process intensification network newsletter pin …process intensification. “process...

PROCESS INTENSIFICATION NETWORK NEWSLETTER

PIN NEWSThe Newsletter of the

Process Intensification NetworkIssue 7 September 2002.

Editorial

In view of my imminent retirement, this is my last PIN Editorial as a full-time employeeof Newcastle University. However, I intend to maintain a vigorous involvement inProcess Intensification technology in general and PIN in particular.

Looking back over the gestation of the intensification concept from its inception around1980 in ICI, it is apparent that we have been riding successive “waves” ofinterest/opportunities. Initially our target was the reduction of the capital cost of theoverall process system by eliminating pipework and structural support etc. This ideawas fine but proved difficult to sell when depreciated plant was already operating andthere were no “intensified” demonstration plants available to generate confidence.

The next opportunity centred upon intrinsic safety which is dramatically improved withthe smaller hazardous inventories encountered with intensified technology. Hopefullythis will make disasters like those at Flixborough and Bhopal a thing of the past. Laterwe realised that the application of PI to fine chemical and pharmaceutical productioncould render the process much more responsive and perhaps allow just-in-timemanufacture. Also, since laboratory scale equipment can often generate full scaleproduction, the delays associated with scale up (e.g. for authorisation by FDA) areavoided and new products can be brought to market more quickly. We have also shownthat higher yields and better quality can usually be achieved. This potential impact onthe overall business process is now raising a great deal of interest world wide.

Currently we are being swept along by the demand for energy-efficient sustainablemanufacture as environmental concerns become more pressing. This plays directly tothe strength of the PI philosophy in respect of the high volumetric heat/mass transferwhich can be achieved and thereby minimise the irreversibilities associated withtemperature and concentration differentials. In this context it has always struck methat the use of electrolysis to execute chemical transformations is particularly elegant.Unfortunately the teaching of organic electro synthesis and electro chemicalengineering does not feature strongly (to put it mildly) in our University undergraduate

Process Intensification Network Newsletter

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courses and so the area remains a Cinderella topic. Nevertheless it has been shown thatHigee electrolysis can avoid electrode gas blinding and considerably enhance the masstransfer within the electrolyte boundary layer. This results in lower cell voltages andimproved current efficiency and product selectivity.

Surely we should be exploring this area more energetically.

Professor Colin RamshawSeptember 2002.

IN THIS ISSUE

*Editorial*PIN Contact Points*The PI Sponsors & Steering Committee* European Commission Call; for Expressions of Interest – PIN Members Active*Swan unveils Supercritical Processing*Automotive Supplier Delphi is Providing Hydrogen Enrichment….*Micro-scale Heat Exchangers/Reactors attract Growing Attention: Industry invited to participate…..*Flex-Reactor: Towards Flexibility in PI*Nanochips launch with New Network*EPSRC Rojects Related to PI*News from the Government's Energy Efficiency Best Practice Programme + Energy & Environment Help Line + A funding opportunity - update*Microreplication and Functional Surfaces*Mobile Phones to run on Methanol*Recent Literature & Patents - including data on accessing patents on the WWW.*Meetings/Conferences *Call for Papers*The Next PIN News *The Next PIN Meeting


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PIN CONTACT POINTS

• For membership information, offers of articles for PIN News, finding collaborators, andnews of meetings, contact: David Reay, PIN Co-ordinator, PO Box 25, Whitley Bay, Tyne &Wear, NE26 1QT, UK. Tel: 0191 251 2985; fax: 0191 252 2229; Email: [email protected]

• For news, past meeting reports, profiles of members, links with other networks etc.,contact: PIN Website: http://www.ncl.ac.uk/pin/

**********THE PIN SPONSORS & STEERING COMMITTEE

The new PIN Steering Committee has had two meetings in 2002. The full membership bringstogether those currently sponsoring PIN, now that the three year EPSRC funding has ceased (as of31 December 2001), and some of the original members. The membership is as follows, with PINSponsors being shown in bold:

Colin Ramshaw – ChairmanDavid Reay – Co-ordinatorDerek Colman – BP Stephen Elsby - EPSRCJanet Etchells – Health & Safety ExecutiveSteve Flynn – DTIAsterios Gavriilidis – University College LondonAndrew Green – BHR GroupDave Holtum – EPSRCRoshan Jachuck – Newcastle UniversityBarry Johnson – Alfa-LavalMike Jones – ProtensiveDag Eimer – Norsk HydroFiona Porter – Future Energy SolutionsPaul Richardson - GlaxoSmithKlineDave Trent – The Dow Chemical Company (USA)Henk van den Berg – Consultant (NL)Terry Winnington – Process Kinetics

Sponsorship amounts range from £1000 to £3000, most covering the financial year 2002/3. As aresult, we have enough funding to cover PIN to April 2003, and a small amount of funding for somelater activities.

Sponsors for 2003/4 are invited to contact David Reay or Colin Ramshaw for details of thebenefits available to sponsors.

CHANGES TO PIN NEWS

It was recommended and agreed that after this issue (No. 7) PIN News would be emailed in theform of short summaries/section headings, with links to appropriate web sites and/or PIN web site.

mailto:[email protected]


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Thus instead of receiving a long document, members will be able to select those articles which theywish to examine in depth by linking to another web address. Important announcements and theEditorial will remain in the shorter version of PIN News.

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European Commission Call; for Expressions of Interest – PIN Members Active

Two expressions of interest, one for a Network of Excellence (MINIPIN) and one for an IntegratedProject (PILOT) have been submitted in the PI area.

MINIPIN - MINIaturisation in the Process INdustries

Newcastle University PIIC has submitted an Expression of Interest in a Thematic Network to theEuropean Commission within the context of the recent call. The proposed network, known asMINIPIN, involves PIN and other European networks, as well as major organisations active inprocess intensification.

“Process miniaturisation is a novel design philosophy which aims to revolutionise processengineering. The perceived benefits of this technology are many and are appropriate for theEuropean Processing industry, which is currently braced with extreme challenges and is striving forcompetitive edge. Process flexibility, improved product quality, speed to market, just in timemanufacturing and sustainable distributed manufacturing capability are some of the benefits of aminiaturised plant. In order to sustain and advance the European process manufacturing capabilityit is proposed to establish an European Network of Excellence in the field of ProcessMiniaturisation with a view to connecting people and encouraging the flow of knowledge forrealisation of the next generation processing plants based upon using nano to micro scale devices”

A Knowledge-driven Process Industry based on Process Intensification Technologies

Many PIN members have agreed to participated in the research proposed by BHR Group as theirPILOT project, should it be incorporated in future funding by the EC. The aim of PILOT issummrised below.

“The ambition of PILOT is to transform the European Process Industry into knowledge-drivensectors that are responsive to consumers desires while being responsible for the greater needs ofsociety. The will be achieved by focussing research activities throughout Europe in the fields ofProcess Intensification and related enabling technology areas and delivering the results asknowledge-driven business solutions.

This entails significant risk and requires a long term commitment by stakeholders. It involves co-ordinating research and the integration of specialities as diverse as: chemical reactions; processintensification and characterisation; equipment design, manufacture, operation and control; smartsensors; on-line chemical analysis; data storage and re-use; rule-based engineering and businesstools; delivery via IT. The project will rely on breakthroughs in other key technical, information,business and societal areas, for which co-operation at a European level is need to make it happen.”

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Swan Unveils Supercritical Processing

A unique multi-purpose processing plant using supercritical fluid (SCF) as solvent beganproduction at Thomas Swan & Co in Consett, Co Durham, in late February. The plant replacesconventional solvents with inert SCFs for reactions like hydrogeneration, Friedel-Crafts alkylationsand acylations, hydroformylations and etherification. The result is cleaner, faster, more selectiveprocesses with no volatile organic solvents to be recovered and little waste.

Carrying out continuous hydrogenation, for example, by hydrogeneous catalysts in supercriticalcarbondioxide over supported platinum or palladium, the plant can make 1000 tonnes of product ayear. The company says that its “Swan-SCF process” has shown 100% selectivity and 100%conversion in a large number of reactions in a single pass. Initially the fullscale plant is makingtrimethyl-cyclohexanone (TMCH) – an acetone derivative used in styrene products – as a trial tocalibrate the equipment. Thomas Swan has operated a smallscale trial plant sucessfully at Consettfor the last four years.

Full-scale production is the culmination of a joint project which began in 1995. Crucial to itsrealisation, says Stephen Ross, Thomas Swan’s fine chemicals manager, was close collaborationbetween three groups.

• Thomas Swan needed simpler, cleaner hydrogenation technology;• Nottingham University chemistry department under Martyn Poliakoff has expertise in the

process use of SCFs and undertook an on-going study funded by Thomas Swan & Co.• Swedish company Chematur has experience of the specialised business of building supercritical

equipment: for extraction, water oxidation and pumping SCFs, compressing and recirculating.And the catalysts? “there was no real catalyst development”, says Ross. “We simply usedDeloxan-type catalysts for hydrogenation work”. Summing up the project: “Collaboration wentvery well and was a model of how industry and academia can work together”.

SCFs are gases compressed to a point where they display some of the properties normallyassociated with liquids. They have both gas and solvent-like properties which can be tuned throughadjustments to pressure the temperature.

Process use of SCFs brings all sorts of advantages. Conventional hydrogenation plants use volatileorganic solvents which must be separated from products by distillation, in the new plant simplyreducing the pressure removes carbon dioxide as gas for recycle. Hydrogen is pretty insoluble instandard solvents, but it is very soluble in supercritical carbon dioxide. So the process can becomecontinuous, with a much smaller reactor: effectively process intensification.

Heat transfer in the reactor is much better. Prior to this new plant, SCF technology has only beenused in a few specialised applications like the decaffeination of coffee. And Stephen Ross adds afinal bite. “SCFs let us look at new synthetic steps like:

• Selectivity in hydrogenation which is not available conventionally;• Friedel-Crafts n-alkylation and mono-etherfication of a diol in one step, even with excess

reagents”.

(This article is reproduced from the Quarterly Newsletter of the Institute of Applied Catalysis. Go towww.iac.org.uk to receive copies of this interesting publication).

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http://www.iac.org.uk/


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AUTOMOTIVE component supplier Delphi is proposing hydrogen enrichment as a solutionto future emissions legislation for internal combustion engines

It is developing a microreformer to generate hydrogen by partial oxidation of fuel. This would beused with a normal petrol engine to reduce emissions of hydrocarbons and nitrigen oxides from coldstarts, and nitrogen oxides when the vehicle is cruising.

No Significant change

The system would not require any significant changes to the design of internal combustion engines,according to Jean Botti, chief technologist of Delphi’s innovation centre for dynamics andpropulsion.

Botti said that hydrogen enrichment would allow the precious metal content of exhaust catalysts tobe reduced by almost half. It would avoid a dramatic increase in the size of catalysts which wouldotherwise be needed under forthcoming emissions rules and which would be difficult to fit intosmall cars.

The microreformer technology has been demonstrated in a component measuring two litres involume. Botti is confident this can be halved by the time production starts by the middle of thedecade.

In the reformation reaction, petrol plus a limited amount of air is partly oxidised to hydrogen andcarbon monoxide, both combustible gases, before entering the engine.

Though this reaction would also need a catalyst to promote it, experts say cheaper materials such asnickel could be used.

Apart from reducing emissions the enriched fuel allows the catalyst to reach “light-off”, thetemperature at which it starts operating effectively, sooner. Delphi says the system will beparticularly useful for larger engined, high emissions vehicles.

Provides electricity

The reformer is a development of the one used in the fuel cell auxiliary power unit, being developedby Delphi with BMW and Renault. This is intended to provide electricity for car ancillary systemssuch as air conditioning, heating and navigation systems, without running the engine or draining thebattery.

The auxiliary power unit employs a solid oxide fuel cell as opposed to the proton exchangemembrane type being developed for traction applications.

As patron exchange fuel cells needs much purer hydrogen than solid oxide, the reformer technologywould not, in its current state of development, be suitable for motive power application.

(Article fist published in The Engineer, 24 May 2002).************************


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Micro-scale Heat Exchangers/Reactors Attracting GrowingAttention – Industry invited to participate in proposed programme

A group of Universities and associated laboratories, together with industry, is preparing a majorproposal for submission shortly to the EPSRC. Under the title ‘Multi-phase transport phenomenain micro-systems’, The project will address the challenges set out below in a co-ordinated andindustrially relevant manner.

The Challenges: In general, classical thermal and fluid dynamic theories which are routinelyapplied at the macro-scale are invalid at the micro-scale. With micro-manufacturing techniquesallowing highly complex geometries to be fabricated for applications such as micro-reactors,cooling of electronics micro-chips, etc., the flow passages at the micro-scale can incorporateextended surfaces, and other enhancement features which can be within the nano-scale. As thethermal demands on equipment increase, due to intensification of chip power, micro-reactorexotherms, or reduced weight/volume in avionics, for example, two-phase heating/cooling systemsbecome increasingly necessary.

At the micro-scale, the lack of fundamental physical understanding is even more acute when phasechange is involved – for example in flow boiling and micro-condensation. Surface tension andinterface curvature considerations affecting condensation and liquid transport at these scales needcomprehensive investigation. Environmental pressures, in some application areas, havenecessitated the use of working fluids such as CO2 in refrigeration and some process duties, againwhere micro-technology is increasing being considered for heat transfer components. Thermalcontrol in fuel cells, now proposed for small devices such as mobile phones, is an additionalchallenge.

Modelling and simulation of transport phenomena in two phases for a range of micro-scales, suchas 1 to 3 mm, 1 mm to 50 microns, and <50 microns is necessary to back up experimentalobservations and to allow design tools to be developed. Multi-channel configurations andmanifolding are particularly challenging at these scales.

The challenges associated with manufacturing the micro-systems, including heat exchangers,capillary devices and micro-reactors, will be addressed by laboratories with expertise in the severalfabrication methods, including UV-LIGA.

The participating Universities: Edinburgh, Heriot-Watt, Newcastle, Nottingham Trent, Oxford,Queen Mary College London, South Bank, & University College London.

The Applications of the Research: The following application areas for the research are among thosewhich have been identified:

Micro-systems involved in thermal control of electronics components and systems, intensifiedprocess technologies, micro-reactors in conventional and biochemical areas, avionics, and inrefrigeration, heat pumping, and heat exchangers in general, (e.g. automotive, aerospace).

For information: Companies interested in participating in this research, by making contributions inkind, helping to direct its industrial relevance, and/or taking researchers into their plants, areinvited to contact David Reay on [email protected] or tel. 0191 251 2985.

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FlexReactor: Towards Flexibility in PI

Andrew Green, Richard Jackson, BHRSolutions.

PIN has showcased many new PI reactor developments over the years. The heart of the PIphilosophy is the matching of plant characteristics (eg mixing time, heat transfer, residence time) tothe process requirements (eg reaction rate, exothermicity, reaction time).

Potential benefits of following a PI strategy are many, including reduced capital and operatingcosts, improved yield and product quality and inherently safe operation. However, there is a catch.Matching plant to process implies that a PI plant is dedicated to that process. Moreover, thephilosophy suggests that the process requirements are known to a high degree of accuracy. Thismay be fine for a bulk chemical that is going to be produced year in year out, but increasingly theUK chemical industry (and indeed that of most of the western world) is moving towards fine andspeciality chemical production. Here the key to competitiveness is responsiveness and time tomarket. In consequence, agile process plant is needed, and there may not be time for fullcharacterisation of each reaction.

So if you have designed a plant for product A, will the plant be suitable for product B when youhave manufactured enough of product A? If you are using stirred tanks in a batch process, theanswer is invariably yes, even if they are not ideal. You may be forced to de-optimise the processand sacrifice yield in order to make it fit the stirred tank reactor. The attraction of converting to acontinuous PI process might seem to be outweighed by the dedicated nature of the plant and the‘easy option’ is to remain with the stirred tanks and batch processing. However, a process streamcontaining a higher yield of your valuable product coupled with a proper consideration of thereduced up- and down-stream costs, may well easily tip the balance.

For PI applications, then, the answer is to use re-configurable reactors and plant to achieve thenecessary flexibility. This would have the benefit of employing PI strategy, without the downsidesof being totally dedicated to one process. The same framework of components would be able to bere-configured to a different process, quickly, efficiently, and cleanly. PI plant, re-configurable to arange of very different processes, has the advantage of being a highly utilised asset, which produceshigh quality product, with minimal by-product, safely, and within a relatively small footprint.

FlexReactor: the Flexible PI Reactor

To meet the requirement for a flexible, reconfigurable PI Plant, BHRSolutions has developedFlexReactor : a multi-purpose, re-configurable reactor system. The concept is simple but powerful.The reactor, which is subject to a number of patent applications, comprises a bundle of static mixerswhich can be easily configured in many different ways using appropriate end connectors (Figure 1).Effective mixing and good heat transfer characteristics means that a wide range of reactions, withtimes from sub-1-second to several minutes can be handled safely and effectively. As it uses staticmixers, which are simple and have well-characterised fluid dynamics, it can be used withconfidence.


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Figure 1. FlexReactor from BHRSolutions

Injection of reactants can be controlled by staged addition along the product flow path. For rapidreactions the means of feeding is key to ultimate performance, and a novel feeding system has beendeveloped which is effective and can easily be modified for different processes. Characterisedcomponents can be ‘plugged’ into the system to create the desired plant capabilities. Potentially awhole range of functionalities can be added between stages, from separation to on-line monitoringand control (illustrated in Figure 2).

Figure 2. Plug-and-play Functionalities of FlexReactor

One unit has already been supplied to a major client to undertake laboratory/pilot trials on a largenumber of its key reactions. BHRSolutions are in detailed discussions with a number of clients inthe fine/speciality chemical and pharmaceutical industries on a diverse range of processes. Thecommon thread is that the combination of performance and multi-product capability whichFlexReactor offers is key to their competitiveness.


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PI Demonstration

A laboratory scale flexible reactor, when combined with an equally flexible semi-continuous flowfacility, can be a very valuable tool to assess the suitability of processes for intensification at theearly stages of process development. It is not very useful to simply provide someone with PIreactor, as the surrounding continuous flow infrastructure (pumps, flowmeters etc) is not likely tobe available. As a result, BHRSolutions, with support from a government Smart Award, isdeveloping and building a highly flexible, small scale PI plant incorporating a FlexReactor.Following tests at BHRSolutions later this year, this will be available to companies wishing to tryout PI on their processes in a laboratory/pilot environment. It is hoped that this will be up andrunning at the forthcoming PIN Meeting in Cranfield on 14 November.

On a more ambitious basis, BHRSolutions has undertaken a full design of a fully flexible andtransportable PI kilo-scale plant through its On Site Process Intensification (OSPRI) project (Figure3). When constructed, this would simply need to plug into standard site services and provide acontinuous or semi-continuous PI Plant. Unfortunately the project is currently on hold as someanticipated government funding has not been forthcoming following the move of EEBPP to CarbonTrust.

Figure 3. BHRSolutions Transportable PI Plant

PI - Scale Down

With PI, the problem is often not so much scale up as scale down. Running PI reactorscontinuously can quickly use up a lot of reactants, even at the smallest practical scale. The facilitymentioned above needs a minimum of a few 10’s of litres of reactants to get some useable results.Scaling down further so, for example, useful data could be obtained with a litre or less will result inreactors which are difficult to build and the fluid dynamics moving from turbulent to laminar flow.The challenge is to build a ‘PI Test Tube’ – and understand how results at this scale can be relatedto pilot and full scale PI application. This is a critical issue in across most PI technologies, and hasbeen the subject of a joint proposal to The Carbon Trust between BHRSolutions and University ofNewcastle.


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Conclusions

PI will continue to provide many research challenges. However, increasingly solutions to many ofthe performance and operability issues are becoming available. FlexReactor addresses the key issueof flexibility, and will provide a key tool in the PI armoury.

For more information contact Andrew Green at BHRSolutions. Tel: 01234 750422, [email protected]

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EPSRC PROJECTS RELATED TO PI

Dave Holtum of EPSRC, a member of the PIN Steering Committee, has provided information onrecently completed and new EPSRC projects which are related to PI. Those interested are invited tocontact the Principal Investigators concerned, and these and other projects may be viewed on theEPSRC web site.

Projects that have recently started or been announced by EPSRC.

• Using generic algorithms for high throughput screening of ionic liquids as reactionsolvents in micro-channel reactors

Abstract: This project unites two institutions together for the common goal of developing acompletely novel way of rapidly and accurately determining the optimal process conditions forindustrially important reactions. This is to be achieved by combining the chemistry and engineeringrequirements to produce an optimised reaction system (including variables such as solvent,temperature, residence time and reagent concentration). Combinatorial techniques are not easilypossible in conventional equipment but by using€ background work derived from a preceding iAcproject, we will develop a high throughput screening approach based on micro channel reactors.Using such systems it is possible to quickly determine reaction performance for numerous ratios ofreagent to solvent at a set temperature. The choice of the optimum solvent is however difficult.Environmental legislation has forced industry to use high boiling liquids, the ultimate of which is anionic liquid. These solvents have proved themselves to be both highl3 effective andenvironmentally friendly media for the reactions proposed, including Friedel-Craft reactions, Diels-Alder reactions and palladium-catalysed allylations (Heck). However choosing the right solventsystem, with the most effective catalyst, at the optimised process conditions involves a parameterspace of many thousands of items. Searching for optimum becomes impossibly time consumingparticularly when more than one exists. Even though standard statistical techniques can alleviate theproblem somewhat the use of genetic algorithms for this function is preferred. Institution: University of SheffieldDepartment: Chemical & Process EngineeringStarts: Jun 1 2002 Ends: May 31 2005 £ Value: 277,746EPSRC Reference: GR/R42078/01Scheme: Standard Research Principal Investigator: Allen, Professor RWKOther Investigators: Styring, Dr P MacInnes, Dr JM





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Hardacre, Dr C Rooney, Dr DW

• Microwave enhanced synthesis in microreactors

Abstract: We will investigate applying microwave radiation to increase the reaction efficiency andpossible selectivity of reaction performed in micro chemical reactors. The study will initially focuson a heterogeneously catalysed aryal cross coupling reaction based on immobilised palladium (theSuzuki reaction) already performed in a micro reactor. This reaction will be carried out in anexisting customised fixed frequency (2.45GHz) focused microwave waveguide system. The workwill then progress by developing a variable frequency low power microwave system specificallydesigned for micro reactor applications which will be used to explore a wider range of single andmulti phase synthetic reactions. Institution: University of HullDepartment: ChemistryStarts: Apr 29 2002 Ends: Apr 28 2004 £ Value: 131,438EPSRC Reference: GR/R50349/01Scheme: Realising Our Potential Awards (ROPA) Principal Investigator: Haswell, Professor SJ

• Using a rotating disc reactor to understand the chemistry and engineering ofheterogeneous reactions in ionic liquids

Abstract: This proposal focuses on developing, evaluating and modelling a reactor capable ofperforming gas/liquid phase heterogeneously catalysed reactions using ionic liquids. This will beaccomplished by using a rotating disc reactor design to maximise the contact between gas andliquid reagents with the heterogeneous catalyst surface and hence reduce the problems associatedwith gas solubility in ionic liquids. Both oxidations and reductions will be performed andbenchmarked against common organic solvents to assess the advantages of ionic liquids. In order tounderstand the properties of this reactor in-situ, Raman spectroscopy will be employedInstitution: Queen's University of BelfastDepartment: Sch of ChemistryStarts: Apr 1 2002 Ends: Mar 31 2005 £ Value: 197,822EPSRC Reference: GR/R68757/01Scheme: Standard Research Principal Investigator: Hardacre, Dr COther Investigators: Rooney, Dr DW

• Quantitative Interpretation of the Flux response of catalytic microreactor

Abstract:. During a current EPSRC grant we have successfully developed an apparatus andmeasured some flux responses of heterogeneous catalytic reactions. Concurrently, one of us hasdeveloped a model to describe the flux response of a catalytic micro reactor. The flux response isthe minute flowrate changes caused by adsorption, reaction and desorption processes within thesystem. The present proposal aims to confirm the model and to measure the relevant parameters ofindustrially important systems, particularly ammonia decomposition and n-heptane isomerisation,







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for which the method is particularly well suited. This will show that the flux response technique canbe used, maybe with other techniques, to gain additional information on catalytic systems and topredict reactor behaviourInstitution: Loughborough UniversityDepartment: Chemical EngineeringStarts: Jan 1 2003 Ends: Dec 31 2005 £ Value: 220,729EPSRC Reference: GR/S00491/01Scheme: Standard Research Principal Investigator: Mason, Dr GOther Investigators: Buffham, Professor BA Hellgardt, Dr K

• PLATFORM: Platform for Process Innovation

Abstract: We wish to build on our current expertise in the field of Process Innovation and providea Cambridge based UK centre of excellence for innovation in both the field of liquid and semi-solidprocessing. In particular the Multipass Rheometers pioneered in our laboratory will be applied tostudy a range of complex fluids and semi-solids. Both the apparatus and its capability will beexplored.. Oscillatory Flow Mixing (OFM) that was also pioneered in Cambridge will also bedeveloped as a bio-diesel reactor and controlled continuous flow mixing device. Majorcollaborative projects in Europe and the UK will be maintained and strengthened. The Groupingwill also continue to provide a sound training base for scientific engineers with a flair forinnovation.Institution: University of CambridgeDepartment: Chemical EngineeringStarts: Oct 1 2002 Ends: Sep 30 2007 £ Value: 408,396EPSRC Reference: GR/R98679/01Scheme: Standard Research Principal Investigator: MacKley, Professor MROther Investigators: Moggridge, Dr GD Kaminski, Dr CF

EPSRC Projects Recently Completed and that are relevant to PIN.

• QUANTITATIVE INTERPRETATION OF THE FLUX RESPONSE OF CATALYTICMICROREACTOR

Abstract: During a current EPSRC grant we have successfully developed an apparatus andmeasured some flux responses of heterogeneous catalytic reactions. Concurrently, one of us hasdeveloped a model to describe the flux response of a catalytic micro reactor. The flux response isthe minute flowrate changes caused by adsorption, reaction and desorption processes within thesystem. The present proposal aims to confirm the model and to measure the relevant parameters ofindustrially important systems, particularly ammonia decomposition and n-heptane isomerisation,for which the method is particularly well suited. This will show that the flux response technique canbe used, maybe with other techniques, to gain additional information on catalytic systems and topredict reactor behaviour








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Institution: Loughborough UniversityDepartment: Chemical EngineeringStarts: Jan 1 2003 Ends: Dec 31 2005 £ Value: 220,729EPSRC Reference: GR/S00491/01Scheme: Standard Research Principal Investigator: Mason, Dr GOther Investigators: Buffham, Professor BA Hellgardt, Dr K

• THE DEVELOPMENT OF OSCILLATORY FLOW REACTORS FOR PROCESSINTENSIFICATION IN THE CHEMICALS INDUSTRY

Abstract: We propose to conduct an experimental and theoretical programme to evaluate anddevelop to an advanced level the technology of Oscillatory Flow Reactors as a new method forcontinuous chemical manufacturing. The program will be divided into four sub areas, namelyprocess development, engineering science, process modelling, and technology transfer. Twocompanies, Croda chemicals Ltd and ADIBIS (BP Chemicals) are committed to the project and willcontribute support. We believe that the success of this project will demonstrate that the technologyis viable for the specific process applications where clear advantages are obtained, and that the casestudies will offer a stepping stone to introducing the technology to a wider market. Keywordsdescribing areas of proposal: Continuos processing, process intensification, novel manufacturingmethodsInstitution: University of CambridgeDepartment: Chemical EngineeringStarts: Mar 29 1999 Ends: Mar 28 2002 £ Value: 212,856EPSRC Reference: GR/M20020/01Scheme: Standard Research Principal Investigator: MacKley, Professor MR

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Nanochips launch with new network

This year’s Turing lecture provided the occasion for the Institution of Electrical Engineers toannounce two new professional networks, one on Microsystems and Nanotechnology and anotheron Materials and Devices. The first is chaired by Dr Marc Desmulliez, the second by Professor IanBoyd at UCL.

The lecture, given by Professor Marc Welland of the University of Cambridge, described thedevelopment of novel devices equipped with magnetic dots a few tens of nanometers across.Professor Willard claims these are capable of storing up to 90 or 180 Gbits of data per square inch.He then went on to describe experimental devices with conductor tracks 50nm across and novelcomputing devices based on the dot technology.

These, he says, will allow the equivalent of more than 5 billion transistors to be placed on a singlechip within a few years while using a very small fraction of the power required by present daydevices.

Marc Desmulliez can be contacted at Heriot-Watt University on [email protected]







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(Article first published in EUREKA, May 2002).

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NEWS FROM THE ENERGY EFFICIENCY BEST PRACTICE PROGRAMME – NOWCALLED ENERGY ACTION

The Environment and Energy Helpline 0800 585794Free help to save your business money…Would you like to know…

• how to increase profits by reducing waste?• how to reduce energy costs?• how to cut water and effluent bills?• how to control transport costs?• how to improve environmental performance and image?

Do you need to know about…• legislation and how it affects your business?• cleaner and more efficient technologies?

…then call the Environment and Energy Helpline on 0800 585794 for free information and advice…

Call the helpline and an advisor will …• answer your question straightaway or• arrange for a specialist to ring you back• send you relevant free publications on reducing your waste or your energy use

And, especially for small businesses…

At the Helpline Manager's discretion, a free site visit from a specialist can be arranged, to help you with:• a specific environmental problem• a technical problem on energy saving• a short review of your site to identify opportunities for reducing your waste at source

Details of all calls to the Helpline are treated in the strictest confidence and all advice is free of charge.

For information on support for projects in the areas of heat transfer, compact heat exchangers, and intensifiedprocesses, contact:

Dr. Fiona Porter, Tel: 01235 433012; Fax: 01235 433727. Email: [email protected]

+++++++Microreplication and functional surfaces

3M’s proprietary microreplication technology dates back to 1964 when it was first used to producethe flat plastic lenses used in overhead projectors. These lenses are made up of thousands of small



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grooved, concentric rings which achieve the same effect as a traditional thick glass lens, but atsignificantly reduced weight and cost. This technique of microreplication – in which amanufactured, miniature three-dimensional surface structure is reproduced exactly, by the million –has led to a wide range of other products, such as ‘hook-and-loop’ fasteners, and ‘brightnessenhancement’ films for laptop screens.

The technique is also being used for fluid transport in application where condensation needs to beremoved. A surface made up of tiny channels, up to 0.2mm wide, can direct condensation bymeans of capillary action away form areas where it could lead to corrosion or electrical short-circuits – inside aeroplanes for example.

Micro reaction techniques in biological analysis are also set to benefit from the work at Neuss.Blood samples, for example, can be spread more evenly over micro structured films coated withsuited chemicals for analysis.

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MOBILE PHONES TO RUN ON METHANOL

A miniature fuel cell for consumer electronics promises to be lighter and cheaper than batteries, andenable mobile phones to last three hundred percent longer.

The cell – which is instantly rechargeable – is half the cost and thirty percent of the weight orvolume of existing rechargeable batteries, according to designers at the Lawrence LivermoreNational Laboratory, California.

Lead researcher Jeff Morse said the cell could be used with laptop computers, personal digitalassistants and other portable electronic devices. It could also power military equipment on thebattlefield.

“The cell has been designed to compete with existing rechargeable batteries in their respectivemarketplaces. Its higher energy capacity will lead to further new classes of personal electronics.These are autonomous sensors and communication devices that are not possible with existingbattery technology.

“This cell will also enable the integration of voice, data and computing technologies that can not[currently be achieved].”

The higher energy capacity stems form the use of a micro electrical mechanical system. Thisinvolves micron-sized mechanical components that work in combination with micro chiptechnology.

The system distributes the cells fuel, which is methanol, to control energy output and makes thepower last longer.

The use of methanol also enables instant recharging. Cartridges of the alcohol can simply beplugged into the cell to renew its energy-generating capacity.

Like a battery the cell has two electrodes. Air is passed over one while methanol covers the other,and the entire interior is heated to aid current generation. This occurs from the release of protonsfrom the alcohol-immersed electrode to the air electrode. The protons react with the oxygen andelectricity is produced.


16

The design is patented and Morse hopes that, with the help of industrial partners, it will replacetraditional rechargeable batteries, that use lithium, iron and lithium-polymer combinations.

Lithium batteries require special disposal because of their toxic contents. Morse predicts that thefuel cells will help to solve the problem of lithium battery disposal because of their long life. Thecell could decrease the number of batteries used by society by up to fifty percent, he believes,reducing the many tonnes of waste that are generated by the old technology.

• Fuel cells for consumer electronics are expected to become a $6bn (£4.2bn) market by 2004.Samsung and Motorola are both working on mobile phone fuel cells. Toshiba is also trying outits own methanol cell for a hand held computer.

*******************

Recent Literature & Patents

In this regular section of PIN News, recent publications are briefly reviewed, and patents believed of interest to readersare identified. The Editor invites contributions identified by PIN members in order to increase awareness of PIactivities world-wide. The transfer of technology from one sector to another allows you to eliminate unnecessary R&D,and helps the solution of problems which may be outside your normal areas of experience or expertise. Some of thereviews are obviously aimed at encouraging this. In this issue, some additional patent web sites are detailed - datawhich first appeared in HEXAG News issue 13 and which will be incorporated in the forthcoming 'Guide to ProcessIntensification'.

"Searches in all databases can be done on the basis of key words for the technology, patent numbers, (where known),companies or inventors. Care should be taken in ascertaining where 'free' access stops and charges begin, e.g. forordering the full patent specification.

The UK Patent Office has its own web site, offering a variety of facilities. Free access to patent abstracts and otherservices is available: http://www.patent.gov.uk/

Once onto the UK Patent Office Home Page, directions to the patent search are given. On clicking on this, one is givenaccess to the interface to the published patent application databases of the UK Patent Office, the European PatentOffice and other European national patent offices. There is also access to the database of published patentapplications: Esp@cenet

Full copies of the specification, drawings and claims can be viewed on line, if they are available. Using a key wordsearch for compact heat exchangers, for example, the user will find patent abstracts from Eastern and Western Europe,as well as the USA.

Perhaps the best data sources for patents, in terms of web accessibility and ease of searching, are those associated withUnited States Patents. Abstracts, and other limited access is free of charge, (except for your own web time charges) attwo sites:

http://www.uspto.gov/ - This is the United States Patent and Trademark Office Home Page and is the official site forsearching the US patent database.

http://www.delphion.com The Delphion Intellectual Property Network also lists US patents, searchable by key words,patent numbers, assignees, etc. *(Note that this has now replaced the IBM patent web site address listed in the lastissue of HEXAG News).

For access to more specific data sources on patents, such as vehicle patents, use the web search engine with key wordssuch as 'patents' or ''US patents' to obtain a full listing.

One useful feature of some patent databases is that you can view a picture of the device being patented - not availablewith most abstract services, such as the one I use for the abstracts below. Patents are one area where a picture isworth many thousands of words!"

http://www.patent.gov.uk/

mailto:Esp@cenet

http://www.uspto.gov/

http://www.delphion.com/


17

********

Penth, B. New non-clogging microreactor.

This microjet reactor, it is claimed, overcomes problems of blocking of the fine channels. Fullinformation can be seen on www.synthesechemie.de A knowledge of German will help.

S.T. Munkejord et al. Micro technology in heat pumping systems. International Journal ofRefrigeration 25 (2002) 471-478

Abstract. Micro heat pumps, with dimensions in the order of centimetres, may be in the future beutilised for the heating and/or cooling of buildings, vehicles, and other products or applications. Anumber of issues have yet to be solved, including the construction of a microscale compressor, anddetermination of micro heat exchanger heat transfer capacities. Test samples of micro heatexchangers and a corresponding test apparatus have been built. Some two- phase experiments withpropane (r-290) as refrigerant have been conducted. Preliminary results for a micro condenser with0.5mm wide trapezoidal channels of 25mm length showed that a heat flux of up to 135 kW/m2,based on the refrigerant-side area, was attainable. The corresponding overall heat transfercoefficient was 10kW/(m2K), with a refrigerant mass flux of 165kg(m2s) and a refrigerant-sidepressure drop of 180kPa/m.

*****

Piboon Pantu and George R. Gavalas. A Multiple Microreactor System for Parallel Catalyst:Preparation and Testing. AIChE Journal. Volume 48, Issue 4, April 2002-07-09 Pages 815-819.

Abstract. A system containing nine catalytic microreactors for parallel preparation and testing ofheterogeneous catalysts is described. The catalyst samples are prepared in the form of thin filmscoated on thin quartz rods by dip-coating in solutions of different composition. Catalyst-coatedrods are placed within thin tubes housed inside a wider tube heated in an electrical furnace. Amultiport valve serves to sequentially conduct the reaction products from each microreactor to amass spectrometer for analysis. The system was tested with the reaction of methane reforming withcarbon dioxide over Pt/Ce 1-xGdxO2-05x and Pt/Ce1-xSmxO2-0.5x at 650 and 700oC. Individualcatalysts were characterised by X-ray analysis, and induction-coupled plasma mass spectrometry forcatalyst mass and elemental composition. The measurements showed that Pt/CeO2 had the highestactivity among the series of catalysts tested and generally the activity increased with the ceriumoxide content. After exposure to the feedstream for 2-3 h at 700oC, most catalysts sufferedsignificant deactivation except the mixed oxides with 25-85% samarium oxide that maintainedrelatively stable activity.

*****W. Lee Perry, Abhaya K. Datye, Anil K. Prinja, Lee F. Brown and Joel D. Katz. MicrowaveHeating of Endothermic Catalytic Reactions: :Reforming of Methanol. AIChE Journal,Volume 48, Issue 4, April 2002-07-10 Pages 820-831

Abstract: In an endothermic reaction, such as methanol-steam reforming, the reaction rate can belimited by the ability to supply heat to the reactor. Heat transfer from the reactor wall normallysupplies the required energy in such processes. Drawbacks, such as operating temperatureconstraints and practical heat-transfer restrictions, limit this practice. In such situations, microwaveheating could provide an effective and efficient method for transferring heat to the catalyst. To

http://www.synthesechemie.de/


18

explore this possibility, the methanol-steam reaction performed by conventional heating andmicrowave heating was studied. Mathematical modelling was performed for 1-D heat transfer in asingle catalyst pellet and used for 2-D heat transfer in a tubular packed-bed reactor. The singlecatalyst pellet model indicated that productivity could increase significantly using microwaveheating. The 2-D model showed that microwave heating could minimise radial heat-transfereffects. Conducting the methanol-steam reaction in a microwave-heated reactor experimentallyverified the improved productivity.

Patents: There are no patents in this issue, as the service provided by Elsevier has been shut downfor a few months, and is just recommencing. Normal service will be resumed in the next issue! –Editor.

*******

MEETINGS/CONFERENCES

United Engineering Foundation Conference on Process Innovation & Process Intensification -(PI)2, Edinburgh, 9-13 September 2002.

A report on this Conference will be given in the next issue of PIN News

International Conference on Process Intensification and Miniaturisation in Biological, Chemical,Environmental; & Energy Conversion Technologies. (PIM 1) – 18-21 August 2003. NewcastleUniversity.

The First Announcement has now been published, and Abstracts are due by 1 October 2002. Prof.Galip Akay, who chaired the Nottingham intensification conference in 1995, chairs this ConferenceCommittee. Email: [email protected] Web Site: www.ncl.ac.uk/pimsym

AIChE Spring Meeting, 2003. USA.

At this meeting there is a topical conference on ‘Process Intensification & MicroreactionTechnology’, chaired by Colin Ramshaw and Joe Rogers. Consisting of 5 sessions, coveringmicroreaction technology, Pi (3 sessions) and a panel discussion, the ultimate outcome will includerecommendations by a panel of experts on how to drive the use of process intensification forward.

************************CALL FOR PAPERS

5th International Conference onProcess Intensification for the Chemical IndustryBETTER PRODUCTS AND BIGGER PROFITS

Maastricht, The Netherlands: October 2003

Continuing the focus towards the industrial applications of Process Intensification (PI), this fifthconference in the series will build upon earlier developments and is designed to provide a forum forthe presentation of successful innovative applications of the technology.

Not designed for the sake of being small, intensified processes are being introduced to givecompanies a competitive advantage through reduced costs, higher yields and better products of


http://www.ncl.ac.uk/pimsym


19

consistent quality. Established PI technologies have moved from the laboratory and the researchcentre into the production process, driven by business needs and regulatory pressures. Newinnovations continue to come from academia and innovative equipment providers. No longer justthe domain of high volume bulk chemicals, intensive continuous processing is being applied in thehigher added value chemicals and pharmaceutical sectors, replacing the ubiquitous, but inherentlyinefficient, stirred pots.

Achieving success with an intensified process is more than just getting the right reactor. It mayrequire redesign of other operations such as heat transfer, separation, crystallisation etc. It mayopen up opportunities for improvements to the chemistry through changes in operating conditionsand/or catalysis. Issues of plant flexibility, reconfigurability and agility are key, particularly forhigher added value chemicals. Pl presents new challenges and opportunities for control,instrumentation and on-line analytics. Enabling technologies such as PI design methodologies,modelling and laboratory scale PI tools are key. Plant operability issues such as fouling andreliability need careful consideration. The HR and management challenges associated with stepchange can be significant. Last, but not least, PI can open up opportunities for fundamental changesin business structures, for example through distributed processing.

SCOPE OF THE CONFERENCE:

The Technical Committee will particularly welcome case studies illustrating successful applicationsof Process Intensification. With these evolving technologies, end-users who are at different stagesof integrating intensification processes are encouraged to present their experiences – either at theinitial stages, or with examples where successful intensification work has been established and hasdelivered the designed production improvements.

FOR FURTHER INFORMATIONTo receive a copy of the conference Call for Papers, please contact:

Catriona Pile, Conference OrganiserBHR Group LimitedCranfield Tel: +44 (0) 1234 750422Bedfordshire MK43 0AJ Fax: +44 (0) 1234 750074United Kingdom Email: [email protected]

PROCESS INTENSIFICATION NETWORK NEWSLETTER

The Next PIN News

The next PIN News will be issued in February 2003. Please send your contributions to DavidReay by 10 January 2003.

THE NEXT PIN MEETING- THE NEXTPIN MEETING- THE NEXT PIN

MEETING- THE NEXT PIN MEETING-THE NEXT PIN MEETING

DATE: 14 NOVEMBER 2002.

VENUE: BHR GROUP, CRANFIELD.

Full information and registration forms will be sent to all PIN members inmid-October, 2002.

process intensification network newsletter pin …process intensification. “process...

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