The Effects of Antifoams on Ultrafiltration Membranes
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1 The Effects of Antifoams on Ultrafiltration Membranes By Jean-Paul Lecomte Dow Corning Corporation Dow Corning Silicone Solutions As the pioneer of silicon-based technology, Dow Corning has been improving customers products and profitability for more than 60 years. With a full range of product and application solutions, reliable supply, world-class manufacturing, and global reach, Dow Corning can meet virtually any silicone-related need through our total solution offering and technology leadership. For more information, call Dow Corning ( provides performance-enhancing solutions to serve the diverse needs of more than 25,000 customers worldwide. A global leader in technology and innovation, offering more than 7,000 products and services, Dow Corning is equally owned by The Dow Chemical Company and Corning Incorporated. More than half of Dow Corning sales are outside the United States. The Effects of Antifoams on Ultrafiltration Membranes By Jean-Paul Lecomte Figure 1: Hydrophilic Surface Formation on Membrane Surface Membrane fouling has been a major drawback to ultrafiltration as a separation and purification system. The causes and theories behind membrane fouling, as well as system optimization and the effect of fouling on membrane life, have been studied extensively 1,2,3. In particular, antifoams have been found to cause significant fouling of membranes. The purpose of this paper will be to discuss the problem of membrane fouling by antifoams, investigate the leading causes of fouling and describe the development of a nonfouling antifoam for processes that use ultrafiltration downstream. Membrane fouling by antifoams may be caused by several factors, including hydrophobic interactions between emulsion components and the membranes, cloud point effects of emulsion stabilizers, and gel layer formation at the water-membrane interface. In the context of foam control in fermentation systems, there are three major kinds of antifoams: silicone compounds emulsified in water, silicone compound emulsified into a polyglycol, and polyglycols used alone. The silicone itself is not water soluble; therefore, the emulsifiers and polyglycols are needed to allow the silicone to be dispersed and released in the water. It was found that the emulsifiers, surfactants, thickeners and polyglycols are the main contributors to membrane fouling.
2 Typical surfactants found in emulsions used in fermentation are glycerol monostearates, polyoxyethylene sorbitan stearates and polyoxyethylene monostearates. Surfactants are molecules that are both hydrophobic and hydrophilic. They contain a lipophilic end, such as a long fatty chain, as well as a hydrophilic end, such as glycerols and ether or ester linkage units. It has been theorized that the hydrophobic end of the molecule may cling to the surface of the membrane and cause fouling. The hydrophobic nature of polysulfone membranes may cause other nonpolar or hydrophobic compounds to be adsorbed onto the surface of the membranes. Fane et al. 4 showed that pretreating the membranes with a wetting agent tends to decrease the hydrophobicity of the membrane surface. The surfactant forms an even layer on the surface of the membrane, creating a hydrophilic surface. (See Figure 1.) As a result, hydrophobic particles in the bulk fluid tend not to cling to the membrane surface as much, allowing greater flux through the membranes. This pretreatment is effective, causing an initial flux increase of approximately 20% and a reduction in the subsequent flux decline. The wettability of the membranes is evidence that the hydrophobic-hydrophobic interactions do exist, and that they have a significant impact on membrane fouling by nonpolar components of the bulk fluid. A more hydrophilic membrane could be substituted for the polysulfone membrane, but polysulfone is more desirable due to its thermal, chemical and ph stability. However, a hydrophilic surface is not always created by the presence of surfactants. An uneven surface may result if the surfactant or organic defoamer falls out of solution and spreads across the surface of the membrane. Figure 2: Micelle Formation at Higher Temperatures Many organic defoamers and silicone antifoams contain non-ionic emulsifiers that have cloud points, the temperature at which liquid-liquid phase separation occurs. When the temperature is increased beyond the soluble range, the water of hydration breaks away, and the surfactant micelles grow in size to such an extent that the solution becomes cloudy. (See Figure 2.) Above the cloud point temperature for a given surfactant, the surfactant may function as a defoamer; below that point it may actually promote foam. A study by McGregor et al. found that these defoamers do not have detrimental effects on the membranes below the cloud point. Above the cloud point, however, significant fouling was observed 1. Fermentation and enzyme reactions are generally conducted at temperatures around 40 C (104 F), well above the cloud points of most of the surfactants. A process stream that contains these antifoams can be successfully ultrafiltered if the temperature can be decreased below the cloud points of the surfactants. However, an easier and more economical solution would be simply to change the defoamer. Studies have shown that even antifoams with no cloud points can cause fouling, but the extent of fouling is not tem-perature dependent 1,2. Another flux-reducing property inherent in cross-flow filtration is that of gel layer formation at the membrane surface 5,7. Particles in the filtration media are deposited on the surface of the membrane, resulting in a layer that inhibits flux through the membrane. Most antifoam emulsions contain water thickeners such as cellulose ethers and xanthan gums. Testing of the emulsions that contain such thickeners showed that they contribute significantly to fouling. These thickeners are long polymer chains of anhydroglucose backbone that have high molecular weight. When the thickeners are dissolved in water, the long thread-like polymers are jacketed with layers of water molecules, which increases the product bulk viscosity. The water molecules act as a lubricant, enabling the long chains to slide over each other and weave together 8. However, these thickeners have a behavioral phenomenon similar to surfactants that is called the gel point. As a solution is heated, the water of hydration breaks away, and a thick gel is formed by the extensive entanglement of the polymer chains. It is believed that a similar phenomenon occurs on the surface of the membrane. As the polymers come in contact with the membrane surface, the loosely bound water breaks away and the chains lock together. This causes a gel layer to form on the surface of the membrane.
3 Experimental Results The membrane fouling tests were conducted using either polysulfone membranes in a plate-and-frame ultrafiltration unit (DDS Filtration, Mini-lab 10, GR 60 PP 10) having a molecular weight cutoff of 25,000, or hollow fiber membranes (Romicon HF1-43-PM50) having a molecular weight cutoff of 50,000. The pressure drop across the membrane was ~5 psi. Ten liters of deionized water were fed through the ultrafiltration system for ~1 hour to allow a steady state to be established. The permeate flux is then measured and defined as initial flux. This is considered to be the 100% to which all subsequent fluxes are compared. Antifoam is added and the permeate flux measured every 30 minutes. The retentate and the permeate are both fed back to the feed solution. Figure 3: Membrane Fouling by Various Antifoams The first tests that were run verified that antifoams do foul ultrafiltration membranes. (See Figure 3.) These data were obtained using 100 ppm active antifoam in deionized water. The data were reported as percent flux as compared with deionized water. The polyglycol used in this study is a polypropylene glycol, the organic/silicone blend is ~5% silicone emulsified into polypropylene glycol, and the emulsions are 10 to 20% silicone compound emulsified into water by the surfactants and thickeners described previously. Since the emulsions contained various amounts of silicone and caused the same fouling as did the organic silicone blends, it was believed that the silicone might not be responsible for the membrane damage. Figure 4: Effect of Surfactants on Relative Flux The components of antifoam emulsions were then examined for membrane fouling. It was found that the surfactants used to stabilize and disperse the silicone emulsions contribute significantly to membrane fouling. (See Figure 4.) Addition of antifoam compound to the surfactant did not increase fouling. Addition of thickener to the surfactant, however, further decreased permeate flux throughout the membrane. Comparisons of various types of antifoams and surfactants with varying cloud points confirm that micelle formation at the cloud points also contributes significantly to membrane fouling 1.
4 Figure 5: Effect of Thickeners on Relative Flux The thickeners used in emulsions were then examined for membrane fouling and found to cause significant decrease in flux. (See Figure 5.) It was also noted that the addition of surfactants and silicone caused additional loss of flux. The silicone compound is typically a polydimethylsiloxane, which is a long polymer chain that may cause further entanglement of the thickeners. These results suggest that, collectively, silicone, surfactants and thickeners cause membrane fouling by silicone and water emulsions, while the low cloud points of organic compounds contribute significantly to membrane fouling by other defoamers. Ultrafiltration membrane fouling by antifoam formulations can be diminished by eliminating the sources of fouling from the other components. This involved modifying the delivery system of the silicone to the aqueous media. The new delivery system must effectively disperse in water; it cannot function via cloud point and cannot contain any gel-forming or long chain polymers. Figure 6: Flux vs. Temperature Dow Corning 1920 Powdered Antifoam is the result of these requirements. It is 20% silicone adsorbed onto a food-grade solid. The antifoam does not function by cloud point nor will it form irreversible gels. As the temperature is increased, the flux through the membrane increases as well. (See Figure 6.) This increase is a function of the membrane. The antifoam will disperse gradually in water to release the antifoam. In addition, the antifoam is safe to fermentation media and organisms and has FDA approval. The product is sterilizable by autoclaving and dry heat at certain conditions.
5 Figure 7: Effect of Dow Corning 1920 Powdered Antifoam on Relative Flux Figure 8: Defoam Performance of Dow Corning 1920 Powdered Antifoam vs. Various Antifoams Dow Corning 1920 Powdered Antifoam has been shown to cause minimal fouling in comparison with organic antifoams and silicone emulsions. (See Figure 7.) The solid antifoam caused only 10 to 20% loss of flux through time, compared with organics and emulsions that caused 60 to 80% loss of flux. The defoam performance of the solid antifoam is also quite good in comparison with polyglycols as well as silicone emulsions. (See Figure 8.) These tests were conducted using a mechanical shaker using 100 ppm of the antifoam in a fermentation nutrient media. It was found that the solid antifoam performs better for a longer period of time due to its gradual release into the media. References 1. W.C. McGregor, J.F. Weaver, S.P. Tansey, Antifoam Effects on Ultrafiltration, Biotech. and Bioengineer, 31: J. Kloosterman, P.C. van Wassenaar, N.K.H. Slater, H. Baksteen, The Effect of Anti-foam Agents on the Ultrafiltration of a Protease Solution, Bioprocess Eng., 3: S.L. Michaels, Crossflow Microfilters: The Ins and Outs, Chem. Eng., January, pp , (1989). 4. A.G. Fane, C.J.D. Fell, K.J. Kim, The Effect of Surfactant Pretreatment on the Ultrafiltration of Proteins, Desalination, Vol. 53, pp , (1985). 5. J.M.S. Cabral, B. Casale, C.L. Cooney, Effect of Antifoam Agents and Efficiency of Cleaning Procedures on the Cross-Flow Filtration of Microbial Suspensions, Biotech. Letters, Vol. 7, No. 10, pp , (1985). 6. S. Wang, G. Hu, Membrane Fouling and Determination of Gel Layer Growth Rate in Membrane Separation, Desalination, Vol. 56, pp.
6 , (1985). 7. J.A. Howell, O. Velacangil, Theoretical Considerations of Membrane Fouling and Its Treatment with Immobilized Enzymes for Protein Ultrafiltration, Journal of Applied Polymer Science, 27: The Dow Chemical Company, Methocel Cellulose Ethers Technical Handbook, pp. 4, 21, How to Contact Us Dow Corning has sales offices, manufacturing sites, and science and technology laboratories around the globe. Telephone numbers of locations near you are available on the World Wide Web at or by calling one of our primary locations listed below. Your Global Connection Americas Europe Asia LIMITED WARRANTY INFORMATION PLEASE READ CAREFULLY The information contained herein is offered in good faith and is believed to be accurate. However, because conditions and methods of use of our products are beyond our control, this information should not be used in substitution for customer s tests to ensure that Dow Corning s products are safe, effective, and fully satisfactory for the intended end use. Suggestions of use shall not be taken as inducements to infringe any patent. Dow Corning s sole warranty is that the product will meet the Dow Corning sales specifications in effect at the time of shipment. Your exclusive remedy for breach of such warranty is limited to refund of purchase price or replacement of any product shown to be other than as warranted. DOW CORNING SPECIFICALLY DISCLAIMS ANY OTHER EXPRESS OR IMPLIED WARRANTY OF FITNESS FOR A PARTICULAR PURPOSE OR MERCHANTABILITY. DOW CORNING DISCLAIMS LIABILITY FOR ANY INCIDENTAL OR CONSEQUENTIAL DAMAGES. Dow Corning is a registered trademark of Dow Corning Corporation. We help you invent the future is a trademark of Dow Corning Corporation Dow Corning Corporation. All rights reserved.
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