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By 
Geethu S 
2011-06-007
INTRODUCTION 
 
 Emulsion is a type of colloid formed from a mixture of 
two or more immiscible liquid such as water and oil 
 Two phase- continuous phase and dispersed phase 
 Two type- water in oil and oil in water emulsion 
 Eg: egg ,cheese, milk, margarine
Methods of preparation of emulsion 
 
 Stirring equipment 
 Colloid mill 
 Homogenizers 
 Ultrasonics or microfluidizers
MEMBRANE EMULSIFICATION 
 
 It’s a novel techniques for producing single and 
multiple emulsions 
 Introduced by Nakashima and Shimizu in 1980s in 
Japan 
 The dispersed phase is forced through the pores of a 
microporous membrane directly into the continuous 
phase by using low pressure 
 Emulsified droplets are formed and detached at the 
end of the pores with a drop-by-drop mechanism
Contd…. 
 
 Droplet detachment of the membrane surface 
dependant on four main forces 
• Shear 
• Interfacial tension between emulsified fluids 
• Inertia/pressure from the flow through the membrane 
• Buoyancy 
 Resulting droplet size is controlled primarily by the 
choice of the membrane
 
Fig: Schematic diagram of ME process
Parameter affecting the emulsion production 
 
Membrane parameters 
 Phase parameters 
 Process parameters
 
Membrane parameters 
 Pore size 
 Pore shape 
 Pore size distribution 
 Porosity 
Wettability 
 Permeability 
 Thickness
 
Phase parameters 
 Interfacial tension 
 Emulsifier type and concentration 
 Viscosity 
 Density
 
Process parameters 
Wall shear stress 
 Transmembrane pressure 
 Temperature
Membrane materials 
 
 SPG membrane (.1-20μm) 
 Silicon membrane 
 silicon nitride microseive membrane 
 Ceramic aluminium oxide membrane 
 Polytetrafloroethylene membrane
Types of membrane emulsification 
 
 Dead end membrane emulsification 
 Cross flow membrane emulsification 
 Vibrated membrane emulsification 
 Rotating membrane emulsification
Dead end membrane emulsification 
 
 Simplest form 
 This method employs applied pressure to force the 
dispersed phase through a porous membrane into the 
continuous phase 
 Droplets form at the pore and detach when they reach 
a specific size relative to the size of the pore 
 Surfactant is added to the continuous phase to stabilize 
the newly formed droplets and prevent droplet 
coalescence 
 PTFE is used as membrane

Cross flow membrane emulsification 
 
 Continuous phase to provide shear by flowing it across 
the surface of the membrane 
 Droplets are detached before becoming large enough to 
spontaneously detach and smaller relative to the 
membrane pore size
+ 

Vibrating membrane emulsification 
 
 Uses vibration of the membrane (either sub sonic or 
ultrasonic) to detach droplets from the membrane 
 Improve the efficiency of emulsification in some 
circumstances
Rotating membrane emulsification 
 
 Centrifugal force will work along with the shear at the 
membrane surface provided by the rotation to detach 
droplets
Preparation of food materials 
 
Simple emulsion 
• Two main types of simple emulsion ,(o/w) 
emulsions and(w/o) emulsions 
• ME is suitable for preparation of large scale 
w/o food emulsions 
• Using SPG membranes, o/w emulsions with 
liquid butter fat or sunflower oil as the 
dispersed phase and a continuous phase 
containing milk proteins
 
Multiple emulsion 
 “Emulsion of emulsion” 
 The primary emulsion may be produced by means of a 
conventional method or by membrane emulsification 
 The mild conditions of membrane emulsification are 
especially useful for the second emulsification step in 
order to prevent rupture of the double emulsion 
droplets
 
Encapsulation 
 Microcapsules containing viable cells (Lactobacillus 
casei) were produced using the ME technique 
 Stability of encapsulated cells are high
 
Aerated gel 
 Food gels are soft solids containing a high amount of 
aqueous phase 
 Aerated food gels were produced recently by 
membrane foaming 
 Pressing the dispersed phase (gas) through the pores 
of a tubular membrane into the continuous phase 
 The bubbles formed are covered with surface-active 
substances of the continuous phase
 
Industrial applications 
 Suitable for large scale production, they are easy to 
scale-up, by adding more membranes to a device 
 Process can done in both batch and semi- continuous 
process 
 Product obtained from ME is very stable, for at least 6 
months without the use of preservative,
ADVANTAGES 
 
 Lower energy input with respect to conventional 
emulsifier 
 No foaming, reduced coalescence phenomenon 
 Narrow droplet size distributions 
 Various configurations: premix emulsification, rotating 
device to reduce fouling and increase productivity
DRAWBACKS 
 
 Additional resistance to mass transfer created by the 
membrane 
 Relatively low membrane lifetime; high replacement 
cost 
 Low permeation rate associated to narrow droplet size 
distribution and reduced productivity 
 Fouling phenomenon on the membrane surface 
and/or in the pores
CASE STUDY 

TITILE :Viscosity change in oil/water food emulsions 
prepared using a membrane emulsification system 
 
Done by: Y. Asano and K. Sotoyama 
Objective: 
 Evaluate the viscosity changes in o/w emulsion 
 Study the physical properties emulsions
Materials and methods 
 
 Membrane emulsification apparatus 
 Materials 
• For the oil phase, corn oil was used. For the water 
phase, deionized water was used 
• Emulsifier polyglycerol esters (PGE) 
• Stabilizer carnageenan
 
Methodology 
 Preparation of emulsion 
 Before emulsification, the MPG tube was pre-soaked in 
the continuous phase in an ultrasonic bath for 30 min 
 The dispersion phase was delivered into the MPG tube 
 The continuous phase circulated in the vessel 
 The pressure of the dispersion phase was gradually 
increased
Contd… 
 
 Dispersion phase was emulsified into the continuous 
phase by passage through the membrane 
 Continued until dispersion phase concentration of 10 
vol% at the emulsifying temperature of 25⁰C was 
reached 
 The dispersion phase volume was calculated by 
measuring the total weight of the vessel 
 Average droplet diameter and the droplet distribution 
were measured using an image analyser system 
 Viscosity by vibration viscometer

Contd… 
 
 Assessment of monodispersed emulsion 
 An index of monodispersion, a coefficient of dispersion 
(α ) 
 α = Sd/Dp 
 Smaller the values, the more monodispersed the 
emulsions (<=.35)
Results and discussion 
 
 The value of α was 0.203, so it was evident that 
emulsion was monodispersed 
 From the micrographs obtained directly after 
emulsification and 1 month after emulsification there 
were no differences between these emulsions

Contd.. 
 
 As the droplet size in the emulsion increased with 
decreasing viscosity
 
Relation ship between droplet diameter and viscosity
CONCLUSION 
 
 Membrane emulsification should is a very interesting 
technique for the food processing industry. 
 Benefits of membrane emulsion for the food processing 
industry may arise from low shear properties, 
especially for the preparation of double emulsions 
 Another advantage of membrane emulsion is the scale-up 
ability of membrane devices 
 Main limitation is fouling phenomenon 
 And it solved by recent process called premix ME
Reference 
 
 Abrahamse, A.J., Lierop, R., Sman, R.G.M., Padt, A.and. Boom, R.M., 2002. Analysis of droplet formation and interactions 
during cross-flow membrane emulsification. J. Membrane Sci. 204: 125–137. 
 Adler-Nissen, J., Mason, S.L.and. Jacobsen, C., 2004. Apparatus for emulsion production in small scale and under 
controlled shear conditions. Trans. Inst. Chem. Eng. C 82: 311–319. 
 Bals, A., Kulozik, U., 2003. The influence of pore size, the foaming temperature and the viscosity of the continuous phase 
on the properties of foams produced by membrane foaming. J. Membrane Sci. 220,:5–11. 
 Bals, A. and Kulozik, U., 2003b. Effect of pre-heating on the foaming properties of whey protein isolate using a 
membrane foaming apparatus. Int. Dairy J. 13: 903–908. 
 Charcosset, C., Limayem, I.and Fessi, H., 2004. The membrane emulsification process – a review. J. Chem. Technol. 
Biotechnol. 79: 209–218. 
 Cheng, C.J., Chu, L.Y., Xie, R., 2006. Preparation of highly monodisperse w/o emulsions with hydrophobicallymodified 
SPG membranes. J. Coll. Interf. Sci. 300:375–382. 
 Christov, N.C., Ganchev, D.N., Vassileva, N.D., Denkov, N.D., Danov, K.D.and Kralchevsky, P.A., 2002. Capillary mechanisms 
in membrane emulsification: oil-in-water emulsions stabilized by Tween 20 and milk proteins. Coll. Surf. A 209:83– 
104.mbrane Sci. 278: 344–348. 
 Dalgleish, D.G., 2006. Food emulsions – their structures and structure-forming properties. Food Hydrocoll. 20: 415–422. 
 Daufin, G., Escudier, J.P., Carrère, H., Bérot, S., Fillaudeau, L.and Decloux, M., 2001. Recent and emerging applications of 
membrane processes in the food and dairy industry. Trans. Inst. Chem. Eng. 79: 89–102. 
 Fuchigami, T.and Toki, M.and Nakanishi, K., 2000. Membrane emulsification using sol–gel derived macroporous silica 
glass. J. Sol-Gel Sci. Technol. 19: 337–341..
Membrane emulsification in food industry

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Membrane emulsification in food industry

  • 1. By Geethu S 2011-06-007
  • 2. INTRODUCTION   Emulsion is a type of colloid formed from a mixture of two or more immiscible liquid such as water and oil  Two phase- continuous phase and dispersed phase  Two type- water in oil and oil in water emulsion  Eg: egg ,cheese, milk, margarine
  • 3. Methods of preparation of emulsion   Stirring equipment  Colloid mill  Homogenizers  Ultrasonics or microfluidizers
  • 4. MEMBRANE EMULSIFICATION   It’s a novel techniques for producing single and multiple emulsions  Introduced by Nakashima and Shimizu in 1980s in Japan  The dispersed phase is forced through the pores of a microporous membrane directly into the continuous phase by using low pressure  Emulsified droplets are formed and detached at the end of the pores with a drop-by-drop mechanism
  • 5. Contd….   Droplet detachment of the membrane surface dependant on four main forces • Shear • Interfacial tension between emulsified fluids • Inertia/pressure from the flow through the membrane • Buoyancy  Resulting droplet size is controlled primarily by the choice of the membrane
  • 6.  Fig: Schematic diagram of ME process
  • 7.
  • 8. Parameter affecting the emulsion production  Membrane parameters  Phase parameters  Process parameters
  • 9.  Membrane parameters  Pore size  Pore shape  Pore size distribution  Porosity Wettability  Permeability  Thickness
  • 10.  Phase parameters  Interfacial tension  Emulsifier type and concentration  Viscosity  Density
  • 11.  Process parameters Wall shear stress  Transmembrane pressure  Temperature
  • 12. Membrane materials   SPG membrane (.1-20μm)  Silicon membrane  silicon nitride microseive membrane  Ceramic aluminium oxide membrane  Polytetrafloroethylene membrane
  • 13. Types of membrane emulsification   Dead end membrane emulsification  Cross flow membrane emulsification  Vibrated membrane emulsification  Rotating membrane emulsification
  • 14. Dead end membrane emulsification   Simplest form  This method employs applied pressure to force the dispersed phase through a porous membrane into the continuous phase  Droplets form at the pore and detach when they reach a specific size relative to the size of the pore  Surfactant is added to the continuous phase to stabilize the newly formed droplets and prevent droplet coalescence  PTFE is used as membrane
  • 15.
  • 16. Cross flow membrane emulsification   Continuous phase to provide shear by flowing it across the surface of the membrane  Droplets are detached before becoming large enough to spontaneously detach and smaller relative to the membrane pore size
  • 17. + 
  • 18. Vibrating membrane emulsification   Uses vibration of the membrane (either sub sonic or ultrasonic) to detach droplets from the membrane  Improve the efficiency of emulsification in some circumstances
  • 19. Rotating membrane emulsification   Centrifugal force will work along with the shear at the membrane surface provided by the rotation to detach droplets
  • 20. Preparation of food materials  Simple emulsion • Two main types of simple emulsion ,(o/w) emulsions and(w/o) emulsions • ME is suitable for preparation of large scale w/o food emulsions • Using SPG membranes, o/w emulsions with liquid butter fat or sunflower oil as the dispersed phase and a continuous phase containing milk proteins
  • 21.  Multiple emulsion  “Emulsion of emulsion”  The primary emulsion may be produced by means of a conventional method or by membrane emulsification  The mild conditions of membrane emulsification are especially useful for the second emulsification step in order to prevent rupture of the double emulsion droplets
  • 22.  Encapsulation  Microcapsules containing viable cells (Lactobacillus casei) were produced using the ME technique  Stability of encapsulated cells are high
  • 23.  Aerated gel  Food gels are soft solids containing a high amount of aqueous phase  Aerated food gels were produced recently by membrane foaming  Pressing the dispersed phase (gas) through the pores of a tubular membrane into the continuous phase  The bubbles formed are covered with surface-active substances of the continuous phase
  • 24.  Industrial applications  Suitable for large scale production, they are easy to scale-up, by adding more membranes to a device  Process can done in both batch and semi- continuous process  Product obtained from ME is very stable, for at least 6 months without the use of preservative,
  • 25. ADVANTAGES   Lower energy input with respect to conventional emulsifier  No foaming, reduced coalescence phenomenon  Narrow droplet size distributions  Various configurations: premix emulsification, rotating device to reduce fouling and increase productivity
  • 26. DRAWBACKS   Additional resistance to mass transfer created by the membrane  Relatively low membrane lifetime; high replacement cost  Low permeation rate associated to narrow droplet size distribution and reduced productivity  Fouling phenomenon on the membrane surface and/or in the pores
  • 28. TITILE :Viscosity change in oil/water food emulsions prepared using a membrane emulsification system  Done by: Y. Asano and K. Sotoyama Objective:  Evaluate the viscosity changes in o/w emulsion  Study the physical properties emulsions
  • 29. Materials and methods   Membrane emulsification apparatus  Materials • For the oil phase, corn oil was used. For the water phase, deionized water was used • Emulsifier polyglycerol esters (PGE) • Stabilizer carnageenan
  • 30.  Methodology  Preparation of emulsion  Before emulsification, the MPG tube was pre-soaked in the continuous phase in an ultrasonic bath for 30 min  The dispersion phase was delivered into the MPG tube  The continuous phase circulated in the vessel  The pressure of the dispersion phase was gradually increased
  • 31. Contd…   Dispersion phase was emulsified into the continuous phase by passage through the membrane  Continued until dispersion phase concentration of 10 vol% at the emulsifying temperature of 25⁰C was reached  The dispersion phase volume was calculated by measuring the total weight of the vessel  Average droplet diameter and the droplet distribution were measured using an image analyser system  Viscosity by vibration viscometer
  • 32.
  • 33. Contd…   Assessment of monodispersed emulsion  An index of monodispersion, a coefficient of dispersion (α )  α = Sd/Dp  Smaller the values, the more monodispersed the emulsions (<=.35)
  • 34. Results and discussion   The value of α was 0.203, so it was evident that emulsion was monodispersed  From the micrographs obtained directly after emulsification and 1 month after emulsification there were no differences between these emulsions
  • 35.
  • 36. Contd..   As the droplet size in the emulsion increased with decreasing viscosity
  • 37.  Relation ship between droplet diameter and viscosity
  • 38. CONCLUSION   Membrane emulsification should is a very interesting technique for the food processing industry.  Benefits of membrane emulsion for the food processing industry may arise from low shear properties, especially for the preparation of double emulsions  Another advantage of membrane emulsion is the scale-up ability of membrane devices  Main limitation is fouling phenomenon  And it solved by recent process called premix ME
  • 39. Reference   Abrahamse, A.J., Lierop, R., Sman, R.G.M., Padt, A.and. Boom, R.M., 2002. Analysis of droplet formation and interactions during cross-flow membrane emulsification. J. Membrane Sci. 204: 125–137.  Adler-Nissen, J., Mason, S.L.and. Jacobsen, C., 2004. Apparatus for emulsion production in small scale and under controlled shear conditions. Trans. Inst. Chem. Eng. C 82: 311–319.  Bals, A., Kulozik, U., 2003. The influence of pore size, the foaming temperature and the viscosity of the continuous phase on the properties of foams produced by membrane foaming. J. Membrane Sci. 220,:5–11.  Bals, A. and Kulozik, U., 2003b. Effect of pre-heating on the foaming properties of whey protein isolate using a membrane foaming apparatus. Int. Dairy J. 13: 903–908.  Charcosset, C., Limayem, I.and Fessi, H., 2004. The membrane emulsification process – a review. J. Chem. Technol. Biotechnol. 79: 209–218.  Cheng, C.J., Chu, L.Y., Xie, R., 2006. Preparation of highly monodisperse w/o emulsions with hydrophobicallymodified SPG membranes. J. Coll. Interf. Sci. 300:375–382.  Christov, N.C., Ganchev, D.N., Vassileva, N.D., Denkov, N.D., Danov, K.D.and Kralchevsky, P.A., 2002. Capillary mechanisms in membrane emulsification: oil-in-water emulsions stabilized by Tween 20 and milk proteins. Coll. Surf. A 209:83– 104.mbrane Sci. 278: 344–348.  Dalgleish, D.G., 2006. Food emulsions – their structures and structure-forming properties. Food Hydrocoll. 20: 415–422.  Daufin, G., Escudier, J.P., Carrère, H., Bérot, S., Fillaudeau, L.and Decloux, M., 2001. Recent and emerging applications of membrane processes in the food and dairy industry. Trans. Inst. Chem. Eng. 79: 89–102.  Fuchigami, T.and Toki, M.and Nakanishi, K., 2000. Membrane emulsification using sol–gel derived macroporous silica glass. J. Sol-Gel Sci. Technol. 19: 337–341..

Editor's Notes

  1. Cont phase-other is suspended as small droplets Methods- rotor, mixer, colloid mill, homogenization Most emulsions are unstable Requre large energy and generate shear force Coalscence,creaming, sepration into 2 layer
  2. utilize a strong shearing stress which may result in coalescence of the dispersed phase. polydispersed, droplet size is difficult to control. Not stable .focculatin, creaming,ostwald ripening,
  3. Distinguishing feature Simplicity Lower energy req Need less surfactant Narrow droplet size distribution
  4. Drplet dia incrses with pore size Monodispersed emulsions can be produced if the membrane pore size distribution is sufficiently narrow not come sufficiently close to allow contact with each other, which may lead to coalescence Max 1.5%
  5. Flux decreses wit incrse in interfacial Flux incses with decrese in viscosity
  6. droplet size becomes smaller as the wall shear stress increases and that the influence is greater for small wall shear stress Trans membrane p incrses flux of dispersed phase incrse High p generate liq jet
  7. Spg-narrow pore size distribtn,tubular shape silicon-o/w emulsion-narrow pore,soft,flat
  8. For effective droplet detatchmnt…to provide shear by flowin the cnti phase across In order to ensure a regular droplet detachment from the pore outlets, shear stress is generated at the membrane by recirculating the continuous phase using a pump
  9. low shear forces on the physicochemical and molecular properties of the proteins
  10. The main applications of membranes are the dairy industry (close to 40%, of which over 10% are used for milk protein standardization), followed by beverages (wine, beer, fruit juices, etc. . .) and egg products (2%). Other fields are emerging: fruit and vegetable juices and concentrates, waste streams, co-products (recovery and recycling of blood plasma in abattoirs), and technical fluids (brines, cleaning-in-place solutions)
  11. The dispersion phase volume was calculated by measuring the total weight of the vessel. emulsifying pressure was 1020 kPa higher than the emulsifying critical pressure
  12. Sd, a standard deviation of the droplet diameter Dp, the average droplet diameter of an emulsion