rheology and solving emulsion processing problems t...
TRANSCRIPT
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RHEOLOGY AND SOLVING EMULSION PROCESSING
PROBLEMS
T. Joseph Lin, PhD
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IMPORTANCE OF EMULSIONS
• Allow incorporation of many water and oil soluble ingredients
• Many applications for cosmetic products • Inexpensive to make
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MOST IMPORTANT REASON:
Our customers love our emulsions! Why?
They are not only safe and effective, they look nice and feel great! (Thanks to their rheological properties!)
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Dr. Albert Kligman (Cosmeceutical)
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POTENTIAL PROBLEMS
• Emulsions are unstable by nature • The Second Law of Thermodynamics • Difficult to predict and assure stability • Must be careful in formulating the product • Must be careful in processing the product
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HOW TO ASSURE QUALITY?
• Good Formulation: Right amount of right surfactants, stabilizers
… • Correct Manufacturing Procedure: Correct equipment, method …
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TWO IMPORTANT VARIABLES
• Composition Variable: cV • Process Variable: pV • Both affect Rheology and Stability
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THE NATURE OF pV
• Difficult to Anticipate • Tricky to Control (Surprise!) • Can Be Your Enemy or Friend
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MY STORY Beauty Counselors, Detroit, 1959 My Boss: Maison G. deNavarre
(SCC Founding Father)
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MY RHEOLOGY LESSONS
• Brookfield Viscometer • Rheology and Process Problems • Art of Emulsion Manufacturing • Betting on Newtonian Shampoo • What You Put in the Product (cV) • How You Put Them Together (pV)
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FINDING THE RIGHT BALANCE
• “More” is not always better • Sometimes, “Less Is More”
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IMPORTANCE OF Zp
• Zp is the optimum point • Finding Zp is not always easy • But it will help solve many
problems • And reducing cost
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HOW TO FIND Zp?
• Understand the basic principles • Experiments • Patience
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FORMULATION
Since rheological properties can affect the product’s stability, efficacy, skin feel and appearance, control of composition variables (cV) is very important in formulation work.
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EXAMPLE OF LESS IS MORE
• Sometimes, we can actually improve the stability of an emulsion by reducing the amount of certain surfactant in the formula.
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MANUFACTURING
Controlling process variables, pVs, is also very important since process equipment can affect rheological properties and degrade the quality of emulsion products.
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THE POWER OF pV
• pVs can affect rheology and drive us crazy
• But pVs can be a powerful tool • We need more research on pVs.
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EXAMPLE: LOW-ENERGY EMULSIFICATION (LEE)
• A simple way to reduce energy use in making emulsions
• No need to change formula • No need to buy new equipment (PPE) • Reduce processing time • Save money while reducing carbon footprint
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LOW-ENERGY EMULSIFICATION (LEE)
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SOLVING A RHEOLOGICAL PROBLEM WITH LEE
Case Study: • My first crisis at Max Factor • A shear-sensitive, thixotropic moisturizer • No problem making 200-gal batch • Low viscosity when making 500-gal batch • Reason: shear-thinning effect of the mixer • Fixed speed mixer, could not reduce speed
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SOLUTION: MODIFIED LEE
• Even if we could reduce mixer speed, cooling time would increase and mixing time would be longer
• Tried a modified LEE procedure to promote faster cooling. It reduced cooling time and shear-thinning effect. The product passed QC.
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ANOTHER EXAMPLE USING LEE TO SOLVE RHEOLOGICAL PROBLEM
Case Study: • Product: Spray-type Sunscreen • Problem: Scale-up • Lab Batch, Pilot Batch : No Problem • 2000-Gallon Production Batch: High
Viscosity • Difficult to Spray, Large Droplets, Unstable !
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INVESTIGATION OF THE CAUSE
• Why does batch size matter? • Slow cooling for large batch • PIT (phase inversion temperature) effect? • Very low surface tension at PIT, producing very
fine, low-viscosity emulsion • Slow cooling promoted coalescence of
droplets to produce high-viscosity emulsion?
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QUESTION?
How fast should it cool ANSWER:
Find out by experiments!
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DISCOVERING THE Z-POINT
Critical Cooling Rate: ~ 1.6 °C/min Safe Cooling Rate: Above 2°C/min
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SOLUTIONS
• LEE • Heat Exchanger
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AIR BUBBLES CONTROL
• Many cosmetics emulsions are shear-thinning type and can trap air bubbles during mixing or transferring. If the product has yield value, the trapped air may not escape, causing an uneven surface appearance.
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Z-POINT FOR PREVENTING AIR BUBBLE ENTRAINMENT
We = 10 (Re)0.74
We = Weber Number = DV2ρ / ϒ Re = Reynolds Number = DVρ / η T J Lin and H G Donnelly, A I Ch E Journal, 12, 563 (May 1966)
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CONCLUSIONS
• Emulsion products are very important. • They can be difficult to formulate and
manufacture. • Understanding of rheology and process
variables (pV) can be very useful in solving formulation and manufacturing problems.
• It will help us finding Z-Points and reducing carbon footprint in manufacturing!
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REFERENCES
• T. J. Lin, “Rheology Fundamentals and Applications in Cosmetic Formulation, Manufacturing and Quality Control” in The Chemistry and Manufacture of Cosmetics, Vol. 1 Basic Science, M. L. Schlossman, editor, Allured Publishing Corp., Carol Stream, IL, (2000)
• T. J. Lin, “Manufacturing Cosmetic Emulsions: Pragmatic Trouble Shooting and Energy Conservation” Allured Books, Carol Stream, IL 60188 (2010)
• T. J. Lin, “Reducing Carbon Footprint in Manufacturing Personal Care Products” in Sustainable Cosmetic
Product Development, Wen Schdoeder, editor, Allured Books, Carol Stream,. IL 60188 (2011) • T. J. Lin and J. C. Lambrechts, “Effect of Initial Surfactant Location of Emulsion Phase Inversion” J. Soc.
Cosmetic Chemists 19, 683. (September 1968) • T. J. Lin, “Mechanisms and Control of Gas Bubbles Formation in Cosmetics” J. Soc. Cosmetic Chemists
22, 323, (May, 1971) • T. J. Lin, T. Akabori, S. Tanaka and K. Shimura, “Low Energy Emulsification, V. Mechanism of Enhance
Emulsification” Cosmetic and Toiletries 98, 67 (October, 1983) • T. J. Lin, “Adverse Effects of Excess Surfactants in Emulsification” Cosmetics and Toiletries 106, 71 (May
1991) • T. J. Lin, “Low-Surfactant Emulsification: Optimizing Formulas and Conserving Resources,” Cosmetics
and Toiletries, 34, (August, 2010) • T. J. Lin and H. G. Donnelly, “Gas Bubble Entrainment by Plunging Laminar Liquid Jets” A.I.Ch.E.
Journal 12, 563, (May 1966)