed phase concentration m the bed were developed by considering drop motion to be analogous to molecular diffusion.The number of possible channels in a bed was predicted from a model in which the pores comprised randomly-interconnected passage-ways between adjacent packing elements and axial flow occured in cylinders on an equilateral triangular pitch. An expression was derived for length of service channels in a queuing system leading to the prediction of filter coefficients. The insight provided into the mechanisms of drop collection and travel, and the correlations of operating parameters, should assist design of industrial particulate bed coalescers.

Uptake and transport of orally-deliverable drugs across caco-2 cell monolayers:the effect of lipid formulations

The aim of this thesis is to investigate the physicochemical parameters which can influence drug loading within liposomes and to characterise the effect such formulations have on drug uptake and transport across in vitro epithelial barrier models. Liposomes composed of phosphatidylcholine (PC) or distearoyl phosphatidylcholine (DSPC) and cholesterol (0, 4, 8, 16 µM) were prepared and optimised in terms of drug loading using the hand-shaking method (Bangham et al., 1965). Subsequently, liposomes composed of 16 µM PC or DSPC and cholesterol (4 µM) were used to monitor hydroxybenzoate release and transport from Iiposomes. The MIT (3[4,5-Dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide) and crystal violet assays were employed to determine toxicity of the Iiposome. formulations towards the Caco-2 cell line, employed to model the epithelial barrier in vitro. Uptake and transport of mannitol, propranolol, glutamine and digoxin was measured in the presence and absence of Iiposome formulations to establish changes in absorption resulting from the presence of lipid formulations. Incorporation of the four hydroxybenzoates was shown to be influenced by a number of factors, including liposome composition and drug conformation. Methyl hydroxybenzo.ate (MP) was incorporated into the bilayer most effectively with percentage incorporation of 68% compared to 45% for butyl hydroxybenzoate (BP), despite its increased Iipophilicity. This was attributed to the decreased packing ability of BP within the hydrocarbon core of the lipid bilayer compared to MP. Release studies also suggested that the smaller MP was more strongly incorporated within the lipid bilayer with only 8% of the incorporated solute being released after 48-hours compared to 17% in the case of BP. Model transport studies were seen to reflect drug release profiles from the liposome bilayers with significantly (p < 0.01) higher amounts of BP partitioning from the liposome compared to MP, Caco-2 cell viability was maintained above 86% in the presence of all Iiposome formulations tested indicating the liposome formulations are non-toxic towards Caco-2 cells. Paracellular (apical-to-basolateral) transport of mannitol was significantly increased in the presence of DSPC, PC / DSPC:Cholesterol (16:4 µM; 1000 µg). Glutamine uptake and transport via the carrier-mediated route was Significantly (p < 0.01) increased in the presence of PC I DSPC:Cholesterol (16:0; 16:4 µM). Digoxin apical-to-basolateral transport was significantly increased (p < 0,01) in the presence of PC / DSPC:Cholesterol (16:0; 16:4 µM); thus reducing digoxin efflux via P-glycoprotein. In contrast, PC:ChoJesterol (16:0; 16:4 µM) significantly (p < 0.01) decreased propranolol uptake via the passive transcellular route. Bi-directional transport of propranolol was significantly (p < 0,01) decreased in the presence of PC/DSPC:Cholesterol (16:0; 16:4 µM). The structure of a solute is an important determinant for the incorporation and release of a solute from liposome formulations. PC, DSPC and cholesterol liposome formulations are nontoxic towards Caco-2 cell monolayers and improved uptake and transport of mannitol, glutamine. and digoxin across Caco-2 cell monolayers; thus providing a potential alternative delivery vehicle.