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Examination of Methods to Reduce Membrane Fouling During EXAMINATION OF METHODS TO REDUCE MEMBRANE FOULING DURING DAIRY MICROFILTRATION AND ULTRAFILTRATION A Thesis Presented to the Faculty of the Graduate School of Cornell University in Partial Fulfillment of the Requirements for the Degree of Master of Science by Michael Corey Adams January 2012 © 2012 Michael Corey Adams ABSTRACT Pressure-driven membrane filtration processes such as microfiltration (MF), ultrafiltration (UF), nanofiltration (NF), and reverse osmosis (RO) provide opportunities for the dairy industry to better utilize milk by separating its components based on size. However, widespread adoption of some of these processes has yet to be realized due to membrane fouling. Membrane fouling is the accumulation of soil, or foulant, on the surface or within the pores of a membrane. Fouling prolongs processing times, increases energy and cleaning costs, decreases separation efficiency, and, in severe cases, may lead to irreversible clogging of the membrane. Microfiltration can be used to remove serum proteins (SP) from skim milk. The process’ SP removal efficiency directly influences the technology’s financial feasibility. Our first objective was to quantify the capacity of 0.14 µm ceramic Isoflux MF membranes to remove SP from skim milk. The Isoflux membranes’ manufacturer claims that using these membranes will reduce localized membrane fouling at the inlet end of the membrane that results from using high cross-flow velocities (5 – 7 m/s) to mitigate overall membrane fouling. Contrary to theoretical cumulative SP removal percentages of 68%, 90%, and 97% after 1, 2, and 3 stages of 3X MF processing, respectively, the 3X Isoflux process removed only 39.5%, 58.4%, and 70.2% after 1, 2, and 3 stages, respectively. Several design aspects of the membrane are thought to have resulted in this inefficiency. Ultrafiltration can be used to concentrate SP and reduce the lactose content of cheese whey or MF permeate of skim milk to produce 80% whey protein concentrates (WPC80) or 80% serum protein concentrates (SPC80), respectively. The objectives of our second study were to determine if adding annatto color to milk or bleaching whey or MF permeate of skim milk with hydrogen peroxide (H2O2) or benzoyl peroxide (BPO) influenced UF flux, diafiltration flux, or membrane fouling during production of WPC80 or SPC80. Addition of annatto color to milk had no effect on flux or fouling. Bleaching with or without added color increased flux during processing. Bleaching with H2O2 produced higher flux than bleaching with BPO. While bleaching with BPO reduced membrane fouling during WPC80 production, it did not impact membrane fouling during SPC80 production. Bleaching with H2O2 led to the largest reduction in fouling for both production processes. BIOGRAPHICAL SKETCH Michael Adams was born on October 2, 1982 in Nashville, TN. After graduating with honors from Hume-Fogg Academic Magnet High School in 2001, Michael left Nashville for Charleston, SC to attend culinary school at Johnson & Wales University. It was here that Michael was introduced to food science during a baking technology course. He was so taken with this new field that after earning his A.S. in baking and pastry arts, Michael returned to his home state and began his B.S. studies in food science at the University of Tennessee, Knoxville. At Tennessee, Michael worked in the sensory lab, performed undergraduate dairy science research, placed first in the nation in ice cream judging at the IDFA collegiate dairy products judging competition, and served as vice-president of the food science club. During the summer and fall of 2005, he completed an internship at Bush Brothers & Company in their R&D department. In 2006, Michael graduated with high honors and eagerly accepted a research scientist position at Daisy Brand’s burgeoning R&D department in Dallas, TX. In 2007, Michael married Shan, his girlfriend of 7 years. During his time at Daisy Brand, Michael learned about the production of sour cream and cottage cheese and gained an appreciation for the importance of making pure and natural dairy products. Although he enjoyed his time in industry, he wanted to gain a deeper understanding of dairy science. In 2009, Michael and Shan moved from Dallas to Ithaca, NY for what was expected to be a two year commitment to the M.S. program in food science at Cornell University. However, because he enjoyed what he was studying (and his wife’s patience matched his love for food science), Michael decided to continue on toward his doctoral training. iii I dedicate this work to my mom, Mary Wigger, who has always encouraged me to follow my passion. iv ACKNOWLEDGMENTS First and foremost I want to extend my deepest gratitude to my advisor, Professor Dave Barbano, for his hours of advice in teaching me to be a more responsible scientist and a more effective presenter. I also want to express my sincere appreciation to Professor Giles Hooker of the Department of Biological Statistics and Computational Biology for taking the time to guide me in my minor studies. I am obliged to the New York State Milk Promotion Board, the Northeast Dairy Foods Research Center, and the Cornell University Department of Food Science for their generous funding. I am grateful for the technical assistance and entertaining pilot plant conversation given graciously by Tim Barnard, Michelle Bilotta, Sara Bova, Tom Burke, Maureen Chapman, Chassidy Coon, Jessica Mallozzi, Mark Newbold, Karen Wojciechowski, and Justyna Zulewska. It always helps to be in the same boat with outstanding colleagues. I want to thank my fellow graduate lab mates Irma Amelia, Steve Beckman, and Emily Hurt for helping me navigate my way through these last two years. I would like to give special thanks to Dr. Brandon Nelson for pushing me to pursue my graduate studies and showing me that dairy science is about far more than just manufacturing sour cream and cottage cheese. Finally, I want to thank my family: my mom, Chris, Stephanie, and especially my intelligent, beautiful, and above all… patient wife, Shan. Your love and support have provided me with more than enough reason and strength to succeed when times have been the most trying. v TABLE OF CONTENTS Biographical sketch………………………………………………………………………… iii Dedication…………………………………………………………………………………… iv Acknowledgements…………………………………………………………………………. v Table of contents……………………………………………………………………………. vi List of figures……………………………………………………………………………….. ix List of tables………………………………………………………………………………… xi List of abbreviations……………………………………………………………………….. xiii Chapter 1: Membrane fouling and flux decline in dairy processing……………………. 1 Introduction………………………………………………………………….. 1 Membrane processes…………………………………………………………. 4 Microfiltration……………………………………………………….. 4 Ultrafiltration………………………………………………………… 5 Nanofiltration………………………………………………………… 6 Reverse osmosis…………………………………………………...… 6 Fouling mechanisms and progression………………………………………... 7 Concentration polarization…………………………………………… 7 Fouling mechanisms…………………………………………………. 8 Stages of fouling…………………………………………………….. 10 Effect of feed material………………………………………………………. 12 Foulant material present in dairy fluids……………………………… 12 Feed concentration…………………………………………………… 15 Feed chemistry……………………………………………………….. 16 Effect of membrane type…………………………………………………….. 18 Membrane material…………………………………………………... 18 Membrane design……………………………………………………. 21 Effect of processing conditions……………………………………………… 23 Membrane flux and cross-flow velocity…………………………….. 23 Transmembrane pressure……………………………………..……… 24 Temperature………………………………………………………..… 25 Fouling reduction…………………………………………………………….. 26 Ceramic microfiltration……………………………………………… 26 Polymeric spiral wound ultrafiltration……………………………….. 29 Cleaning……………………………………………………………… 29 Fouling quantification………………………………………………………... 31 Fouling coefficient…………………………………………………… 31 Hydraulic resistance………………………………………………….. 31 Membrane imaging…………………………………………………... 32 Conclusions………………………………………………………………….. 33 References……………………………………………………………………………. 34 vi Chapter 2: Serum protein removal from skim milk with a 3-stage, 3X ceramic Isoflux membrane process at 50°C………………………………………………………………… 40 Abstract…………………………………………………………………………..….. 40 Introduction………………………………………………………………………..… 41 Materials and methods………………………………………………………………. 44 Experimental design and statistical analysis………………………………… 44 Microfiltration operation…………………………………………………….. 45 Cleaning prior to processing…………………………………………. 46 Processing……………………………………………………………. 47 Cleaning after processing……………………………………………. 49 Chemical analyses…………………………………………………………… 50 SP removal estimation using Kjeldahl analysis of permeates……….. 50 Color analysis of skim milk and retentates…………………………………... 51 SDS-PAGE electrophoresis………………………………………………….. 51 Relative percentage of β-LG to β-LG plus α-LA in skim milk, permeate and retentate samples……………..……………………… 53 CN passage through the membrane………………………………….. 53 Comparison of membranes for 95% SP removal……………………………. 53 Stage number calculation…………………………………………….. 53 Membrane surface area calculation………………………………….. 54 Results………………………………………………………………………………... 54 MF processing parameters…………………………………………………… 54 Composition and color……………………………………………………….. 61 Skim milk composition……………………………………………… 61 Permeate composition……………………………………..………… 61 Retentate composition………………………………….….………… 62 Stage feed, retentate, and permeate pH……………………………… 63 Skim milk and retentate color…………………………………..…… 64 SP removal and CN passage………………………………………………… 64 SP removal…………………………………………………………… 64 β-LG and α-LA partitioning…………………………………….……
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