NETWORK YOUNG MEMBRAINS 14 The 14th conference in the NYM series, a platform for young membrane scientists to exchange ideas and build contacts Thursday 20 – Saturday 22 September 2012 Department of Chemical Engineering Imperial College London South Kensington Campus London SW7 2AZ

1

Welcome and introduction......................................................................................... 2 Course programme...................................................................................................... 3 Directory of participants............................................................................................. 9 Speaker biographies.................................................................................................... 14 Presentation abstracts................................................................................................. 31 Poster abstracts........................................................................................................... 61 Technical demonstrations.......................................................................................... 72 Conference sponsors................................................................................................... 74 Practical information and maps................................................................................. 76 Notes............................................................................................................................ 80

CONTENTS

2

Dear participant, Welcome to the fourteenth conference in the Network Young Membrains series, hosted this year at Imperial College London, and organised with the support of the European Commission FP7 funded project, MemTide, and the European Membrane Society. The aim of NYM14 is to bring together creative people working in Membrane Technology as postgraduate students, or in industry. All participants will have the opportunity to present and share their research and to learn about an array of projects related to membrane science. This dissemination of knowledge and research may lead to solutions for current or future problems and, we hope, may even offer the opportunity for future collaborations. We are pleased to have assembled a range of excellent speakers active at the forefront of membrane research, and drawn from much academia and industry. Their talks will be complemented by the posters and oral presentations given by participants in the young mentor sessions. In addition to the technical aspects of the course, we hope that you will enjoy the networking opportunities on offer, both during the course and at the planned social events, which include a bus tour of London, and dinners on each of the three days. We hope that you will find the course both useful and enjoyable, and will be happy to answer any questions that you may have. Yours sincerely, The NYM14 Organising Committee.

Alan Ashton-Smith – Project Administrator James Campbell – PhD Student Dr Patricia Gorgojo Alonso – Marie Curie Experienced Researcher Ana Gouveia Gil – PhD Student Jeong Kim – Marie Curie Early Stage Researcher Ruslan Kochanov – PhD Student Tao Li – PhD Student Nur Muna Mazlan – PhD Research Student Nur Hidayati Othman – PhD Student Irina B Valtcheva – Marie Curie Early Stage Researcher

WELCOME AND INTRODUCTON

3

9.00am Registration and refreshments Level 2 Concourse 9.30am Opening ceremony LT1 11.15am Refreshments Level 2 Concourse

Thursday 20 September 2012

9.45am Plenary 1: LT1 Chair: Nur Muna Mazlan

Klaus-Victor Peinemann (King Abdullah University of Science and Technology) How to invent new membranes

Andrew Livingston (Imperial College London) Organic liquids – a new frontier for nanofiltration

11.40am Young mentor sessions 1: Parallel session 1A: Process (1) LT1 Chair: Dr Patricia Gorgojo Alonso

Elsi Koivula (Lappeenranta University of Technology) Pretreatment to decrease fouling in membrane filtration of wood hydrolysate Jani Siitonen (Lapeenranta University of Technology) Hybrid separation process – steady-state recycling chromatography with an integrated membrane filtration unit Agata Zarebska (University of Southern Denmark) The application of membrane contactors for ammonia recovery from raw and digested manure

CONFERENCE PROGRAMME

Parallel session 1B: Development (1) LT2 Chair: Dr Santanu Karan

Daniela Porfírio Rodrigues (University of Coimbra) Electrospun PCL nanomembranes: polymer blends and surface modifications – physical characterization and comparison Tobias Lülf (Aachen University) Recovery of an argon rich reaction atmosphere by membrane hybrid processes

4

1.00pm Lunch Level 2 Concourse 3.30pm Refreshments Level 2 Concourse 7.00pm Dinner at Eastside Restaurant, Prince’s Gardens, London SW7 1AZ

2.15pm Plenary 2: LT1 Chair: James Campbell

Miguel Menendez (Universidad de Zaragoza) Zeolite membranes and membrane reactors Ivo Vankelecom (Katholieke Universitet Leuven) High-throughput equipment for fast synthesis, characterization and screening of membranes

4.00pm Poster session: Room 252

All participants are invited to attend this session featuring posters from early career researchers. For full details of all posters being presented, please see the Poster Abstracts section on pp.61-71.

5

10.45am Refreshments Level 2 Concourse 12.30pm Lunch Level 2 Concourse

Friday 21 September 2012

Chair: Tao Li Christopher Pink (GSK) Membranes in the pharma industry Andrew Boam (Evonik MET Ltd) Membrane development

2.00pm Young mentor sessions 2: Parallel session 2A: Process (2) – Ultrafiltration LT1 Chair: Dr Ludmila Peeva

Christina Winterscheid (Aachen University) Fouling characterization of silica gel ultrafiltration with flow field flow fractionation María-José Corbatón-Báguena (Polytechnic University of Valencia) Ultrafiltration membrane cleaning using NaCl solutions: influence of cleaning conditions María José Luján Facundo (Polytechnic University of Valencia) Ultrasonic cleaning of ultrafiltration membranes fouled with BSA solution

9.30am Plenary 3 (pharmaceutical & industry session): LT1

11.15am Plenary 4: LT1 Chair: Nur Hidayati Othman

Richard Baker (Membrane Technology and Research, Inc.) Starting a membrane company Enrico Drioli (Consiglio Nationale delle Ricerche) Membrane engineering and process intensification

6

3.20pm Refreshments Level 2 Concourse 7.00pm Gala Dinner – Sauterelle, The Royal Exchange, London EC3V 3LR

Parallel session 2B: Development (2) LT2 Chair: Irina Valtcheva

Ali Farsi (Aalborg University) Reverse osmosis ceramic membrane: Interlayer preparation by polymer derived SiC dip-coating on silicon carbide supports Lars Peters (Aachen University) Layer-by-layer assembly of polyelectrolyte multilayers on polyethersulfone hollow fibres: dry-wet spinning, physiochemical characterizations and performance assessment Aida Garcia Rodríguez (Universitat de Girona) Development of a membrane-based device for the monitoring of antibiotics

3.45pm Sightseeing Bus Tour:

We have arranged a sightseeing bus tour of London, which will take in many of the city’s landmarks, and then drop us off at our venue for dinner. The bus will depart from Imperial College London at 4.00pm, and we will convene beforehand in the Level 2 Concourse at 3.45pm.

7

10.45am Refreshments Level 2 Concourse 12.30pm Lunch Level 2 Concourse

Saturday 22 September 2012

Chair: Ruslan Kochanov Petrus Cuperus (SolSep BV): Membrane Technology in organic solvents: Membranes and processes in chemical industry Dominic Ormerod (Vito) Process intensification via OSN assisted synthesis: towards more environmentally benign chemical production

2.00pm Young mentor sessions 3: Parallel session 3A: Modelling LT1 Chair: Dr Dimitar Peshev

Patrizia Marchetti (Lonza) Permeation through NF and UF membranes Sam Stade (Lappeenranta University of Technology) Real-time monitoring of membrane performance with ultrasonic time-domain reflectometry Carina Rodrigues (ICEMS-IST/UTL) Holographic interferometry visualization and CFD simulation of the concentration boundary layer developed in NF spiral-wound modules feed channels Serafin Stiefel (Aachen University) Acid-base reactions enhancing membrane separation: Model development and implementation

9.30am Plenary 5 (industry session): LT1

11.15am Plenary 6: LT1 Chair: Zhiwei Jiang

Joao Crespo (Universidade Nova de Lisboa) Biological processes Adel Sharif (University of Surrey) Low-Energy Production of Fresh Water from the Sea: Manipulated Reverse Osmosis

8

3.20pm Refreshments Level 2 Concourse 7.00pm Dinner at The Britannia, 1 Allen Street, Kensington, London W8 6UX

3.45pm Technical demonstrations: Labs Demonstrations of the following processes will take place in Imperial’s Separation Engineering Laboratory:

Casting machine Spinning machine

For further details about the equipment processes, please see the Technical Demonstrations section of this programme, on pp.72-73.

Parallel session 3B: Applications LT2 Chair: Jeong Kim

Sebastian Banwarth (Aachen University) Siloxane removal using silicone-rubber membranes

Patrick Schiffman (TU Bergakademie Freiberg) From lab to pilot scale - Module design and Process Simulation for organoselective Pervaporation Sayed Sadr (University of Surrey): Modelling the removal of organics in nanofiltration for water reuse

9

BAKER Richard

USA

BOAM Andrew

UK

CRESPO Joao

Portugal

CUPERUS F Petrus

Netherlands

DRIOLI Enrico

Italy

LIVINGSTON Andrew

UK

MENENDEZ Miguel

Spain

ORMEROD Dominic

Belgium

PEINEMANN Klaus-Viktor

Saudi Arabia

PINK Christopher

UK

SHARIF Adel

UK

VANKELECOM Ivo

Belgium

DIRECTORY OF PARTICIPANTS

Invited Speakers

10

ALI Ola

Saudi Arabia

ASHTON-SMITH Alan

UK

BANNWARTH Sebastian

Netherlands

BURGAL Joao

UK

CAMPBELL James

UK

CAPAR Goksen

Ankara University

Turkey

CHEN Wenqian

Switzerland

CORBATON-BAGUENA

Maria-Jose

Spain

CUPANI Anna

Belgium

DE LA PAZ CASTRO

Vida

Institute for Research in Biomedicine

Spain

ELJADDI Tarik

Université Hassan II

Morocco

FARSI Ali

Denmark

GARCIA IVARS Jorge

Spain

GARCIA RODRIGUEZ

Aida

Spain

Participants

11

GIMENEZ MOLINA

Alejandro

Finland

GORGOJO ALONSO

Patricia

UK

GOUVEIA GIL Ana

UK

JIMENEZ SOLOMON

Maria

UK

JIANG Zhiwei

UK

KARAN Santanu

UK

KILSGARRD Bjorn

Sogren

Denmark

KIM Jeong

UK

KOCHANOV Ruslan

UK

KOIVULA Elsi

Finland

KUNGURTSEV Vyacheslav

Finland

LI Tao

UK

LONERGAN Angela

UK

LUJAN FACUNDO

Maria Jose

Spain

LULF Tobias

Netherlands

12

MARCHETTI Patrizia

Switzerland

MAZLAN Nur Muna

UK

METZE Michael

Germany

MIRANDA Andreia

UK

OTHMAN Nur

Hidayati

UK

PEEVA Ludmila

UK

PESHEV Dimitar

UK

PETERS Lars

Netherlands

POSTMA Tobias

Institute for Research in Biomedicine

Spain

RODRIGUES Carina

Portugal

RODRIGUES Daniela

University of Coimbra

Portugal

SADR Sayed

UK

SCHIFFMAN Patrick

TU Bergakadmie Freiberg

Germany

SHI Binchu

UK

SIITONEN Jani

Finland

13

STADE Sam

Finland

STIEFEL Serafin

Netherlands

VATCHEVA Irina

UK

WINTERSCHEID Christina

Netherlands

ZAREBSKA Agata

Denmark

14

Invited Speakers

Richard Baker Principal Scientist and Founder Membrane Technology and Research, Inc. baker@mtrinc.com Richard Baker received his doctorate in physical chemistry in 1966 at Imperial College London, where he studied under Professor R. M. Barrer, one of the pioneers of membrane science. Subsequently, he joined Amicon Corporation, Lexington, MA, and developed a series of ultrafiltration membranes now sold under the name Diaflow®. While at Alza Corporation (Palo Alto, CA) from 1971 to 1974, he collaborated in the development of the Ocusert® ocular delivery system. In 1974, he co-founded Bend Research, Inc. (Bend, OR), where he was the Director of Research until 1981. Dr. Baker founded Membrane Technology and Research, Inc. (MTR) in 1982, as a research and development company specializing in membrane technology. Dr. Baker is the author or co-author of more than 100 papers and 120 patents, all in the membrane area. His book, Controlled Release of Biologically Active Agents was published in 1987. Two editions of his book Membrane Technology and Applications were published in 2000 and 2004, and the third is being published this month by Wiley UK.

Andrew Boam

Technical Director Evonik MET Ltd andrew.boam@evonik.com Andrew Boam is Technical Director at Evonik Membrane Extraction Technology Ltd. (EMET), with responsibility for development of processes and applications utilising OSN membranes. He obtained both his MEng and PhD degrees from Imperial College London. In 1996, following one year of post-doctoral work, he was one of the founders of EMET with Prof. Andrew Livingston. In his 15 years with EMET, he has been involved in the development of membrane-based technologies for both environmental and production improvements, and responsible for pilot and industrial installation of these technologies. In the last 5 years, his team has focussed on the development and use of organic solvent nanofiltration membranes across many sectors of the chemical process industries, particularly the Pharma, fine chemicals and natural products sectors. He is a co-author of 20+ referreed journal publications and articles, and is co-inventor of multiple patents. He regularly presents on the topic of organic solvent national nanofiltration at national and international conferences.

SPEAKER BIOGRAPHIES

15

Professor Chemical Engineering Universisdade Nova de Lisboa jgc@dq.fct.unl.pt João Crespo is Professor of Chemical Engineering at Universidade Nova de Lisboa (NOVA), Portugal, where he is Vice-Rector for Research and Innovation. He is former Vice-President of Fundação para a Ciência e a Tecnologia (Portuguese National Science Foundation) and former Academic Dean of the Faculty of Sciences and Technology at NOVA. Prof. Crespo is a Member of the editorial board of Journal of Membrane Science, Journal of Biotechnology, and Desalination and Water treatment. He is also founder and member of two university spin-off companies. Research interests: Membrane separation processes; Membrane bioreactors; Process monitoring.

João Crespo

Petrus Cuperus

Managing Director SolSep BV cuperus@solsep.com Dr Ir F.P. Cuperus is co-founder and current managing director of SolSep BV. SolSep develops and produces membranes and membrane separation devices for use in organic solvents. Since 1990 Dr Cuperus is involved in R&D leading to new separation and reactor technology for the environment-friendly processing. He has done extensive work on membranes and membrane reactors for food and non-food industry. He took part in many European projects (FAIR, CRAFT, Brite-Euram, FP6, FP7). Dr Cuperus has been working for the Agrotechnological Research Institute (ATO-DLO), Wageningen,1990-2000) The Netherlands. He was involved part-time as Research Coordinator with the “Stratingh Institute” of the University of Groningen. Within this institute chemical engineers and experts on organic synthesis and catalysis are working on integrated projects. Dr Cuperus owns a Ph-D degree of the University of Twente (Prof. Dr C.A. Smolders) on Membrane Technology (1986-1990). The theme of his masters thesis was the development of ceramic gas separation membranes (Burggraaf, TH Twente). He is (co-)author of more than 50 papers and 7 patents and has been (invited) speaker at more than 50 scientific and engineering (membrane) conferences.

Enrico Drioli

Founding Director Institute on Membrane Technology e.drioli@itm.cnr.it Education Doctor in Chemistry, University of Naples 1965 Research Interests Membranes in Artificial Organs, Integrated Membrane Processes, Membrane Preparation Transport Phenomena, Membrane Distillation and Membrane Contactors, Catalytic Membrane and Catalytic Membrane Reactors

16

Andrew Livingston

Head of Department of Chemical Engineering Imperial College London a.livingston@imperial.ac.uk Andrew Livingston is currently Head of Department at the Department of Chemical Engineering at Imperial College London, a position he has held since 2008. He obtained a BEng (Hons) in Chemical Engineering from the University of Canterbury, New Zealand and after spending two years as Company Chemical Engineer at Canterbury Frozen Meat Co. Ltd, New Zealand, he undertook a PhD in Chemical Engineering at Trinity College, University of Cambridge, which he completed in 1989. He joined the Department of Chemical Engineering at Imperial as a lecturer in 1990. Professor Livingston is interested in research into and development of novel technologies for manufacturing chemicals/ (bio)pharmaceuticals. His research team works with polymer synthesis, formation of polymeric and ceramic membranes, design, fabrication and testing of membrane elements, and modelling and understanding membrane transport processes. Recently they have been working extensively on the use of membrane separations in solvent systems, where they are able to provide new routes to catalyst recycle, product separation, and solvent operations.

Career 2012 Emeritus Professor, University of Calabria 2011 – Present Coordinator of Erasmus Mundus Doctorate in Membrane Engineering (EUDIME) 2009 – Present, Visiting WCU Professor, Dept of Energy Engineering, Hanyang University 2002 – 2008, Director, Institute on Membrane Technology(ITM) of CNR 2008, Present, Founding Director, Institute on Membrane Technology 1993 – 2001, Director, Institute on Membranes and Chemical Reactors of the National Research Council 1982 – 1985, Dean of the School of Engineering, University of Calabria 1981 – 2011 Full Professor, School of Engineering, University of Calabria Professional Activities & Awards 2012, Honorary Membership of the Czech Society of Chemical Engineering 2011, “Richard Maling Barrer Prize” of the European Membrane Society, for his “outstanding contributions to membrane science and technology” 2009, Doctorate Honoris Causa from University of Paul Sabatier of Toulouse, France 2005, International Cooperation Honor Award, Membrane Industry Association of China (MIAC) for special dedication to International Cooperation between China and Europe in the field of membrane science and technology 2005 – Present, Guest professor, Jiangsu Polytechnic University, China 1999, Honorary President, European Membrane Society 1992, Doctorate Honoris Causa in Chemistry and Chemical Technology, Russian Academy of Science 1991, Honorary Professor, China Northwest University in Xi’an, Shaanxi, China 1982 – 1998, President, European Society of Membrane Science and Technology (European Membrane Society) Member of the Advisory Board of the “Journal of Membrane Science” and of the “Polish Journal of Chemical Technology”; Member of the Editorial Board of Desalination, Separation Science and Technology and various other inter. Scientific Journals. Exec. Editor: Applied Water Science Journal, Springer Berlin Heidelberg (Germany) Exec. Editor (for Europe): Membrane Water Technology, Techno Press (Korea) Author of about 650 scientific papers, 18 patents, and 18 books

17

Professor of Chemical Engineering University of Zaragoza qtmiguel@unizar.es Miguel Menendez is Professor of Chemical Engineering at the University of Zaragoza (Spain). His main research lines are related with the improvement of chemical reactors and in particular with fluidized bed and membrane reactors. He started the research in membrane reactors in 1990 and in zeolite membrane reactors in 1995. He has published more than 120 articles and 7 patents, 5 of them on membrane reactors.

Miguel Menendez

Dominic Ormerod Researcher in Process Intensification Vito dominic.ormerod@vito.be Dominic Ormerod obtained his Ph.D. in organic synthesis from the Université catholique de Louvain (Louvain-la –Neuve, Belgium) under the supervision of Prof. I.E. Markó. In 1998 on completion of his Ph.D. he moved to the department of chemical process research at Janssen Pharmacetica (Beerse, Belgium) where he worked from 1998 until January 2012. He has extensive knowledge of all aspects concerning the development of synthetic routes to complex molecules that are usable on large scale. In the latter years of his time in Janssen he developed an interest in Organic solvent Nanofiltration, an interest that precipitated his move in February 2012 to the Flemish institute for Technological Research, VITO in Mol. Currently he is a researcher in Vito leading projects on Process Intensification with membranes, focusing on difficult organic solvent streams.

Klaus-Viktor Peinemann Professor of Chemical Engineering King Abdullah University of Science and Technology klausviktor.peinemann@kaust.edu.sa Klaus-Viktor Peinemann is Professor of Chemical Engineering in the division of Chemical and Life Sciences and Engineering at KAUST in Saudi Arabia. Before joining KAUST he worked at the Helmholtz Research Center in Geesthacht, Germany. There he was for 15 years Head of the Department “Membrane Development”. In this position he directed numerous large research projects and was involved in the development of many new materials and membrane types. In this field he has more than 85 papers in international scientific journals, 160 papers in conferences and is co-editor of four books. He is named as inventor in 25 national and international patents. He was co-founder of the membrane company GMT Membrantechnik in Rheinfelden, Germany, which is today a successful company in Europe active in the field of production of membranes for gas and vapor separation. Dr. Peinemann is Honorary Professor at the Leibniz University of Hannover and he served as President of the European Membrane Society. He belongs to the Editorial Board of the Journal of Membrane Science and he is member of the European and the North American Membrane Society.

18

Christopher Pink Senior Process Engineer Christopher.x.pink@gsk.com Christopher Pink is a senior process engineer currently working in the Particle Generation, Control and Engineering department within GSK R&D. After graduating from the University of Leeds in 2004 he was drawn to pursuing a career in research and was attracted by the possibilities of emerging membrane technologies. A particular article in The Chemical Engineer really captured his imagination, it suggested that fractionation of crude oil may one day be possible using a series of membranes. He then spent 4 years studying at Imperial College in Professor Andrew Livingston’s research group, focussing on homogeneous catalyst separations using organic solvent nanofiltration. GSK recruited Chris in 2008 where his experiences to date include designing and building a continuous lab scale API production facility, process design for both continuous and batch processes across lab, pilot and manufacturing scales. He has also co-supervised a full time industrial PhD student with Professor Andrew Livingston where applications of organic solvent nanofiltration were investigated with a focus on separations specific to GSK.

Adel Sharif Professor of Water Engineering and Process Innovation University of Surrey a.sharif@surrey.ac.uk Adel Sharif is Professor of Water Engineering and Process Innovation, and Founder Director of the Centre for Osmosis Research and Applications, (CORA) at the University of Surrey, UK. Prof. Sharif is a winner of the 2011 Queen’s Anniversay Prize and the 2005 UK Royal Society Brian Mercer Award for Innovation in Science and Technology. He is also the winner of the 2008 Science Business first pan-European Academic Enterprise Award in the category of Energy/Environment. Prof. Sharif founded CORA in 2003, the UN Year of Fresh Water. The centre’s research activities in the area of osmosis science and applications have resulted in a number of inventions in the areas of desalination, water treatment, and renewable power generation. These inventions have the capacity to significantly change the economic and performance characteristics of industries such as desalination, water treatment, power generation, oil, chemical and energy industries that use or produce large quantities of dilute solutions. CORA water technologies were also awarded the Institute of Chemical Engineers 2011 Innovation and Excellence award in the Water Supply and Management category. He is a founder of Modern Water plc, a London Exchange AIM Market listed company specialised in desalination and renewable power generation. Prof. Sharif is a member of the Qatar Foundation’s Expatriate Arab Scientists Forum. He obtained his first degree in Chemical Engineering from Baghdad University in 1986, followed by M.Sc and PhD from University of Wales Swansea in 1989 and 1992 respectively. He has over 100 publications; is an inventor and co-inventor of 12 patents and has supervised over twenty PhD projects and more than 40 M.Sc dissertations.

19

Ivo Vankelecom Professor of Bioscience Engineering KU Leuven ivo.vankelecom@biw.kuleuven.be Ivo Vankelecom (°Ninove, Belgium, 1967) studied Bioscience Engineering at the Catholic University of Leuven (K.U.Leuven), Belgium, where he graduated in 1990. In 1994, he obtained his PhD in Applied Biological Sciences from the Department of Interphase Chemistry on "Inorganic Porous Fillers in Organic Polymer Membranes". Until 2002, he worked at K.U.Leuven as postdoc on membrane catalysis. During this period, he spent 6 months at the Ben-Gurion University of the Negev (Beersheva, Israel) and at Imperial College (London, England). Since 2002, he is professor at K.U.Leuven where he teaches Membrane Technology, Adsorption and Chromatography. He is author of more than 130 peer-reviewed papers and 15 patents.

20

Young Membrains

Sebastian Bannwarth Aachen University Sebastian.Bannwarth@avt.rwth-aachen.de Education and Work 2000 - 2001 - Social service in Santiago de Chile 2002 - 2003 - Pre-Diploma in process engineering, at the Technical University of Clausthal, Germany 2003 – 2010 - Diploma in mechanical engineering, field of study: process engineering 2000 - Internship at Quarzwerke 2002 - Internship at RWE power AG 2009 - Internship at Infraserv Knapsack, Germany 2011 - PhD, Institute of Chemical Process Engineering, RWTH Aachen University, Germany, research field: Membrane characterisation by impedance spectroscopy Theses 1.student thesis: Disturbance prediction for wastewater treatment plant and sewage system control - a literature review 2.student thesis: Characterisation of polyamid membranes for reverse osmosis and nanofiltration with zeta potential measurements 3. diploma thesis: Biogas purification: Investigating a membrane-based process

James Campbell Imperial College London j.campbell10@imperial.ac.uk Born in South London in 1987, James Campbell has always had a keen interest in science and technology. It was because of this interest that he decided to undertake an undergraduate degree in Chemical Engineering at The University of Manchester, this period included a year working at a sugar factory in Bury St Edmunds. His experiences at undergraduate level led him to pursue a career in research. James Campbell returned to London as a PhD student at Imperial College working in the area of Organic Solvent Nanofiltration membranes, specifically organic-inorganic hybrid membranes containing Metal Organic Frameworks.

SPEAKER BIOGRAPHIES

21

María-José Corbatón-Báguena

Universitat Politècnica de València macorba@upvnet.upv.es María-José Corbatón-Báguena holds a Bachelor’s degree in Chemical Engineering and a Master’s degree in Environmental and Industrial Safety from the Universidad Politécnica de Valencia, obtaining the “Prize awarded to the Student with the Best Academic Record” in Chemical Engineering at the same university in 2011. She is carrying out the PhD studies on “Engineering and Industrial Production” and she is working on a research project directed by Dr. Silvia Álvarez- Blanco and funded by the Spanish Ministry of Science and Innovation (MICINN), focused on the cleaning of ultrafiltration membranes used in the food industry by means of non conventional techniques. She presented several works in the International Congress on Membrane and Membrane Processes (ICOM) and the Network Young Membrains 13 (NYM13), which took place in The Netherlands in July, 2011. She also presented works in the Conference and Exhibition of Desalination for the Environment: Clean Water and Energy and in the International Congress of Chemical Engineering, which were celebrated in Barcelona and Seville, 2012, respectively.

Tarik Eljaddi Universite Hassan II eljaddi@gmail.com Professional Experience 05/01/2012 - 15/07/2012: internship at laboratory polymers and biopolymers surface (PBS), Rouen, France 12/07/2007 - 14/03/2008: internship at the Pasteur Institute of Morocco, Casablanca. 12/07/2007 - 12/01/2008: internship at the topographic cabinet "Rachid Tellati", Casablanca, Morocco Professional Skills: Chemistry: Analytical, kinetics, electrochemistry, inorganic, organic.... Quality: ISO 90001,18001,22000,14001, MRP, MSP, AUDIT, TQ, QMS, QSE..... Computer: Office, Microsoft office programming, maintenance, installation, .... Topography: GPS, Total Station, AutoCAD, Topogène, Covadis, CAD Education: 2010 - now: PhD student membrane processes for the metal ions - Laboratory interface materials environment University Hassan II Casablanca. 2009 - 2010: Masters Degree Applied Chemistry University Hassan II Casablanca 2007 - 2008: licence en chimie (Equivalent to a Bachelor’s degree.)University Hassan II Casablanca.

22

Aalborg University alf@bio.aau.dk Ali Farsi, Ph.D. Fellow of chemical engineering is member of separation group of Department of Biotechnology, Chemistry and Environmental Engineering, Aalborg University, where he is a part of Reverse osmosis ceramic membrane project. He is also the Morris Loeb Professor of Chemistry and Chemical Biology at Harvard University. This project has been funded by Danish National Advanced Technology Foundation. He is also Director of membrane reactor group of Shahid Bahonar University of Kerman, Iran as well as member of Iranian chemical engineering society.

Ali Farsi

Jorge García-Ivars

Universitat Politècnica de València jorgariv@posgrado.upv.es Jorge García-Ivars holds a Bachelor’s degree in Chemical Engineering and a Master’s degree in Environmental and Industrial Safety from the Polytechnic University of Valencia. He is carrying out the PhD studies on “Engineering and Industrial Production” and he is working on a research project directed by Dr. María-Isabel Alcaina-Miranda and Dr. María-Isabel Iborra-Clar, focused on the study of pervaporation membranes, fabrication and characterization. He assisted in the International Congress on Chemical Engineering, which took place in Seville (Spain) in June, 2012.

Ana Gouveia Gil

Imperial College London a.gouveia-gil11@imperial.ac.uk Ana Maria Gouveia Gil, born 1987, graduated in 2008 at the University of Coimbra, Portugal, in Chemical Engineering. She received her MSc degree in Chemical Engineering in 2010 from a joint program between University of Coimbra and University of Leeds, United Kingdom. Her master thesis was on development of an intumescent fire retardant glazing product in collaboration with CGI International, Haydock, Lancashire, United Kingdom. From 2010 to 2011, she was a researcher in the European Project "ONLY WATER", focused in water purification by membrane processes (ultrafiltration). Currently, she is a PhD student at Imperial College London with research topic “Novel Catalytic Membrane Micro-reactors for CO2 Capture via Pre-combustion Decarbonization Route”.

23

Bjørn Sjøgren Kilsgaard Aarhus University bjornsk@hotmail.com Bjørn got his bachelor in 2010, writing about the separation of gallic acid from shea nuts. A project offered by AarhusKarlshamn, a Danish company making oil, mainly for the production of chocolate. The oil is often extracted from shea nuts, giving AarhusKarlshamn about 50.000 tons of shea nut residue each year. At the moment he is writing his masters at the Department of Chemical Engineering at Aarhus University. Here he is working with the characterization of membranes, mainly Cation conduction membranes. He is working together with other master students who are characterizing and/or synthesizing membranes. The main idea of this research is to investigate membranes for electrochemical energy conversion.

Jeong Kim Imperial College London j.kim10@imperial.ac.uk Oct 2010 – present: Ph.D & Early Stage Researcher in Marie Curie MemTide project at Imperial College London, UK May 2010 – Aug 2010: Research intern in RISE program at Forschungszentrum Juelich, Germany. Jan 2009 – May 2010: Research student in Dr. Hess' laboratory at Georgia Institute of Technology, USA May 2009 – Aug 2009: Process engineer intern in Celanese Company at Texas, USA Jan 2008 – Jan 2009: Research student in Dr. Chaikof's laboratory at Emory University, USA Aug 2007 – May 2010: Bachelors in Chemical & Biomolecular Engineering at Georgia Institute of Technology, USA

Ruslan Kochanov Imperial College London r.kochanov10@imperial.ac.uk Ruslan Kochanov earned MSc and BSc degrees in chemical engineering from the University of Chemical Technology and Metallurgy – Sofia, Bulgaria (2005 – 2010). During his studies at UCTM-Sofia he also spent time at Otto von Guericke University, Magdeburg, Germany (2007), and at the Department of Chemistry and Industrial Chemistry, University of Genoa, Italy (2010) where he first started working with membranes for industrial applications. He currently is a PhD student in the research group of Professor Andrew Livingston at the Department of Chemical Engineering at Imperial College London.

24

Elsi Koivula Lappeenranta University of Technology Elsi.Koivula@lut.fi 2010 - Master of Science, Lappeenranta University of Technology, Finland 2010 - Doctoral student, Laboratory of Membrane Technology and Technical Polymer Chemistry, Lappeenranta University of Technology, Finland. Topic: Methods for minimization of fouling and improvement of separation efficiency in membrane filtration applications in biorefineries 2011 - Researcher exchange at University of Oviedo, research group of Susana Luque, Oviedo, Spain

Tao Li Imperial College London tao.li10@imperial.ac.uk Biography

• Oct 2011-present: PhD Chemical Engineering at Imperial College London • Sep 2010-Sep 2011: Msc Chemical Engineering at Imperial College London • Sep 2006-Jul 2010: Bsc Chemistry at Dalian University of Technology •

Research Interests • Fabrication of multi-layer ceramic hollow fibers • Solid oxide fuel cell test and stack design •

Awards • May 2010 First Prize NALCO Scholarship awarded by American NALCO

Corporation • Nov 2008 National Scholarship awarded by the Ministry of Education of the

P.R.C.

25

María José Luján Facundo

Universitat Politècnica de València malufa@etsii.upv.es Academic training 2003-2010: Chemical engineering in the discipline of environment, at the polytechnique university of Valencia (UPV), with an average marks of 6,7 and having obtained the prize to the best Final degree Project 09/10 at the high school of industrial engineers. 2010/2011: Official master at the UPV, entitled “Industrial Safety and Environment”. Professional experience 2009-2011: Grant holder at the chemical and nuclear engineering department, at the polytechnique university of Valencia, working on research about membranes and waste water treatment. 2009: Riba-roja de Túria city council: worked with a practice contract to benefit from the awarding of the grants programme “La Dipu te beca”, helping the environment manager of the city council. 2008: Compo Iberia S.L: fertilizer company situated in La Vall d’Uixó. Worked with a practice contract and held the position of supporting the maintenance and quality manager.

Tobias Lülf Aachen University Tobias.Luelf@avt.rwth-aachen.de Since May 2012: Ph.D. Student at Aachener Verfahrenstechnik, Chemical Process Engineering, RWTH Aachen University 5/2011 – 10/2011: Internship: EnviroChemie GmbH: Component selection and construction of a pilot set-up for washwater recycling by membrane filtration 4/2010 – 8/2010: Student research project in Beersheba, Israel on monopolar and bipolar ion exchange membrane characterization 2006 – 2012: Diploma of Mechanical Engineering at RWTH Aachen University. Major: Chemical Process Engineering

Lonza p.marchetti09@imperial.ac.uk Patrizia Marchetti is completing her PhD in Chemical Engineering as industrial-based student at Lonza AG (Visp, Switzerland), and Imperial College London (UK). She earned her master degree in Chemical Engineering at Politecnico di Milano (Italy) in 2009. During her PhD, she has focused on the development of membrane technology for purification/separation of APIs (specifically peptides) and has investigated the fundamentals of solute and solvent transport through membranes.

Patricia Marchetti

26

Lars Peters

Aachen University Lars.Peters@avt.rwth-aachen.de Career 12/2011- PhD student, RWTH Aachen University, Germany 11/2011 - Diploma thesis - Topic: Fabrication and characterization of mixed matrix membranes for the separation of biomolecules 04/2010 – 07/2010 - MEMFO – Chemical Engineering Department of the Norwegian Engineering Department, NTNU, Norway Student research project - Topic: CO2 removal from natural gas by employing amine absorption and membrane technology – a technical and economical analysis 06/2009 - Three months student research project Topic: Aspen Plus Simulation of an Amine Absorption Process for CO2 recovery from power plant flue gases 10/2006 – 11/2011 – Student, RWTH Aachen University, Germany - Chemical Engineering Internships and Work Experience 02/2011 – 04/2011 – Evonik – Trainee, Membrane Process Development 09/2010 – 12/2010 - Vaperma, Quebec, Canada – Trainee, Development of a gas permeation membrane for Nitrogen/Oxygen

Nur Hidayati Othman

Imperial College London n.othman10@imperial.ac.uk Nur Hidayati Othman received her B.Eng in Chemical-Gas Engineering in (2006) from Faculty of Chemical Engineering, Universiti Teknologi Malaysia (UTM), Malaysia. Her passion in membrane starts when she did her undergraduate research, focused on the development of reverse osmosis membrane for drinking water application. She then continues her Master Engineering research, still in the membrane area but for different application (Direct Methanol Fuel Cell). She has published a paper in Journal of Membrane Science and few papers in International Conference on Membrane Science & Technology. She received the National Science Fellowship (NSF) from the Ministry of Science, Technology and Innovation of Malaysia for her masters degree and graduated in (2009). She then takes up a position as a lecturer in Universiti Teknologi Mara (UiTM), Malaysia. She has particular interest in developing membrane for water and waste water treatment and was awarded an Exxon Mobil research grant in 2008 to carry out the pre-treatment of produced waters (PWs) from oil & gas production using reverse osmosis membrane. Currently, she is pursuing her doctoral studies in Department of Chemical Engineering, Imperial College London focusing on the development of dual layer ceramic hollow fibre membrane reactor for methane conversion.

27

Carina Rodrigues

ICEMS-IST/UTL carina.rodrigues@ist.itl.pt Carina P. Rodrigues completed her MSc in Biomedical Engineering at Instituto Superior Técnico, Technical University of Lisbon in 2007. In 2008, she joined Prof. Norberta de Pinho’s group of Membrane Separation and Processes, as an investigator. Under the supervision of Prof. Vítor Geraldes, she focused her investigation in analysing the flow structure and mass-transfer in spacer-filled membrane channels with relevance for spiral-wound modules used in biomedical and water purification applications. In 2010, she was granted a PhD scholarship to continue her work. Using techniques as Holographic Interferometry, Limit Current Technique and CFD simulations, the combination between them is essential to predict, programme and validate new experiments using new spacer configurations and membrane configurations, a work in progress.

Daniela Maria Porfírio Rodrigues

University of Coimbra dmprodrigues@iol.pt Daniela Maria Porfírio Rodrigues was born in Coimbra, Portugal on January 11th, 1984. She joined Coimbra Technical Institute (IPC), College of Agriculture (ESAC), Food Engineering Department in 2002 and graduated from the Department in 2007 with B.S. degree. After graduation, she started her career in research field as Research Fellow in the project MARE FDR 27 – Innovation in Cod fish Industry: Development of a new fermented product and brine reutilization, at College of Agriculture. While working she started pursuing her master degree, again in food engineering program at ESAC-IPC in the fall semester of 2008. During her masters graduation, and after her research project ended, she worked also as a trainer in the areas of quality control in microbiology; quality management; microbiological analysis of water; food chemistry; HACCP systems; nutrition and dietetics. In April of 2010 she graduates with Master degree and continues working as a trainer. In September of 2011 she returns to work as a Reseaserch Fellow at the Department of Chemical Engineering, University of Coimbra in the project PTDC/CTM-POL/112289/2009 NanoBioCats. Her current interests are polymers electrospinning, surface modification, enzyme immobilization and biocathalysis.

28

Aida Garcia-Rodríguez

Universitat de Girona aida.garcia@udg.edu I completed my undergraduate degree in Chemistry at the University of Girona (Catalonia, Spain) in July 2009. In September 2010 I concluded an Interuniversity Master of Applied Chromatographic Techniques. I started my PhD studies in October 2010 at the University of Girona and in 2011 I got a three years research fellowship from the University. Currently I am working at the Chemistry Department under the guidance of Dr. Clàudia Fontàs and Dr. Víctor Matamoros at the Environmental and Analytical Chemistry unit. My studies are focused on the regeneration of waste water and on the development of analytical methods for the determination of organic contaminants in environmental matrices. Seyed Sadr

University of Surrey s.sadr@surrey.ac.uk Seyed started his PhD at the University of Surrey in Water and Chemical Process Engineering in April 2011. The title of his research is: “Application of Membrane Assisted Technologies in Water Reuse Scenarios”. He completed his master in Water Sciences Engineering at Azad University of Shoushtar, Iran in 2009 and his B.Sc. in the same subject at Azad university of Ahvaz, Iran in 2006. He worked for a civil and environmental company in Iran for four years (part-time) before he came to undertake his PhD. Jani Siitonen

Lappeenranta University of Technology Jani.Siitonen@lut.fi 2009 - Master of Science, Lappeenranta University of Technology, Finland. 2009 - Project engineer, Lappeenranta University of Technology, Finland. 2010 - Doctoral student, Lappeenranta University of Technology, Finland. Topic: Theoretical analysis and design methods for advanced separation processes based on chromatography and membrane filtration. 2011 - Research visit at Nanyang Technological University, research group of Asst Prof. Arvind Rajendran, Singapore.

29

Sam Stade

Lappeenranta University of Technology Sam.Stade@lut.fi 2010 - Master of Science, Lappeenranta University of Technology, Finland 2011 - Project Researcher, Lappeenranta University of Technology, Finland 2012 - Master of laboratory, Laboratory of Membrane Technology, Lappeenranta University of Technology, Finland 2012 - Doctoral student, Lappeenranta University of Technology, Finland. Topic: Real-time monitoring of membranes and its applications

Serafin Stiefel

Aachen University Serafin.Stiefel@avt.rwth-aachen.de Practical Experience 07/2009-02/2011 - 3M Germany, Neuss, Germany Trainee program. 04/2008-10/2008 - Internship at Boehringer-Ingelheim, Biberach. Division Engineering & Technology Studies 02/2011 - Graduate Student, Institute for Chemical Process Engineering (Prof.Matthias Wessling), RWTH Aachen University Project focus: Electrochemical Membrane Reactors 10/2002-05/2009 - Rheinisch Westfälische Technische Hochschule Aachen University Diploma in Mechanical Engineering, Majoring: Biochemical Process Engineering 01/2007-05/2007 - Diploma Thesis, Institute for Chemical Process Engineering, RWTH Aachen University Title: “Modelling and Optimisation of a Membrane-based Reactive Extraction for the Separation of Organic Acids and Bases” 04/2007-04/2008 - Graduate research assistant for the Institute for Chemical Engineering, RWTH Aachen University

30

Christina Winterscheid

Aachen University Christina.Winterscheid@avt.rwth-aachen.de Since 06/2012 - Ph.D. Student, Institute of Chemical Process Engineering, RWTH Aachen University 2009 – 2010 - Student exchange, École Polytechnique Fédérale de Lausanne 2008 – 2009 - Student Assistant, Institute of Thermal Process Engineering, RWTH Aachen University 2006 – 2012 - Diploma of Mechanical Engineering at RWTH Aachen University, Major: Chemical Process Engineering

Agata Zarebska

University of Southern Denmark agz@kbm.sdu.dk Agata Zarebska is a PhD fellow in the Department of Chemical Engineering, Biotechnology and Environmental Technology at the University Of Southern Of Denmark. She has received her Master of Science Degree in Chemical Engineering from Silesian University of Technology in specialization Green Process Technologies. During her graduate studies, she had opportunity to spend a half year visiting the faculty of Engineering at the University of Southern Denmark. Prior to joining SDU, she spent three months as trainee in Renew Energy Company in Svendborg in Denmark working with biogas and nine months as research fellow at the Lulea University in Sweden working with biofuels. Agata's main research interests lie with sustainable and environmentally friendly technologies and renewable energies. Her thesis focuses on optimization membrane separation process that can produce ammonium fertilizer and reusable water from the liquid part animal wastes. Main challenge to the performance of membrane contactor process is fouling on the membrane surface, which is going to be her topic during NYM14 conference.

Irina Valtcheva

Imperial College London i.valtcheva@imperial.ac.uk Born: Sofia, Bulgaria University: University of Chemical Technology and Metallurgy, Sofia, Bulgaria in a joint program with the Technical University, Hamburg-Harburg, Germany Degree: M.Sc. in Chemical Engineering Current Status: PhD student in Chemical Engineering at Imperial College, London, UK

31

Klaus-Viktor Peinemann King Abdullah University of Science and Technology

How to invent new membranes If one wants to learn how to invent new useful membranes, it is a good starting point to study well-known break-through membrane patents. Famous examples are the Loeb-Sourirajan asymmetric desalination membrane, the Henis-Tripodi multicomponent gas separation membrane and the Cadotte reverse osmosis membrane. It is inspiring not only to study the actual patents, but to analyze the activities which finally resulted in the discovery. In some cases the building blocks of a discovery are already there and all what is required is to put them together or to make small modifications. In this context we will analyze the history of the phase-inversion process and the interfacial polymerization. In many cases serendipity – the knack of finding things not sought for - plays a major role. The Henis-Tripodi multicomponent gas separation membrane and the Gore-Tex membrane are examples here. These inventions were accidental, but it was not blind luck, which led to these discoveries. “Chance favors only the prepared mind” is a famous quote of Louis Pasteur, who made break-through discoveries in chemistry and microbiology. The ultimate goal of this lecture is to prepare your mind for future discoveries in the membrane field. Andrew Livingston Imperial College London

Organic Liquids – A New Frontier for Nanofiltration Organic liquids are ubiquitous in chemical science based industries, which range in scale from refining to pharmaceutical production. It is generally accepted that 40-70% of capital and operating costs in these industries are dedicated to separations; and a substantial fraction of this cost is related to processing of organic liquids, both as product streams and solvents. Membrane technology has the potential to provide game changing alternatives to conventional concentration and purification technologies such as distillation, liquid extraction, adsorption and chromatography. In order to achieve this potential, membrane modules must meet several challenges. They must be stable in organic solvents, offer attractive fluxes and rejections for systems of interest, and give reliable and predictable service lifetime and performance. The obvious benefits of membrane processing have been apparent for many years, and have attracted research, development and commercialisation efforts from academic groups, end users, and membrane suppliers. In the last few years these efforts have resulted in a growing range of commercially available membranes, and an increasing number of industrial applications. Organic Solvent Nanofiltration (OSN) is finally emerging as a new frontier for membrane technology.

PRESENTATION ABSTRACTS

Thursday 20 September 2012

32

This presentation will describe research and development on membranes for OSN. Several polymers (polyimides, polyaniline, polybenzimidazole) have been used to create membranes stable in organic solvents. A key step is the post-formation chemical crosslinking of the polymers, which imparts stability even in harsh polar solvents such as DMF, THF and DMSO. Recently developed membranes include thin film composites based on interfacial polymerisation (TFC-IP). By using inert supports, TFC-IP membranes having good flux and rejection in polar aprotic solvents have been developed. A further innovation is the development of OSN membranes that can withstand highly basic and acidic environments, which further widens the scope of the technology. There are a growing number of applications of OSN to industrial separation problems, and some will be outlined, together with the advantages OSN brings to commercial systems. Osmotic pressure, concentration polarisation, and prediction of process performance for organic liquid systems will be discussed. Finally, the attributes of “ideal“ membranes, and likely limitations on system performance will be outlined. Elsi Koivula Lappeenranta University of Technology

Pretreatment to manage fouling in ultrafiltration of wood-based solutions

The future forest biorefineries could produce valuable compounds such as hemicelluloses, lignin derivatives and wood extractives for further processing. For example, hemicelluloses or xylooligosaccharides, can be used in production of films, barriers and food-additives etc., and lignin can be used in production of activated carbon, carbon fiber, and activated carbon fiber. The valuable compounds could be extracted from wood at high temperature and at high pressure at slightly acidic or at alkaline conditions, or with enzymes. The stream produced in the extraction process is called wood hydrolysate. It is a mixture of all the compounds possible to extract from wood. Therefore, from the economical point of view, the separation of the valuable compounds from the wood hydrolysate is one of the most significant steps in biorefinery process schemes. Membrane filtration has been found to be a feasible technique in separation of the valuable compounds from wood hydrolysates. For instance, hemicelluloses can be recovered, fractionated and purified from wood hydrolysates by ultrafiltration. The wood hydrolysates are, however, challenging to filter due to their great fouling potential and, especially, in recovery of sugar oligomers the fouling problems have to be solved before gaining cost effective membrane processes. This study is focused on the development of a pretreatment step, which decreases fouling effectively without causing hemicellulose or sugar oligomer losses. It has been shown that lignin derived material and wood extractives foul the membranes. In this study the goal of the developed pretreatment step is on efficient removal of lignin, because the amount of wood extractives is smaller than the amount of (acid soluble) lignin in the hydrolysates. However, both lignin and wood extractives contain phenolic compounds which means that in

33

several pretreatment options the developed pretreatment affects actually both, lignin derived material and wood extractives. The results achieved so far show that the pretreatment methods, which have decreased most the UV absorbance of the hydrolysate and increased the permeate flux, are pulsed corona discharge treatment (degrading method), polymeric adsorbents (adsorption), and enzyme treatment (degrading method). The pulsed corona discharge treatment improved the filtration capacity six fold compared to the untreated hydrolysate. It has been seen that for instance adsorption cause also hemicellulose losses. This is due to the linkage between some hemicelluloses (mostly xylan) and lignin. Thus, to minimize hemicellulose losses the pretreatment process should consist of two stages. First the hemicellulose-lignin bonds should be cleaved, and the lignin should be removed, for instance by adsorption, only after that. The experiments focused on the two stage pretreatment processes of that kind are at the moment going on. Jani Siitonen Lappeenranta University of Technology Hybrid separation process – steady-state recycling chromatography with

an integrated membrane filtration unit A process concept where a membrane filtration unit is integrated to a steady-state recycling chromatography (SSR) is analyzed theoretically. In an SSR process, the performance of single column chromatographic separation is enhanced by recycling the unresolved part of the chromatogram. The pure leading and trailing sections of the elution profile are collected, while the unresolved middle part is mixed with fresh feed and re-injected into the column. The recycling fraction is typically more dilute than the fresh feed. This limits the amount of fresh feed that can be processed per cycle. The process performance can be enhanced by removing some of the solvent from the recycle fraction, e.g. by using membrane filtration (SSR–SR). The membrane filtration unit can be integrated to different positions of the process. In this study, the performance of the following three SSR–SR configurations is investigated: solvent removal from: I) the fresh feed, II) the recycle fraction, and III) the actual feed solution into the column (obtained by mixing the fresh feed and the recycle fraction). A method is developed to choose the cut times for fractionating the outlet stream of the chromatography column and the capacity of the membrane filtration unit such that user-given purity and/or yield requirements are satisfied. The amount of fresh feed that can be processed per cycle and the injection volume into the column are identified as the only free operating parameters. It is shown that the three SSR–SR configurations have identical performance with the same operating parameters. In contrast, the configurations differ with respect to the maximum amount of fresh feed as well as the range of feasible injection volumes. The effect of concentration limits on applicability and performance of different SSR–SR configurations is studied. The following two types of limits for the extent of solvent removal are discussed: maximum concentration achievable in the membrane filtration unit (solubility or osmotic pressure limit) and maximum concentration of the solution fed into the column

34

(viscosity limit). It is observed that the process configuration where solvent is removed from the column feed (configuration III) is typically the most flexible one with respect to the operating parameters and provides highest productivity. In addition, it is shown than an SSR chromatography with a membrane filtration unit yields higher productivity and lower eluent consumption than an optimized batch chromatography process that employs a similar solvent removal unit or a conventional SSR process without solvent removal. Agata Zarebska University of Southern Denmark

The application of membrane contactors for ammonia recovery from raw and digested manure

Anaerobic digestion and solid-liquid separation of animal wastes are a viable technology for waste management to reduce transport cost and environmental hazards in areas with increased livestock production (1). However, post processing of manure is necessary due to significant amount of nitrogen and phosphorus, which even though they are essential nutrients also pose potential risk of over fertilizing fields leading to contamination of water streams and air (1). Liquid-liquid membrane contactors (MC) present a possible technology for ammonia recovery. In general one of the main obstacles though impeding the implementation of membrane contactors is membrane fouling (2). This must also be expected to be the case for the recovery and concentration of ammonia from swine manure. The presence of organic matter and multivalent ions in pig slurry may greatly influence the membrane fouling due to surface adsorption and pore plugging (3). The aim of this work is to add knowledge on how the overall mass transfer coefficient of ammonia (km) is affected by different solid-liquid separation techniques of pig slurry at different temperatures (30ºC, and 50ºC) and feed flow velocity (0.9 m/s and 1.8 m/s). Further a comparison on how digestion of manure influences membrane fouling at 40ºC and a feed velocity of 0.9 m/s is conducted. Ammonia stripping of the liquid fraction of both digested and undigested manure was performed using tubular polypropylene (PP) membranes. Intensity, morphology and composition of fouling layers have been determined using Scanning Electron Microscopy and Fourier Transform Infrared Spectrometry (ATR-FTIR). Based on the experimental results, it can be concluded that mass transfer of ammonia from the liquid fraction is neither influenced by solid-liquid separation nor by anaerobic digestion. For digested manure the overall mass transfer coefficient km was equal to 19±1∙10-3 m/h and for undigested km was found to be 18.9±0.9∙10-3 m/h at 40ºC, and flow velocity of 0.9 m/s. Further, investigations show that increasing the temperature from 30ºC to 50ºC doubled the overall mass transfer coefficient of ammonia, while increasing feed flow velocity had negligible effect on the overall mass transfer coefficient of ammonia. No significant difference was found between undigested manure effluents with different dry matter content but similar particle size distribution, meaning that pre-processing of manure has little influence on the mass transfer coefficient of ammonia as long as the particle size is unchanged. Membrane fouling in case of digested and undigested pig slurry was a combination of organic fouling, biofouling and colloidal fouling. SEM observations revealed presence of bacteria suggesting biofouling, while the obtained ATR-FTIR spectra are characteristic for proteins and carbohydrates deposit.

35

References 1. Zeng, L.; Mangan, C.; Li, X. Ammonia recovery from anaerobically digested cattle manure by steam stripping. Water Science and Technology 2006, 54 (8), 137-145. 2. Gryta, M. Fouling in direct contact membrane distillation process. Journal of Membrane Science 2008, 325 (1), 383-394. 3. Ko, M. K.; Pellegrino, J. J.; Nassimbene, R.; Marko, P. Characterization of the Adsorption-Fouling Layer Using Globular-Proteins on Ultrafiltration Membranes. Journal of Membrane Science 1993, 76 (2-3), 101-120.

Daniela Maria Porfírio Rodrigues University of Coimbra

Electrospun PCL nanomembranes: polymer blends and surface modifications – physical characterization and comparison

Tailor-made micro/nanofibers have been widely used for several applications due to their high surface area to volume ratio, high porosity and nanofiber size, which can be controlled by adjusting the solution properties and the process parameters [1]. The aim of this work was to develop a nanomembrane by electrospinning with improved performance for use in biocatalytic processes. Electrospinning has recently been widely explored as a method to fabricate nanofibers for various applications, including filtration media, fibre-reinforced plastics and fibres loaded with catalysts and chemical indicators [2]. Poly(epsilon-caprolactone) (PCL), a semicrystalline aliphatic polyester, was submitted to electrospinning and collected as a mat. After modification, it will be used for the immobilization of enzymes in order to create a system which could be applied in biotechnological processes. Additionally, PCL has been suggested for various applications such as drug delivery and tissue-engineered scaffolds [3]. To get a more active membrane for enzyme immobilization, different approaches were attempted: i) blends of PCL with different types of poly(lactic acid) (PLA) (with different ramification degrees); ii) PCL surface modifications with plasma and UV radiation in order to create radicals on the surface of the mat which were used for the copolymerization of polyacids, and iii) copolymerization of methacrylic acid (MAA) and 2-hydroxyethyl methacrylate (HEMA) onto PCL. The electrospun micro/nanofibers prepared from a PCL solution, alone or in a mixture with monomers and polymers, modified or not by UV radiation or plasma, were analyzed by SEM in order to attain a full analysis of morphology, porosity, fiber dimensions and surface properties. The results show that PLC with PLA generates thinner fibers with fewer beads at 8% (w/w) polymer concentration in the electrospinning solution, with a flow rate of 1.5 mL/h. In fact, the average micro/nanofiber diameters of the pure PCL fibers and PCL/PLA fibers were 200 ± 50 and 100 ± 30 nm, respectively. It was also observed that the mats obtained by plasma modification appear to be destroyed in its fiber structure; there was a disruption in fiber connection. Mechanical properties were evaluated by uniaxial extension, including tensile strength, Young’s modulus and elongation. DSC was used to study the thermal properties of the electrospun membranes, namely the crystallization and melting behavior. Contact angle measurements were done to evaluate the mats hydrophobicity. The chemical composition of the mat was evaluated by FTIR.

36

References [1] Yabin Zhu, Changyou Gao, Jiacong Shen, “Surface modification of polycaprolactone with poly(methacrylic acid)and gelatin covalent immobilization for promoting its cytocompatibility” , Biomaterials 23 (2002) 4889–4895. [2] Hyeon Yoon and GeunHyung Kim, “Micro/Nanofibrous Scaffolds Electrospun from PCL and Small Intestinal Submucosa”, Journal of Biomaterials Science 21 (2010) 553–562. [3] Fang Jian, Niu HaiTao, Lin Tong, Wang XunGai, “Applications of electrospun nanofibers”, Chinese Science Bulletin 53 (2008) 2265-2286. Tobias Lülf Aachen University

Recovery of an argon rich reaction atmosphere by membrane hybrid processes

Silicon carbide is widely used as an abrasive and in high temperature applications. Applications as reinforcements are also present, as silicon carbide is thermal and mechanically stable. In a silicon carbide production process an argon and hydrogen containing gas stream is used as reaction atmosphere. During the reaction, carbon monoxide is formed. The net reaction equation is given by:

SiO2(s) + 3C(s) ↔ SiC(s) + 2CO(g). To maintain an economically sustainable process, the reaction atmosphere must be recycled. Different suitable process chains have been identified. Carbon monoxide can be transferred to carbon dioxide and hydrogen by means of water gas shift reaction (WGS). The carbon dioxide level is reduced by means of absorptive processes of monoethanolamine or pressurized water scrubbing (MEA or PWS), whereas the desired hydrogen concentration can be realized by the application of a membrane process (MEM). The derived process chains were modeled in Aspen Plus®. Models for membrane separation were implemented in Aspen Custom Modeler® and imported to Aspen Plus®. To investigate the performance, each process was modeled in stand-alone mode. Thus, optimum operation points in terms of material and energy demands were identified. In a second step the stand-alone blocks were interconnected to give coupled process chains. Optimum operation points for the connected process chains were investigated by sensitivity analyses of relevant process parameter. If coupling was observed to shift the point of optimal operation, operation conditions of each process in the process chain were adapted. Recycling impurities were considered by setting the inlet boundary conditions of the separation process chains to the maximum content for each component, whereas the product stream of the separation route had to fulfill the boundary conditions for the reaction atmosphere. The absorption fluid recycling was modeled by the same procedure.

37

The water gas shift reactor is modeled by equilibrium conversion, depending on temperature and stream composition. Operational costs were estimated by applying cost factors for material streams and energy demands to evaluate the process efficiencies. Stand-alone modeling showed a minimum in energy consumption in the amine scrubbing process for a carbon dioxide loading of about 0.28 moles CO2 per mole of monoethanolamine. For the membrane process the trade-off between the application of large membrane areas and high pressures affects the membrane costs, energy consumptions and material costs due to argon losses. Thus optimum operation depends on the applied economical boundary conditions. In comparison to other process chains, namely water gas shift - pressurized water scrubbing - membrane separation and water gas shift - membrane separation the presented process chain operates at lowest costs. Here a hydrogen rich byproduct stream is found in the membrane permeate. This stream can be used in heat generation or energy conversion. Miguel Menendez Universidad de Zaragoza

Zeolite membranes and membrane reactors The talk will explain how zeolite membranes offer new opportunities for molecular separation and will describe several ways in which zeolite membranes have been successfully used in membrane reactors. This will include the use of zeolite membranes to remove a reaction product, in order to increase the conversion in a reaction with thermodynamic limitations or by other reasons. Other possibilities include the removal of an intermediate product in a series reaction, the use of the membrane as reactant distributor or as simultaneous separator and catalyst, and several other uses which have not been less explored than the previous ones. Finally, the hurdles for the development of zeolite membrane reactors and some ideas for their future development will be discussed. Ivo Vankelecom Katholieke Universitet Leuven

High-throughput equipment for fast synthesis, characterization and

screening of membranes An overview will be given of the high-throughput equipment, designed and patented by KU Leuven, for the fast synthesis, characterization and screening of membranes. The equipment allows very fast development of membranes prepared via phase inversion or interfacial polymerization. The screening in NF, RO, FO, PRO, UF, MF, GS and MBRs can happen with up to 20 different membranes or different feeds at the same time. To steer the membrane development towards really high-performance membranes, combinatorial techniques based on genetic algorithms, have been applied. Special equipment was also developed for in-situ characterization of membrane fouling.

38

Christopher Pink GSK

Membranes in the pharma industry Increasing demand for more sustainable processing has led to a renewed focus on improving mass and energy efficiency of processes within the pharmaceutical industry. Distillation has been the conventional unit operation of choice for solvent recovery, and though generating high purity solvent, distillation can be energy-intensive and a low energy alternative is desirable. A potential method has been identified in emerging separation technique organic solvent nanofiltration (OSN). The work presented investigates the feasibility of using OSN as an alternative to distillation for solvent recovery. While separations of molecules with size differences of over 400Da are easily achievable using OSN, fractionation of similarly sizes molecules is less straightforward, counter current chromatography (CCC), an emerging liquid-liquid based chromatographic separation technique, is capable of such fractionation. It was realised that infact coupling CCC and OSN not only provides a solution for large scale sample preparation, but OSN can also help to significantly reduce the solvent burden required by chromatographic processes (see Figure 1).

Figure 1. A schematic showing OSN coupled with CCC to facilitate large scale CCC and boost

mass efficiency

Andrew Boam Evonik MET Ltd

Membrane Application and Chemical Synthesis

This presentation will provide examples of the benefits of applying membrane technology, specifically organic solvent nanofiltration (OSN), to syntheses in pharmaceutical compound production through several pharma-relevant case studies. These include the use of OSN as a stand-alone technology, or as a part of a hybrid separation technique (e.g. coupled with chromatography) to enhance the performance of a conventional separation technology. OSN’s impact on process yield, product purity, processing time, energy consumption, etc. will be presented.

CCC

5. Fresh CCC mobile phase

6. CCC stationary phase

7. Recovered CCC mobile phase

1. Multi-component feed stream

2. CCC Mobile phase solvent

OSN 1

8. a. Concentrated API solution8. b. Concentrated impurity solution

Sample Preparation Solvent Recovery3. CCC Mobile phase solvent

4. Waste

OSN 2

Friday 21 September 2012

39

Richard Baker Membrane Technology and Research, Inc.

Starting Your Own Membrane Company In 1982, being out of work and with nothing else to do, I started a membrane company (MTR). For the first ten years, the company was closer to a research institute than a commercial organization. We were financed by research contracts from U.S. Government Agencies interested in various membrane processes. In the early 1990s, we started an effort to turn some of our research results into commercial products. This was harder than we thought and we didn’t have real success until 1996, when we found a “killer app”: the separation and recovery of propylene from polypropylene plant resin degassers. Over the next 15 years, the company gradually evolved into a commercial business. Our 2011 sales were about $24 million, and the company has grown to 70 employees. Research is still a big part of the organization, and we have dreams for the future. In this talk, I will describe the MTR history in a bit more detail. From a distance, the growth of our company looks like a smooth trajectory; up close, it was a bumpy ride. I will spend the final portion of my talk describing some of the lessons learned along the way. Enrico Drioli Consiglio Nationale delle Ricerche

Membrane Engineering and Process Intensification The world’s population has crossed the figure of seven billions and is still growing at significant rate. The demand of associated material utilities and energy has emerged even at a higher rate due to modern life style. On the other hand, most of the conventional resources of raw material and energy are following the depleting trend. The environmental concerns allied with the industrial growth and implementation of more stringent rules and regulation point out additional issues for the modern society and process industry. These facts clearly indicate the need of revolutionary changes in state-of-the-art processes and equipment designs being practiced in process industry. The sustainable growth of process industry is strictly adhered with the most economical and efficient use of energy and raw materials and overcoming the environmental problems. Membrane technology addresses the most severe problems of the modern society including the rational use of energy and material resources to extract the maximum benefits from them, exploring new sources for energy and raw materials and handling of the environmental problems. Membrane engineering has proven its excellent coherence with the recommendation of process intensification strategy to cope with these challenges. Desalination is the typical case where the membrane based processes have reduced energy consumption 10 times of the conventional thermal process. Membrane engineering is not only a smart tool to save the energy but it provides the innovative and exciting ways to generate and utilize the power from sustainable resources. Fuel cells have really fueled the

40

innovative ideas of generating and storing energy. The blue energy generated from the salinity gradient is expected to be one important source of power production in near future. Membrane technology offers extremely interesting path way to utilize the raw material in a more efficient way. The membrane reactors possess the capability to increase the efficiency and productivity of the processes through better control of molecular interactions and selective separation. The simultaneous conversion and separation achieved in such systems comes with numerous rewards. The development of the membranes based on new nanostructured material with specific morphology and configuration offers the possibility to improve selectivity and permeability of the new generation membranes. The immobilization of the catalyst in specific structure of such membranes provides an interesting approach for the catalyst designing and hence boosting the process efficiency. The idea of integrated systems has established novel concepts to use the potential of a process in the most proficient fashion. In case of fresh water production, membrane bio reactors, membrane operations and integrated membrane systems are providing interesting solutions to different water problems. The development of the membranes with high selectivity for certain species opens new horizon to obtain the materials from sustainable resources. New innovative unit operations membrane based such as Membrane Distillation and Membrane Crystallizers, Membrane Condenser, Membrane Emulsifier, etc. will contribute to redesign a modern process engineering . Relevant bibliography 1. Enrico Drioli , Adele Brunetti , Gianluca Di Profio and Giuseppe Barbieri, Process intensification strategies and membrane engineering, Green Chem., 2012,14, 1561-1572. 2. Enrico Drioli, Efrem Curcio, Membrane engineering for process intensification: a perspective, Journal of Chemical Technology and Biotechnology,Volume 82, Issue 3, pages 223–227, March 2007. 3. Enrico Drioli, Enrica Fontananova, Future progresses in membrane engineering, presented in XXIX EMS Summer School on Membranes, Nancy France, 10-13 July 2012 4. Andrzej Górak, Andrzej Stankiewic, Research Agenda for Process Intensification Towards a Sustainable World of 2050. Christina Winterschied Aachen University

Fouling characterization of colloidal silica gel ultrafiltration with flow-field flow fractionation

Colloidal silica gel is a stable aqueous dispersion of amorphous silicon dioxide particles. This environmentally friendly product has a wide range of applications, for example as a de-inking agent during paper recycling, for anti-soiling and abrasion resistant coatings. Silica gels produced from native silicon dioxide is synthesized with sodium carbonate and sulfuric acid in salty and aqueous slurry. After synthesis silica gels are desalted applying a downstream process such as ultrafiltration. In this study the ultrafiltration process is investigated in detail concerning fouling mechanisms. The highly viscous silica gel dispersion has a low gelation point around 15-35 wt%. Repulsion forces between the particles, which stabilize the system and prohibit gelation, can be intensified or repressed by changing pH, particle and salt concentration or temperature of

41

the slurry. Due to concentration polarization in the vicinity of the membrane during ultrafiltration, silica gel is deposited on the membrane, causing fouling and reducing membrane performance. The fouling behavior is quantitatively analyzed using flow-field flow fractionation (flow-FFF), a technique which originally separates particles through hydrodynamic forces and diffusion in a flow channel. The hydrodynamics of flow-FFF resemble the conditions of a cross-flow or dead-end flat sheet filtration module. In flow-FFF a permeate flow through a membrane presses the particle towards the membrane, while the particle diffuse back in opposite direction. Then, a laminar cross flow elutes the particles out of the flow channel. First smaller particles are eluted out of the channel by the laminar flow field, because they have a higher diffusion coefficient. Particle-particle and particle-membrane interaction during ultrafiltration are investigated in this study varying surface charge of the membrane, pH and ionic environment of the medium and hydrodynamics in the flow-FFF channel. Agglomeration of particles as well as reversible and irreversible fouling is determined by the average particle size, particle size distribution, recovery rate of the injected silica volume and the critical permeate flux. The membrane surface charge is tuned applying layer-by-layer technique. A strong positively charged polyelectrolyte poly(diallyl dimethyl ammonium chlorid) (PDADMAC) and strong negatively charged poly(sodium styrene sulfonate) (PSS) are deposited on the negatively charged polyethersulphone membrane (PES). Electrolytes with different ionic strength, sodium chloride (NaCl), potassium chloride (KCl), sodium bromide (NaBr) and calcium chloride (CaCl2), influence the stability of the suspension. The impact of salt concentration on attraction and repulsion forces of particles and membrane and therefore on the fouling behavior is studied. Long-term dead-end filtration experiments including backflush, a high cycle number and an increasing permeate flux will be conducted under the same chemical, physical and hydrodynamic conditions to validate the results of flow-FFF. María-José Corbatón-Báguena Polytechnic University of Valencia

Ultrafiltration membrane cleaning using NaCl solutions: influence of cleaning conditions

Most of the industrial developments of membrane technologies in the food industry have been originated from the dairy industry, being ultrafiltration (UF) the most widely used process in the world dairy industry when concentration, purification and fractionation of milk and whey is required [1]. In the last years, consolidation of UF in the dairy industry has been due to the fact that this separation process is a non-thermal process and it does not involve phase changes or any addition of chemical agents [2]. However, the major disadvantage of UF is membrane fouling. In the dairy industry, this is mainly due to protein accumulation and deposition on the membrane surface and inside its pores. Membrane fouling is responsible for the increase in the hydraulic resistance of the membrane and the decrease in permeate flux. Therefore, it is necessary to use cleaning

42

processes to restore the initial membrane conditions. Cleaning procedures consume a great amount of water, chemicals, energy and time. Thus, optimization of operating conditions during membrane cleaning is an essential step in UF processes. Response Surface Methodology (RSM) is one of the most often used statistical tools to optimize the operating conditions in UF processes [3, 4]. Experiments were performed in an UF pilot plant using a ceramic monotubular membrane of 15 kDa (TAMI Industries, France). Each run consisted of four steps: fouling, first rinsing, cleaning and second rinsing. An aqueous solution of bovine serum albumin (BSA) with a concentration of 1% (w/w) was used in the fouling step. The fouling conditions were a transmembrane pressure of 2 bar and a crossflow velocity of 2.4 m/s. Cleaning was performed with NaCl solutions at a transmembrane pressure of 1 bar, a crossflow velocity of 4.2 m/s and three different temperatures (25, 37.5 and 50 ºC) and concentrations (0, 2.5 and 5 mM). After the experiments, the membrane was conditioned with a 20 g/L NaOH solution, to restore its initial permeability when necessary. The hydraulic efficiencies of the first rinsing (HRE) and cleaning (HCE) steps were calculated by means of Eqs. 1 and 2:

The influence of temperature and NaCl concentration on the hydraulic cleaning efficiency (HCE) was studied. When the temperature of the cleaning process increases, HCE increases. This is due to the positive effect of the temperature on the rate of the chemical reaction between the salt and the foulants. Moreover, high temperatures favour the transport of foulant molecules to the bulk solution. However, HCE increases when NaCl concentration increases up to an optimal value, but a further increase of salt concentration has a negative effect on HCE. Optimal values of temperature and concentration were obtained by means of a Response Surface analysis. Temperatures higher than 44 ºC and concentrations of about 3 mM, resulted in HCE values higher than 98 %.

43

Acknowledgments This work was supported by the Spanish Ministry of Science and Innovation through the project CTM2010-20186 and by the Polythecnic University of Valencia through its program PAID-06-10. References [1] G. Daufin, J.-P. Escudier, H. Carrère, S. Bérot, L. Fillaudeau, M. Decloux, Recent and emerging applications of membrane processes in the food and dairy industry, Trans IChemE 79 (2001) part C, pp. 89-102. [2] C. Almandoz, C. Pagliero, A. Ochoa, J. Marchese, Corn syrup clarification by microfiltration with ceramic membranes, Journal of Membrane Science 363 (2010) 87-95 [3] M-C. Martí-Calatayud, M-C. Vincent-Vela, S. Álvarez-Blanco, J. Lora-García, E. Bergantiños-Rodríguez, Analysis and optimization of the influence of operating conditions in the ultrafiltration of macromolecules using a response surface methodological approach, Chemical Engineering Journal 156 (2010) 337-346. [4] E. Alventosa-deLara, S. Barredo-Damas, M.I. Alcaina-Miranda, M.I. Iborra-Clar, Ultrafiltration technology with a ceramic membrane for reactive dye removal: optimization of membrane performance, Journal of Hazardous Materials 209-210 (2010) 492-500. María José Luján Facundo Polytechnic University of Valencia

Ultrasonic cleaning of ultrafiltration membranes fouled with BSA solution

Introduction Although membrane processes are widely employed in the dairy industry, the major disadvantage of their application is permeate flux decline due to membrane fouling. In food industries, membrane fouling is mainly due to protein adsorption onto the membrane surface and the internal pore blockage [1]. This work is focused on comparing the membrane cleaning with and without ultrasounds (US) application. In recent years, the US technique has been tentatively introduced in membrane filtration process [2].

44

Methods A UF Minipilot plant (Orelis, France) was used for the experiments. It was equipped with a Rayflow flat sheet module from ORELIS (France) with capacity for two membranes of 100 cm2 each one, working in series. The tank for the cleaning solution was a TSD-D 18 ultrasonic bath (TSD, Spain) wich was connected to US generator TSD RF 300 (TSD, Spain). Two polymeric membranes (UP005 and UH030) supplied by Microdyn Nadir were tested. Their MWCOs were 5 and 30 kDa, respectively. The feed solution was a bovine serum albumin (BSA, purity>98%, Sigma-Aldrich, Germany) solution with a concentration of 1% w/w. The membrane fouling tests were carried out at 25 ºC and transmembrane pressure of 2 bar. After the fouling test, the cleaning procedure included a rinsing step (30 min), a chemical cleaning with NaOH solution at 1 bar and a final rinsing step. Temperature and pH of the cleaning solution were varied according to an experimental design carried out by STATGRAPHICS. Membrane cleaning was performed by means of US at a 20.5 kHz frequency and 300 W of nominal power. Permeability recovery higher than 95% after each test was required before beginning the following experiment. Results Results clearly show that the use of US has a positive effect because higher permeability recovery values than those obtained without US application at the same conditions of temperature and pH of the cleaning solution. In addition, it is important to note the effect of the pH and temperature of NaOH solution during the cleaning process. The best result is achieved when temperature and pH are 45º C and 9, respectively. Regarding with membrane permeability recovery, the highest value (for the test with US) was 100% and 76.20% for UH030 and UP005 membranes, respectively. Conclusion Experimental results from this study showed significant improvements of the permeability recovery using ultrasounds in the cleaning process. The enhancement factor using US is between 1.2 and 1.8 across the full range of our experiments. Acknowledgements This research was supported by the Spanish Ministry of Science and Innovation (CTM 2010-20.186). References [1] Argüello M. A., Álvarez S., Riera F. A., Álvarez R. (2003) Enzymatic cleaning of inorganic ultrafiltration membranes used for whey protein fractionation. Journal of Membrane Science 216, 121-134. [2] Ming C., Shuna Z., Hanhua L. (2010) Mechanisms for the enhancement of ultrafiltration and membrane cleaning by different ultrasonic frequencies. Desalination 263, 133-138.

45

Ali Farsi Aalborg University Reverse osmosis ceramic membrane: Interlayer preparation by polymer

derived SiC dip-coating on silicon carbide supports The aim of the present work is to make allyl-hydridopolycarbosilane (AHPCS) derived silicon carbide (SiC) interlayer on SiC support in order to prepare smaller pore size surface for top layer coating. A suspension of 5% SiC powder with 200 nm average particle size in solution of 10% AHPCS in n-Hexane has been employed to make pre-ceramic layer by dip coating technique with 2 mm/s rate. Sintering process has been occurred in 750oC for two hours using a regulate temperature program in presence of argon with 3oC/min cool down rate. Four flat disc supports which were cleaned by different methods has been coated at the same conditions to compare with non-cleaned coated support so as to investigate the influence of support cleaning on interlayer performance. In cleaning procedure, all the supports have been contacted with air in 450oC for 2 hours though they have been sonicated with acetone in various times and amounts and then they have been dried at 120oC overnight before sintering process. Concerning this method, a uniform lower crack surface layer has been produced compare to its SiC support. SEM analyzed has shown that the supports’ average pore sizes have been reduced intensively and the remained cracks on interlayer might be caused due to layer thickness that should be thinner. Beside the cracks, there are also some non-coated zones on surface which have been observed for all samples, therefore, it can be concluded that this undesired zones might be related to non-stable suspension. The stability of mentioned suspension might be increased by replacing the n-Hexane with more polar AHPCS’s solvents like Tetrahydrofuran with 4 times more dielectric constant than n-Hexane. The SEM investigations have also shown a number granulation spots remained from support’s surface which have been vanished sharply for cleaned supports. In addition, support cleaning has increased the stability of SiC interlayer that is more evidenced for optimized cleaned conditions surface although sintering program can influence on this parameter obviously. On the other hand, by increasing the sonication time in cleaning process, most prepared surface was obtained for SiC interlayer coating. Key words: Inorganic membrane, Silicon carbide support, Dip-coating technique. Acknowledgments The authors would like to thank Danish National Advanced Technology Foundation for project funding (Project # O59-2011-1). Lars Peters Aachen University

Layer-by-Layer assembly of polyelectrolyte multilayers on polyethersulfone hollow fibres: dry-wet spinning, physicochemical

characterizations and performance assessment The development of asymmetric membranes in the 1960s was a major breakthrough for membrane technologies. Hollow fibre membranes combine the advantages of a large specific surface area with high mechanical strength and have found use in various industrial

46

applications. In this work we report the fabrication of hollow fibres produced via a dry-wet spinning process [1] from polyethersulfone (PES) and polyvinylpyrrolidone (PVP). The outer surface of the obtained hollow fibres was then modified using the layer-by-layer (LbL) technique [2], a technique that involves the direct sequential adsorption of polyelectrolyte multilayers onto the membrane surface [3]. The polyelectrolytes used in this work are polyethyleneimine (MW=750 KDa), or PEI, and polystyrene sulfonate (MW = 70 KDa), or PSS. The formation and growth of the polyelectrolyte multilayers were monitored by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). ATR-FTIR confirms that the deposition of the layers stay on the outer surface of the hollow fibres and do not penetrate into the membrane during coating. The stability of the layers will also be discussed with regard to common chemical cleaning procedure such as exposure to sodium hypochlorite (NaOCl). Bundles of 10Layer-, 20L-, 30L-, 40L-, and 50L-coated hollow fibres (between 3 and 10) were encased into modules to assess their performance in terms of clean water permeability. To the best of our knowledge, this is the first time attempt is also made to (i) evaluate the effective pore size of LbL-coated hollow fibre membranes (dry and wet conditions) and (ii) assess the tensile strength directly on the wet (operating condition) LbL-coated hollow fibres. Aida Garcia Rodríguez Universitat de Girona

Development of a membrane-based device for the monitoring of antibiotics

Antibiotics are a class of pharmaceutical compounds which are widely used for veterinary and human therapy. Due to their incomplete removal in conventional wastewater treatment plants (WWTPs), considerable amounts of these compounds can be found in different environmental matrices where they can represent a potential ecotoxicologial risk. For this reason, it is of interest the development of reliable analytical methods for routine monitoring of antibiotics in waters, which normally include sample cleanup and preconcentration steps. Passive sampling is considered a practical technology which is able to achieve the enormous sampling requirements posed by the presence of chemicals in the environment. This technique owns simplicity and cost effectiveness. It is based on free flow analyte molecules from the sampled medium to a receiving phase in a sampling device, as a result of a difference between the chemical potentials of the analyte in the two media. In the case of polar organic pollutants, such as antibiotics, polar organic chemical integrative samplers (POCIS) are often used. However, in this passive sampling design an elution/desorption step of the analytes is needed prior to the final instrument analysis. This drawback can be overcome with the use of permeable membranes devices, where one side of the membrane is exposed to the aqueous environment, while the other is in contact with a strip solution where the analytes are released. Polymer inclusion membranes (PIMs), in which the carrier is incorporated into a gel network of a polymeric material, can be used for this purpose. Hence, the use of PIMs in front of POCIS has several advantages such as an effective carrier immobilization, easy preparation, versatility, and good mechanical properties.

47

In the present work we have evaluated the use of several PIM compositions for the transport of two families of antibiotics (sulfonamides and tetracyclines) in water samples. Different parameters affecting the membrane system were optimized using as feed phase a mixture of antibiotics at pH 9 and a stripping phase consisting of 1M NaCl. Firstly, the effect of the polymer on the transport efficiency was studied testing two different polymers, cellulose triacetate (CTA) and polyvinyl chloride (PVC). Best results were achieved with the use of CTA. Then, in order to assess the effect of the plasticizer nature and using CTA as a polymer, diverse membranes were created with different plasticizers. Nitrophenyl octyl ether (NPOE) was the plasticizer which allowed better transport efficiencies. Therefore, from our results, it was found that better membrane composition was 46% CTA + 20% Aliquat 336 (carrier) + 34% NPOE. The designed membrane system successfully transported antibiotics contained in environmental matrices such as river and sewage waters after the addition of EDTA to eliminate calcium interaction with tetracyclines. Our present studies are focused on the use of such membranes in special home-made devices to be used as passive samplers for the monitoring of antibiotics in different water matrices. Acknowledgements The financial support by Ministerio de Ciencia e Inovación through project CTM2011-28765-C02-02 is gratefully acknowledged. Aida Garcia wants to acknowledge a BR2011/27 research fellowship from the University of Girona.

48

Petrus Cuperus SolSep BV Membrane Technology in organic solvents: Membranes and processes In

chemical industry Currently, developments in membrane technology in organic solvents are focused on materials as well as process engineering. Very often it is typically a co-development of membrane company and end-user. In the past years SolSep BV has been working on nanofiltration of organic solvents to obtain a solvent or a valuable compound from an organic solvent. Focus is at economically sound technology using polymeric membranes and spiral wound elements. At this moment Solsep produces membrane modules of the spiral wound type. These have been tested in long term tests in solvents like: methanol, ethanol, acetone, ethyl acetate, toluene, chlorobenzene, other chlorinated solvents, many alkanes, alkenes as well as solvent mixtures. By their special design also highly viscous feeds can treated.

To be discussed: solvent recovery processes (chlorinated solvent, acetone/MEK) reclaim of (natural) compounds (natural carbohydrates, bio-fruit-waxes) influence membrane materials on performance

Saturday 22 September 2012

49

Dominic Ormerod Vito

Process intensification via OSN assisted synthesis: towards more

environmentally benign chemical production With increasing pressure being placed upon the environment and natural resources, sustainability is becoming increasingly important within all aspects of society. This manifests itself in an increasing awareness by Governments and the public of the effects industry is having on the environment. Also, sometimes erroneously, the chemical industry is perceived to be one of the most polluting of industrial activities. As such sustainable methods of production and processing are of fundamental importance, not only from an economic stand point but also to improve the public perception of chemistry as a whole. The emergence 15 to 20 years ago of membranes resistant to organic solvents has opened up a whole new field of separation technology to the chemical industries. A technology that can be applied to reducing the environmental impact of solvent based industrial processes. This presentation will outline the results obtained in order to achieve this goal, especially in the realms of chemistry encountered within the pharmaceutical industry. Using organic solvent Nanofiltration (OSN) and including membranes within a reactor set-up we have demonstrated their ability to have a positive effect not only on the environmental impact of a chemical process but also the reaction itself. Results from two industrially relevant case studies will be presented, namely a macrocylisation and metal catalyzed reactions. Whereas, molecules containing macrocycles are becoming more prevalent as active pharmaceutical ingredients (API’s)[1] their large scale production is made costly and problematic by the fact that they must be performed at low concentration in order to favour the intramolecular cyclisation process over intermolecular oligomerization. This results in only small quantities of products being formed in large solvent volumes. By including a membrane within the process we have demonstrated the ability to perform this type of reaction with a significant reduction of the solvent required. Initial results also suggest a positive effect on reaction yields as compared to a more classic batchwise process. Chemical reactions catalyzed by organometallic compounds have become more common within organic synthesis. A fact that has been reflected in the award of three Nobel prizes in chemistry since the turn of the millennium (i.e. in 2001, 2005 and 2010) for the discovery and development of reactions catalyzed by organometallic compounds. However, efficient as they are these catalysts are often expensive and the metals toxic resulting in the need for them to be efficiently removed and preferably recycled. Incorporating a membrane within a reaction set-up allows these catalysts to be used in a continuous or flow reactors leading not only to a concomitant increase in turn over number and a reduction of catalyst loading. But also allowing them to be used in the solution phase thus circumventing mass transfer problems associated with heterogeneous catalysts. Again initial results would suggest the membrane plays an active role in the progress of the reaction.

50

Joao Crespo Universidade Nova de Lisboa

Membrane Engineering in Bioprocesses This lecture will discuss the development of membrane solutions in several bioprocesses. A particular emphasis will be given to the development of cellular membrane bioreactors – both pressure-driven and Donnan dialysis controlled bioreactors – as well as the use of enzymatic multiphasic membrane reactors / contactors for enantiomeric resolution and capture of carbon dioxide. The development of membrane processes for the recovery and fractionation of target biological compounds – small bioactive molecules and proteins – will be also presented and discussed. On-line process monitoring will be discussed, namely using non-invasive molecular probing techniques. Adel Sharif University of Surrey

Low-Energy Production of Fresh Water from the Sea: Manipulated Reverse Osmosis

Water is not just the essential ingredient for life, but also a fundamental factor in the economy and security of any country. Coupled with increased population and climate change effect, the availability of food, water, and energy are the biggest challenges that the world faces. Over the next two decades water demand will exceed water supply by about 40% according to many scientific studies and reports. Food and energy shortages have also been described by the UK Government’s Chief Scientific Advisor, Prof. Sir John Beddington, to create the “perfect storm’’ by 2030. The provision of drinkable supplies through desalination could offer a sustainable solution to the drinking water problem but also presents a technical challenge too. Seawater and brackish water are desalinated by thermal distillation and membrane methods such as reverse osmosis (RO) and electrodialysis. All these methods involve high operating and investment costs. RO is the most widely used desalination techniques, while thermal methods are mainly used in the Gulf countries. However, the high operating cost of RO is due to essential pre-treatment, scaling, bio-fouling and the high-energy consumption. A novel Manipulated Reverse Osmosis (MRO) desalination and water purification process has been invented and developed at the Centre for Osmosis Research and Applications at the University of Surrey in collaboration with Modern Water plc. In the MRO process seawater is converted into an osmotic agent’s solution by taking advantage of the natural osmosis process. Pure water is then recovered from the osmotic agent’s solution using a membrane process, where the agent is reused.

51

The technical obstacles being overcome in this process are the avoidance of all scaling, bio-fouling, high operating pressures, and necessity for pre-treatments and the associated chemical wastes, which result in direct and indirect reduction of cost. The pilot plant and Modern Water’s commercial plants data in Oman and Gibraltar that follow from the MRO process route offers up to 30% saving in the specific energy consumption over a conventional RO process. The MO process also offers an increase in fresh water recovery rate coupled with minimal membrane fouling propensity and brine disposal. Additionally, the process can be incorporated into existing RO and thermal plants with reasonable modifications. New plant based on the MRO principle should also have lower capital costs and smaller footprint. The new technology can be used to obtain clean water from any available water source irrespective of its purity, such as waste streams, seawater, brackish water, river water, etc. Patrizia Marchetti Lonza

Permeation through NF and UF membranes Permeation of water, organic solvents and peptide mixtures through ceramic nanofiltration and ultrafiltration membranes was investigated. Experimental results clearly indicated that the Hagen-Poiseuille equation fails in describing solvent permeation through NF membranes, whereas it is able to describe the experimental permeability through UF membranes. A number of empirical models have been developed to approach this problem. These models are all characterized by the introduction of several solvent-membrane interaction parameters to describe the fluid transport confined in nanoscale pores. Unfortunately, these interaction parameters are often specific for the solvent-membrane couple and the generalization of the model to different solvent-membrane combinations is not possible. In this work, a new model is proposed to describe solvent permeation through NF and UF membranes in the absence of solutes. The development of the model started from the Hagen-Poiseuille equation, which assumes the viscosity as the main influencing parameter for the permeation, and introduces several correction factors to account for the surface phenomena that arise in a nanotube due to solvent-membrane surface interactions. This approach has been initially introduced in the Washburn equation, where the Laplace pressure is used to describe the capillary rise due to surface tension. Additional correction factors were used in the proposed model to account for the effects due to solvent polarity and solvent molecular dimension. The model parameters were regressed on experimental data for five solvent with different physical characteristics. Its predictive capability was tested on other six solvents, in both NF and UF range.

52

The model was also applied to selected aqueous and organic mixtures. It was observed that viscosity represents again the most influencing factor, being the permeability profiles very similar to the viscosity profiles of the corresponding mixtures. The model showed good predictions for all of them, apart from the singular exception of ACN / water mixture. The formation of complexes between water and ACN molecules was taken into account to explain the anomalous behavior of this mixture. Finally, the work was extended to consider the influence of peptides on the permeability of the mixture. The effects of peptide concentration, pH, buffer, pressure and tangential velocity are presented. Sam Stade Lappeenranta University of Technology

Real-time monitoring of membrane performance with ultrasonic time-domain reflectometry

Pressure-driven membrane filtration processes have become more common in many industrial applications. Membrane performance as well as their operating costs are the key factors limiting their attraction. Performance can be increased and operating costs decreased with process optimization. However, this kind of process optimization requires very good knowledge on the filtration process and understanding what is happening inside the module in real-time. In this study novel tools and methods are developed for real-time monitoring of membrane performance. Until now, the research in this study has been focused on the development of a ultrasonic time-domain reflectometry (UTDR) based tool, which can be used for both, measuring of membrane compaction and fouling in real-time. UTDR technique has been successfully used to monitor membrane fouling in real-time also in earlier studies. Due to two improvements in the system developed in this study enables more accurate determination of measurement error than in previous studies have been presented. The first improvement is that the transducer which measures the distance to membrane is implemented inside the filter. Thus, sonic waves are not introduced into the filter chamber through the cover of the cell but straight into feed water and reflections from the interface between the filter cover and feed water are avoided. The second improvement is that a secondary transducer is used for determination of sonic speed, which is needed in calculation of the distance from the primary transducer to the membrane. Sonic speed depends on temperature, pressure and flow conditions prevailing in the filter. Varying of these conditions causes changes in sonic speed during filtration. If sonic speed is not determined but evaluated, the variation of filtration conditions increases measurement error in distance values At this stage of the research, the UTDR tool has been used in measuring of compaction of different ultrafiltration membranes, which have been manufactured from regenerated cellulose (RC) and polyethersulfone (PES). It has been found that there are crucial differences in compaction tendencies of different membranes. The UTDR results showed that the tested RC membrane compacted clearly more than the tested PES membranes. Based on the scanning electron microscopy (SEM) pictures, the support layer of the RC

53

membrane was clearly compacted. A phenomenon of this kind was not seen with the PES membranes. Compaction caused flux decline for all the tested membranes. However, flux of the RC membrane recovered to some extent while the fluxes of the PES membranes were permanently reduced after the compaction. Furthermore, compaction caused a permanent increase in PEG retentions of the PES membranes while with the RC membranes the retentions were at the similar level before and after the compaction. Thus, the results achieved in this study indicate that the PES membranes could be easily modified with precompaction to increase retention. On the other hand, the results demonstrate that it is possible to weaken membrane performance permanently by introducing, for instance, the precompaction stage of the process at a too high pressure. At the next stage of the research real-time monitoring of fouling to achieve information especially on the early-stage of fouling will be the goal. In addition to the developed UTDR tool, also other possible methods will be used in fouling monitoring. Carina Rodrigues ICEMS-IST/UTL

Holographic Interferometry Visualization and CFD Simulation of the Concentration Boundary Layer Developed in NF Spiral-Wound Modules

Feed Channels In recent years, simulation methods based in CFD-techniques have been widely developed for the study of the polarization layer formed in the membranes separation processes [1]. However, these models are not usually accompanied by a comparison with experimental data. Holographic Interferometry (Fig 1) is a technique that allows measuring the changes in the concentration of a solution, which can be seen as a series of interference fringes. Therefore, the formation of the polarization layer, which involves a change in the concentration of the solution, may be seen as an interference fringe pattern. In this paper, the experimental study of the polarization layer has been carried out using a cell that has been used in a previous work [2]. The cell has been slightly modified to adapt it to the technique of holographic interferometry. Basically, two windows have been placed in the cell to allow the laser beam crossing the solution, and a new support for the nanofiltration membrane was introduced. The fluid in the cell flows through a narrow rectangular channel with and without ribs, which act as the typical spacers of spiral-wound modules. The ribbed piece is interchangeable, so the distance between the ribs can be modified to study its effect on the polarization layer. Besides using different ribbed pieces or none (open channel), the study of the formation of the polarization layer at steady state will be carried out using different working conditions. Different cross flow velocities (Reynolds between 1 and 40, based on channel height) and a variable pressure between 5 and 8 bar were used. Different fluid solutions were used, namely aqueous solutions of potassium sulphate, sucrose and glucose, all with concentrations of 2 and 4 g/l. The solute concentration profiles obtained were adjusted using a data interpolation method [3, 4] to determine the influence of light diffraction and posteriorly compared with those

54

obtained by CFD simulation of the system investigated. As predicted, it is necessary to correct the solute concentration profiles taking into account diffraction to obtain the numerical predicted profiles. References [1] G.A. Fimbres-Weihs, D.E. Wiley (2010) Review of 3D CFD modeling of flow and mass transfer in narrow spacer-filled channels in membrane modules , Chemical Engineering and Processing: Process Intensification, 49 (7), , 759-781 [2] C. Rodrigues, M. N. de Pinho, V. A. Semião, V. Geraldes (2012) Mass-transfer entrance effects in narrow rectangular channels with ribbed walls or mesh-type spacers, Chemical Engineering Science, 78 , 38-45. [3] Anurag Sharma, D. Vizia Kumar, and A. K. Ghatak (1982) Tracing rays through graded-index media: a new method, Appl. Optics, 21 (6), 984-987 [4] K. W. Beach, R. H. Muller, and C. W. Tobias (1973) Light-deflection effects in the interferometry of onedimensional refractive-index fields, J. Optic. Soc Amer. 63(5) 559-566. Serafin Stiefel Aachen University

Acid-Base Reactions Enhancing Membrane Separation: Model Development and Implementation

Membranes are an efficient means of extracting organic acids from an aqueous solution. Separation performance can be increased by utilizing the acid-base behavior of the target molecules. In this work, a composite membrane separates the feed stream and the stripping fluid and is preferably permeable for non-polar molecules. The organic acids (e.g. phenol) permeate through the active layer of the membrane and deprotonate in the alkaline stripping fluid present in the porous membrane support, leading to a higher concentration of the respective conjugated base (e.g. phenolate). The consequence of the reaction is an increased concentration gradient of phenol across the membrane and thus improved mass transport. In addition, the charged bases in the stripping fluid are retained by the non-polar membrane. An additional phenomen raises the complexity of the simulation: a convective water flux across the membrane can occur. The exact nature of how the water crosses the membrane has yet to be evaluated, but it is assumed that the osmotic pressure across the membrane is the main driving force. The influence of the water flux on the separation performance is highly complex, as it affects the transport of target molecules but might also hinder the influx of hydroxide-ions into the support structure and so lead to an undesired shift in the acid-base equilibrium in the support. To improve understanding of the non-linear behavior of the governing system parameters and to investigate the character of the convective water flux across the membrane, the objective of this work is to develop a model covering mass transport coupled to the acid-base equilibrium reaction inside a composite membrane with Comsol Multiphysics.

55

Sebastian Bannwarth Aachen University

Siloxane removal using silicone-rubber membranes The interest in using landfill and digester gas as a sustainable energry sources has grown. A major challenge using these sources is the precence of volatile methylsiloxanes (VMS). When a gas containing VMS is combusted silica deposits are formed. These deposits harm the Siloxane removal using silicone-rubber membranescombustion engines and reduce their lifetime. State-of-the-art technology to remove the siloxanes from the gas is adsorption on activated carbon. Alternative methods are absorption, deep chilling or condensation. A new purification technology using membranes has now been tested. The permeabilities of common VMS in a commercially available polydimethylsiloxane (PDMS) membrane are determined as a function of temperature. A synthetic biogas mixture containing silicon in landfill gas-typical concentrations is purified in 3-end and 4-end operation. The results are presented using dimensionless numbers to facilitate upscaling. In general, PDMS can be used for siloxane removal, especially in 4-end operation using ambient air as sweep gas, where energy demand is significantly lower than in 3-end. However, depending on the desired degree of purification, methane losses of approximately 7% must be accepted. Only alternative membrane materials with higher carbon dioxide–methane selectivities have the potential for lower methane losses. Jorge García-Ivars Polytechnic University of Valencia

Recovery of ethyl acetate of aqueous solutions by means of self-made polydimethyl siloxane pervaporation membranes

Introduction Pervaporation (PV) is a kind of membrane separation process with some attractive features like low energy consumption, moderate cost and compact and modular design, compared to traditional processes of dehydration of organic mixtures such as distillation [1, 2]. In a PV process, the components change their aggregate state from liquid to vapour while permeating. In many cases, PV is an economical alternative compared with distillation process due to its demand of energy. The efficiency of PV has been approved in the elimination of water from organic solutions [3]. This application has a great interest in many industrial fields, such as the recovery of ethyl acetate from wastewater of paints and varnishes industries. The PV performances for separating ethyl acetate/water mixtures were investigated to seek the potential application in treating organic solvent contaminated waters to recover and reintroduce the treated organic solvent in the industrial process. Methods In the present work, experiments were carried out in a PV pilot plant, provide with a membrane flat module using different feed concentrations (1, 3 and 5% ethyl acetate-water

56

mixtures) at different temperatures (40, 50 and 60 ºC). The effective membrane area was 78.54 cm2. The pervaporation vapour was condensed by a liquid ethylene glycol/water (50/50) mixture at -30 ºC and the composition of the permeation flux was analyzed by means of a refractive index. Two different kinds of PV membranes were tested: a commercial polydimethylsiloxane membrane (PERVAP-1060, Sulzer Chemtech Membrane Systems A.G.) and a self-made polydimethylsiloxane composite membrane. The copolymer solution of polydimethylsiloxane was prepared into composite membrane as skin layer on microporous support. The surface morphology of both membranes, which were coated with gold to be tested, was observed by a scanning electron microscope (SEM JSM6300, JEOL) [4]. All investigated hydrophobic membranes were selective toward ethyl acetate; however selectivity was dependent on the kind of membrane used for the separation. For this comparison, the separation factor (α) and the partial flux (or permeation flux, Jp) of each investigated membrane were studied. Both parameters were calculated according to the following equations:

Where yEtA refers to the liquid fraction of ethyl acetate in the permeate and xEtA refers to the liquid fraction of ethyl acetate in the feed. Results In contact with aqueous ethyl acetate solutions, the behaviour of both membranes improved, increasing the partial flux and the separation factor with the increase of the feed concentration and the operating temperature (Fig. 1). Comparing the investigated membranes, the highest selectivity was found for PERVAP-1060 at an operating temperature of 40ºC. However, self-made polydimethylsiloxane membrane greatly improved its selectivity at higher temperatures, showing the best results at an operating temperature of 60ºC.

57

Generally, when the operating temperature increased, the polymer chains became more flexible at higher temperatures, leading to the increase of free volume in the polymer matrix [5]. Thus, permeation fluxes increased with the increase of the feed temperature. On the other hand, the selectivity was dominated by the transport properties of the membrane and the thermophysical properties of the feed solution. The selectivity of the membrane changed when the activity coefficient and the saturated vapour pressure changed. Therefore, an increase of the feed temperature caused an increase of the partial pressure of the organic compound, making possible the preferential pass of the organic compound through the membrane. During the process, another important effect was observed. As the process progressed, both membranes showed a swelling effect. This effect is produced by the mutual interactions between the liquid in contact with the membrane (solvent) and the active polymer layer of the membrane. Generally, swelling effect made the membranes more permeable, reducing their selectivity. However, the excessive swelling of the active layer impeded the transport of ethyl acetate (with larger molecule diameter). The most serious consequence of swelling effect is the breaking of the membrane, thus they must be regenerated. Therefore, further studies would be needed to prevent the negative behaviour of the swelling effect in the characteristics of the membrane. Conclusions In this work, the influence of operating temperature and feed ethyl acetate content on the PV performance were investigated. This study demonstrates that an increase of the feed temperature causes an important increase of the membrane’s permselectivity (permeation flux and separation factor) and, moreover, an improvement of the membrane’s behaviour was observed in PV process. This particular property was observed when the fraction of ethyl acetate in feed increased. References [1] S. Xia, X. Dong, Y. Zhu, W. Wei, F. Xiangli, W. Jin. Dehydration of ethyl acetate–water mixtures using PVA/ceramic composite pervaporation membrane. Separation and Purification Technology 77 (2011) 53-59. [2] W. Kujawski, A. Warszawski, W. Ratajczak, T. Porebski, W. Capala, I. Ostrowska. Removal of phenol from wastewater by different separation techniques. Desalination 163 (2004) 287-296. [3] B-K. Zhu, X-Z. Tian, Y-Y. Xu. Recovering ethyl acetate from aqueous solutions using P(VDF-co-HFP) membrane based pervaporation. Desalination 184 (2005) 71-78. [4] H. Matsuda, H. Yanagishita, H. Negishi, D. Kitamoto, T. Ikegami, K. Haraya, T. nakane, Y. Idemoto, N. Koura, T. Sano. Improvement of ethanol selectivity of silicalite membrane in pervaporation by silicone rubber coating. Journal of Membrane Science 210 (2002) 433-437. [5] D. Yongquan, W. Ming, C. Lin, L. Mingjun. Preparation, characterization of P(VDF-HFP)/[bmim]BF4 ionic liquids hybrid membranes and their pervaporation performance for ethyl acetate recovery from water. Desalination, 295 (2012) 53-60. Sayed Sadr University of Surrey

Modelling the removal of organics in nanofiltration for water reuse Nanofiltration (NF) is an effectual and ecologically convenient technology for decontamination and water reuse. NF in a large number of studies has shown the capability

58

of removing different emerging organic micro-pollutants such as endocrine disrupting compounds (EDCs) and pharmaceutical active compounds (PhACs). The major problems involved in nanofiltration application and during the filtration are rejection decline and increase in fouling which might not be completely predictable. There are some models to assess and predict the rejection of organics. However, they are generally either statistic models or more related to the material science of the membranes. Therefore, the study aims to represent a mechanism-based model which can evaluate the behaviour of organics in nanofiltration rejection. The mechanisms to be considered in the model can be divided into three different assortments: 1) Steric hindrance: Steric hindrance plays a major role when the large size of groups within a molecule and/or the spatial structure of a molecule prevent chemical reactions that can be observed in some other molecules with smaller groups or sizes. Steric hindrance is mainly correlated to the ratio of the size of the solute to the size of the membrane pores. 2) Hydrophobic-hydrophobic adsorption: Van der Waals interaction is defined as the sum of the attractive or repulsive forces between molecules. Hydrophobic-hydrophobic (Van der Waals) interactions between the solutes and the membranes are likely to affect organic rejection. 3) Electrostatic repulsion: This arises if two molecules carry the same charge approach each other. Electrostatic repulsion between charged molecules and the charged membrane surface might positively affect the rejection of micropollutants. The description of the model is made up of the parameters, such as Molecular weight, flux, time, and hydrophobicity, which are correlated to the organic rejection mechanisms. The organic rejection has been modelled as: R (%) = f (Steric hindrance) + f (Adsorption) + f (Electrostatic repulsion) Where R is rejection efficiency. After understanding the mechanisms and considering the parameters, parameter estimation, calibration and validation of the model should be conducted. The software AQUASIM has been used for parameter estimation, calibration and validation. The results show that this model is able to correctly assess and model the organics rejection in nanofiltration. It has been concluded that a classification of compounds into four major assortments is needed. Presumably, the validation of the model with more sets of data will lead to having better results. In addition, combination of this new model with statistical models would be worthwhile in order to undertake further research. Keywords: Nanofiltration; Pharmaceuticals; Endocrine disruptors; Modelling; Rejection mechanism

72

On Saturday afternoon we will be holding demonstrations of the Continuous Membrane Casting and Spinning processes. Further information about these processes is below.

Continuous Membrane Casting Demonstration

A commonly used technique for polymer membrane preparation is the immersion precipitation process. This process involves spreading a previously prepared polymer solution onto a flat surface, followed by insertion into a coagulation bath in order to obtain a solid film. Bench top casting machines are used for laboratory membrane preparation. However, these machines are not suitable for preparing membranes in a commercial scale. For that purpose a continuous casting process needs to be implemented. We, at the Chemical Engineering Department in Imperial College, have one such machine built in-house (Figure 1).

Figure 1: Schematic representation of a continuous casting machine – 1) mother roll with non-woven material, 2) alignment reels, 3) casting knife, 4) casting table, 5) non-woven membrane support, 6)

collection roll for the cast membrane, 7) motor, 8) non-solvent (water) bath [1]

Usually an even film of polymer dope solution is spread across a non-woven support. The support fabric is placed on the mother roll (1) and pulled over the alignment reels (2) to the collection roll (6). To ensure that the film will be cast evenly, the non-woven needs to be fixed on the rolls (1) and (6) with enough tension. Following this, the coagulation bath (8) is filled with non-solvent (in our case water) until a desired level. The level is chosen based on whether a partial solvent evaporation step prior to immersion precipitation is desired or not. The next step is to adjust the gap between the casting knife (3) and the support fabric to set the desired polymer film thickness. The motor (7) has a control box which can generate speeds up to 4.5 m/min. Finally, the prepared dope solution is poured gently into the casting knife trough (3) and the motor (7) is switched on. This will begin the rotation of the collection roll (6) and pull the applied film through the coagulation bath (8) where phase inversion takes place. The finished membrane is collected on the roll (6) and ready for post formation treatment and rolling into membrane modules.

[1] Soroko I., Makowski M., Spill F., Livingston A. Journal of Membrane Science 381 (2011) 163

TECHNICAL DEMONSTRATIONS

73

Spinning Demonstration

Spinning is one of most widely adopted techniques for fabricating ceramic hollow fibres. There are three main steps in preparing the ceramic hollow fibre membranes: preparation of spinning suspension, spinning of hollow fibre precursors and finally sintering of hollow fibre membranes. Firstly, ceramic powders, organic binders, solvent and additives are mixed to obtain a homogeneous spinning suspension. After degassing, the suspension is transferred to a stainless steel reservoir and the extrusion rate is controlled by a syringe pump. The hollow fibres are spun through a tube in orifice, which consist of a central bore and an annulus. Internal and external coagulant (tap water) is used to promote the phase inversion.

The membrane morphology can be varied by controlling the spinning parameters (air gap, extrusion rate of spinning suspension and type and flow rate of internal coagulant).

After the spinning process, the hollow fibre precursors need to undergo a high temperature treatment known as sintering to transform it into the hollow fibre membrane.

Figure 2 – Schematic diagram of spinning process for hollow fibre.

74

We would like to acknowledge the financial support provided by the European Commission’s FP7 People programme. This course is being run as part of MemTide (Membrane Enhanced Tide Synthesis - A New Paradigm Peptide/Oligonucelotide Synthesis Technology), a four year Marie Curie Initial Training Network funded by the 7th Framework Programme of the European Commission's Marie Curie Initiative. MemTide's main goal is to train researchers within the context of a network-wide scientific target in line with FP7 People Programme's key objectives, namely to strengthen the scientific and technological base of European industry and to foster its international competitiveness. Some funding has also been made available to offer training to researchers from outside the network The MemTide project will run until November 2013, bringing together six partners from five European countries, namely Imperial College London, University of Turku, Institute for Research in Biomedicine, Evonik MET Ltd, Janssen and Lonza. Their combined expertise will be used to develop research programmes to create a new generation of synthesis technologies for peptide and oligonucleotide ('tide') manufacture, with focus on the use of emerging membrane technology to effect critical separations. For further information about MemTide please visit the project website: http://www.imperial.ac.uk/memtide

CONFERENCE SPONSORS

EC FP7 PROGRAMME – THE MEMTIDE PROJECT

75

We are grateful to the European Membrane Society for supporting this conference. The EMS is a non-profit society devoted to the promotion and transfer of scientific information. It is a meeting forum for scientists and engineers who work in the field of membrane science and technology. Joining the Society will help you to keep informed of the most recent developments in the field of membranes. You’ll also get discounted registration fees to all the scientific meetings (schools, conferences, workshops) that are approved by the Society. You can be an individual member, or your company or institution can become a corporate member of the Society. In the latter case, a corporate member receives two copies of the newsletters, two members of the company get discounted fees when attending EMS events, and the corporate member clearly shows its support for the activities in science and technology of membranes and membrane processes. For further information about the EMS, including details of how to become a member, please visit their website at www.emsoc.eu

THE EUROPEAN MEMBRANE SOCIETY

76

NYM14 will be held in the Department of Chemical Engineering at Imperial College London, which is highlighted in orange on the campus map below.

PRACTICAL INFORMATION AND MAPS

Conference Venue

77

Due to ongoing renovation works, access to the building’s main entrance is not currently available. Participants will therefore need to enter the Chemical Engineering (ACE Extension) building at Level 1 – which is at street level. If you are entering the campus through the main building on Exhibition Road, walk straight through the Business School lobby and you will see the Faculty Building (blue glass building) on your left. Continue straight ahead towards the walkway which is directly under the large white sign for “Sherfield Building, Restaurants, Shops etc”. Once you have passed the Imperial College shop on your right, you will see a staircase leading down to street level. Once you have reached street level, turn around and walk between the two buildings to the left. The entrance to the Chemical Engineering building is located to your right. Directions from the walkway are shown in the diagram below.

If you are entering the campus from the Prince Consort Road entrance, turn left when you reach a junction and can see the main walkway ahead of you. Walk between the two buildings on your left, and you will see the entrance to the Chemical Engineering building to your right. The conference will take place on Level 2 of the Chemical Engineering building. Take either the lift of the stairs up, and the registration desk will be sited in the main concourse. The route towards registrations will be signposted from the entrance on Level 1.

78

The first of the conference dinners, to which all participants are invited as our guests, will take place on the evening of Thursday 20 September, from 7.00pm. The venue is the Eastside Restaurant and Bar, Prince’s Gardens, London SW7 1AZ. Eastside is located on Imperial College London’s South Kensington Campus, around a five minute walk from the Chemical Engineering building. Eastside is marked as building number 19 on the campus map below (on the far right of the map).

Thursday dinner – Eastside Restaurant

79

The gala dinner will be preceded by a bus tour taking in all of London’s major landmarks. The open-top bus will collect us from Imperial College London at 4.00pm on Friday 21 September, and after a two and half hour tour of the city, we will be dropped off at the dinner venue. Although the venue for the gala dinner has not yet been confirmed, the location will be easily accessible since transportation to the restaurant will be provided. Further details will be circulated at the conference. The final conference dinner, a traditional pub meal, will take place on Saturday 22 September, from 7.00pm. The venue is The Britannia pub in Kensington, at 1 Allen Street, London W8 6UX, which is a 10-15 minute walk away from the Imperial College London campus. The location is shown on the map below – The Britannia is marked in red to the left of the map, and the Imperial College London campus is outlined in red on the right. The simplest route to the venue is to walk along Kensington Road (the orange road running along the top of the map). However, it is also possible to walk the short distance from the Imperial campus to South Kensington underground station. From here, travel on the Circle or District line westbound for two stops to High Street Kensington station.

Friday bus tour and gala dinner

Saturday dinner – The Britannia

80

NOTES

81

NOTES

82

NOTES

83

NOTES

84

NOTES

85

NOTES