Contents XVII. Preface

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1 V Preface XVII 1 General Introduction Suspensions Latexes Emulsions Suspoemulsions Multiple Emulsions Nanosuspensions Nanoemulsions Microemulsions Pigment and Ink Dispersions Foams 5 References 9 2 Surfactants Used in Formulation of Dispersions General Classification of Surface-Active Agents Anionic Surfactants Carboxylates Sulphates Sulphonates Phosphate-Containing Anionic Surfactants Cationic Surfactants Amphoteric (Zwitterionic) Surfactants Nonionic Surfactants Alcohol Ethoxylates Alkyl Phenol Ethoxylates Fatty Acid Ethoxylates Sorbitan Esters and Their Ethoxylated Derivatives (Spans and Tweens) Ethoxylated Fats and Oils Amine Ethoxylates Amine Oxides 21

2 VI Specialty Surfactants Fluorocarbon and Silicone Surfactants Gemini Surfactants Surfactants Derived from Monosaccharides and Polysaccharides 23 References 24 3 Physical Chemistry of Surfactant Solutions and the Process of Micellisation Thermodynamics of Micellisation Kinetic Aspects Equilibrium Aspects: Thermodynamics of Micellisation Enthalpy and Entropy of Micellisation Driving Force for Micelle Formation Micellisation in Surfactant Mixtures (Mixed Micelles) 40 References 43 4 Dispersants and Polymeric Surfactants Solution Properties of Polymeric Surfactants General Classification of Polymeric Surfactants Polyelectrolytes 53 References 54 5 Adsorption of Surfactants at the Air/Liquid, Liquid/Liquid, and Solid/Liquid Interfaces Introduction Adsorption of Surfactants at the Air/Liquid (A/L) and Liquid/Liquid (L/L) Interfaces The Gibbs Adsorption Isotherm Equation of State Approach The Langmuir, Szyszkowski, and Frumkin Equations Interfacial Tension Measurements The Wilhelmy Plate Method The Pendant Drop Method The Du Nouy s Ring Method The Drop Volume (Weight) Method The Spinning Drop Method Adsorption of Surfactants at the Solid/Liquid (S/L) Interface Adsorption of Ionic Surfactants on Hydrophobic Surfaces Adsorption of Ionic Surfactants on Polar Surfaces Adsorption of Nonionic Surfactants 72 References 74 6 Adsorption of Polymeric Surfactants at the Solid/Liquid Interface Theories of Polymer Adsorption 80

3 VII 6.2 Experimental Techniques for Studying Polymeric Surfactant Adsorption Measurement of the Adsorption Isotherm Measurement of the Fraction of Segments, p Determination of Segment Density Distribution ρ(z) and Adsorbed Layer Thickness δ h Examples of the Adsorption Isotherms of Nonionic Polymeric Surfactants Adsorbed Layer Thickness Results Kinetics of Polymer Adsorption 98 References 98 7 Colloid Stability of Disperse Systems Containing Electrical Double Layers Origin of Charge on Surfaces Surface Ions Isomorphic Substitution Structure of the Electrical Double Layer Diffuse Double layer (Gouy and Chapman) Stern Grahame Model of the Double Layer Distinction between Specific and Nonspecific Adsorbed Ions Electrical Double Layer Repulsion van der Waals Attraction Total Energy of Interaction Deryaguin Landau Verwey Overbeek (DLVO) Theory Flocculation of Suspensions Criteria for Stabilisation of Dispersions with Double Layer Interaction 113 References Stability of Disperse Systems Containing Adsorbed Nonionic Surfactants or Polymers: Steric Stabilisation Introduction Interaction between Particles Containing Adsorbed Nonionic and Polymeric Surfactant Layers (Steric Stabilisation) Mixing Interaction G mix Elastic Interaction G el Total Energy of Interaction Criteria for Effective Steric Stabilisation Flocculation of Sterically Stabilised Dispersions Weak Flocculation Incipient Flocculation Depletion Flocculation 122 References 123

4 VIII 9 Formulation of Solid/Liquid Dispersions (Suspensions) Introduction Preparation of Suspensions Condensation Methods: Nucleation and Growth Dispersion Methods Wetting of Powders by Liquids Structure of the Solid/Liquid Interface and the Electrical Double Layer Electrical Double Layer Repulsion van der Waals Attraction Total Energy of Interaction Criteria for Stabilisation of Suspensions with Double Layer Interaction Electrokinetic Phenomena and the Zeta-Potential Calculation of the Zeta-Potential Measurement of the Zeta-Potential Dispersing Agents for Formulation of Suspensions Adsorption of Surfactants at the Solid/Liquid Interface Steric Stabilisation of Suspensions Flocculation of Sterically Stabilised Suspensions Properties of Concentrated Suspensions Characterisation of Suspensions and Assessment of their Stability Optical Microscopy Electron Microscopy Confocal Laser Scanning Microscopy Scattering Techniques Bulk Properties of Suspensions Rheological Measurements Sedimentation of Suspensions and Prevention of Formation of Dilatant Sediments (Clays) Prevention of Sedimentation and Formation of Dilatant Sediments 156 References Formulation of Liquid/Liquid Dispersions (Emulsions) Introduction Creaming and Sedimentation Flocculation Ostwald Ripening (Disproportionation) Coalescence Phase Inversion Industrial Applications of Emulsions Physical Chemistry of Emulsion Systems The Interface (Gibbs Dividing Line) 164

5 IX Thermodynamics of Emulsion Formation and Breakdown Interaction Energies (Forces) between Emulsion Droplets and Their Combinations van der Waals Attractions Electrostatic Repulsion Steric Repulsion Adsorption of Surfactants at the Liquid/Liquid Interface Mechanism of Emulsification Methods of Emulsification Role of Surfactants in Emulsion Formation Role of Surfactants in Droplet Deformation Selection of Emulsifiers The Hydrophilic Lipophilic Balance (HLB) Concept The Phase Inversion Temperature (PIT) Concept Creaming or Sedimentation of Emulsions Creaming or Sedimentation Rates Very Dilute Emulsions (φ <0.01) Moderately Concentrated Emulsions (0.2 <φ<0.1) Concentrated Emulsions (φ >0.2) Prevention of Creaming or Sedimentation Matching the Density of Oil and Aqueous Phases Reduction of Droplet Size Use of Thickeners Controlled Flocculation Depletion Flocculation Flocculation of Emulsions Mechanism of Emulsion Flocculation Flocculation of Electrostatically Stabilised Emulsions Flocculation of Sterically Stabilised Emulsions General Rules for Reducing (Eliminating) Flocculation Charge-Stabilised Emulsions (e.g., Using Ionic Surfactants) Sterically Stabilised Emulsions Ostwald Ripening Emulsion Coalescence Rate of Coalescence Phase Inversion 200 References Formulation of Suspoemulsions (Mixtures of Suspensions and Emulsions) Introduction Suspoemulsions in Paints Suspoemulsions in Sunscreens and Colour Cosmetics Suspoemulsions in Agrochemicals 219

6 X Model Suspoemulsion of Polystyrene Latex and Isoparaffinic Oil stabilised with Synperonic PE (PEO PPO PEO A-B-A Block Copolymer) Model Systems of Polystyrene Latex with Grafted PEO Chains and Hexadecane Emulsions 227 References Formulation of Multiple Emulsions Introduction Preparation of Multiple Emulsions Types of Multiple Emulsions Breakdown Processes of Multiple Emulsions Factors Affecting Stability of Multiple Emulsions, and Criteria for Their Stabilisation General Description of Polymeric Surfactants Interaction between Oil or Water Droplets Containing an Adsorbed Polymeric Surfactant: Steric Stabilisation Examples of Multiple Emulsions Using Polymeric Surfactants Characterisation of Multiple Emulsions Droplet Size Measurements Rheological Measurements 248 References Preparation of Nanosuspensions Introduction Nucleation and Growth, and Control of Particle Size Distribution Preparation of Nanosuspensions by Bottom-Up Processes Solvent Antisolvent Method Use of a Nanoemulsion Mixing Two Microemulsions Preparation of Polymer Nanoparticles by Miniemulsion or Minisuspension polymerisation Preparation of Nanosuspensions Using the Bottom-Down Process Wetting of the Bulk Powder Breaking of Aggregates and Agglomerates into Individual Units Wet Milling or Comminution Stabilisation of the Resulting Dispersion Prevention of Ostwald Ripening (Crystal Growth) 268 References Formulation of Nanoemulsions Introduction Mechanism of Emulsification 273

7 XI 14.3 Methods of Emulsification and the Role of Surfactants Preparation of Nanoemulsions High-Pressure Homogenisation Phase Inversion Composition (PIC) Principle Phase Inversion Temperature (PIT) Principle Preparation of Nanoemulsions by Dilution of Microemulsions Steric Stabilisation and the Role of the Adsorbed Layer Thickness Ostwald Ripening Practical Examples of Nanoemulsions Nanoemulsions Based on Polymeric Surfactants 293 References Formulation of Microemulsions Introduction Thermodynamic Definition of Microemulsions Mixed-Film and Solubilisation Theories of Microemulsions Mixed-Film Theories Solubilisation Theories Thermodynamic Theory of Microemulsion Formation Reason for Combining Two Surfactants Factors Determining W/O versus O/W Microemulsions Characterisation of Microemulsions Using Scattering Techniques Time-Average (Static) Light Scattering Calculation of Droplet Size from Interfacial Area Dynamic Light Scattering (Photon Correlation Spectroscopy; PCS) Characterisation of Microemulsions Using Conductivity NMR Measurements Formulation of Microemulsions The HLB System Phase Inversion Temperature (PIT) Method The Cohesive Energy Ratio (CER) Concept Cosurfactant Partitioning 322 References 322 Further Reading Formulation of Foams Introduction Foam Preparation Foam Structure Classification of Foam Stability Drainage and Thinning of Foam Films Theories of Foam Stability 330

8 XII Surface Viscosity and Elasticity Theory The Gibbs Marangoni Effect Theory Surface Forces Theory (Disjoining Pressure π) Stabilisation by Micelles (High Surfactant Concentrations > cmc) Stabilisation by Lamellar Liquid Crystalline Phases Stabilisation of Foam Films by Mixed Surfactants Foam Inhibitors Chemical Inhibitors That Lower Viscosity and Increase Drainage Solubilised Chemicals Which Cause Antifoaming Droplets and Oil Lenses Which Cause Antifoaming and Defoaming Surface Tension Gradients (Induced by Antifoamers) Hydrophobic Particles as Antifoamers Mixtures of Hydrophobic Particles and Oils as Antifoamers Physical Properties of Foams Mechanical Properties Rheological Properties Electrical Properties Electrokinetic Properties Optical Properties Experimental Techniques for Studying Foams Studies on Foam Films Structural Parameters of Foams Foam Drainage Foam Collapse 343 References Formulation of Latexes Introduction Emulsion Polymerisation Mechanism of Emulsion Polymerisation Block Copolymers as Stabilisers in Emulsion Polymerisation Graft Copolymers as Stabilisers in Emulsion Polymerisation Polymeric Surfactants for Stabilisation of Preformed Latex Dispersions Dispersion Polymerisation Mechanism of Dispersion Polymerisation Influence of Polymeric Surfactant Concentration and Molecular Weight on Particle Formation Effect of Monomer Solubility and Concentration in the Continuous Phase Stability/Instability of the Resulting Latex Particle Formation in Polar Media 364 References 365

9 XIII 18 Formulation of Pigment and Ink Dispersions Introduction Powder Wetting Effect of Surfactant Adsorption Wetting of Powders by Liquids Measurement of Wettability of Powders Submersion Test: Sinking Time or Immersion Time Measurement of Contact Angles of Liquids and Surfactant Solutions on Powders Wetting Agents for Hydrophobic Pigments Dynamics of Processing of Adsorption and Wetting Experimental Techniques for Studying Adsorption Kinetics Breaking of Aggregates and Agglomerates (Deagglomeration) Classification of Dispersants Surfactants Polymeric Surfactants Polyelectrolytes Assessment and Selection of Dispersants Adsorption Isotherms Measurement of Dispersion and Particle Size Distribution Wet Milling (Comminution) Bead Mills 394 References Methods of Evaluating Formulations after Dilution Introduction Assessment of the Structure of the Solid/Liquid Interface Double Layer Investigation Analytical Determination of Surface Charge Electrokinetic and Zeta-Potential Measurements Measurement of Surfactant and Polymer Adsorption Assessment of Sedimentation of Suspensions Assessment of Flocculation and Ostwald Ripening (Crystal Growth) Optical Microscopy Phase-Contrast Microscopy Differential Interference Contrast (DIC) microscopy Polarised Light Microscopy Sample Preparation for Optical Microscopy Particle Size Measurements Using Optical Microscopy Electron Microscopy Transmission Electron Microscopy Scanning Electron Microscopy Confocal Laser Scanning Microscopy Scanning Probe Microscopy 409

10 XIV Scanning Tunneling Microscopy Atomic Force Microscopy Scattering Techniques Light-Scattering Time-Average Light Scattering Rayleigh Gans Debye Regime (RGD) λ/20 < R < λ Turbidity Measurements Light-Diffraction Techniques Dynamic Light Scattering (DLS): Photon Correlation Spectroscopy (PCS) Back-Scattering Techniques Measurement of Rate of Flocculation Measurement of Incipient Flocculation Measurement of Crystal Growth (Ostwald Ripening) Bulk Properties of Suspensions: Equilibrium Sediment Volume (or Height) and Redispersion 420 References Evaluating Formulations without Dilution: Rheological Techniques Introduction Steady-State Measurements Rheological Models for Analysis of Flow Curves Newtonian Systems Bingham Plastic Systems Pseudoplastic (Shear Thinning) System Dilatant (Shear Thickening) System Herschel Bulkley General Model The Casson Model The Cross Equation Time Effects during Flow: Thixotropy and Negative (or Anti-) Thixotropy Constant Stress (Creep) Measurements Analysis of Creep Curves Viscous Fluid Elastic Solid Viscoelastic Response Viscoelastic Liquid Viscoelastic Solid Creep Procedure Dynamic (Oscillatory) Measurements Analysis of Oscillatory Response for a Viscoelastic System Vector Analysis of the Complex Modulus Dynamic viscosity η Strain Sweep 434

11 XV Frequency Sweep The Cohesive Energy Density E c Application of Rheological Techniques to Assess and Predict the Physical Stability of Suspensions Rheological Techniques to Assess Sedimentation and Syneresis Role of Thickeners Assessment of Flocculation Using Rheological Techniques Strain Sweep Measurements Oscillatory Sweep Measurements 441 References 442 Further Reading Assessment and Prediction of Creaming, Sedimentation, Flocculation, and Coalescence of Formulations Assessment and Prediction of Creaming and Sedimentation Introduction Accelerated Tests and Their Limitations Application of High-Gravity (g) Forces Rheological Techniques for Prediction of Sedimentation or Creaming Separation of Formulation ( Syneresis ) Examples of Correlation of Sedimentation or Creaming with Residual (Zero Shear) Viscosity Model Suspensions of Aqueous Polystyrene Latex Sedimentation in Non-Newtonian Liquids Role of Thickeners Prediction of Emulsion Creaming Creep Measurements for Prediction of Creaming Oscillatory Measurements for Prediction of Creaming Assessment and Prediction of Flocculation Using Rheological Techniques Introduction Wall Slip Steady-State Shear Stress-Shear Rate Measurements Influence of Ostwald Ripening and Coalescence Constant Stress (Creep) Experiments Dynamic (Oscillatory) Measurements Strain Sweep Measurements Oscillatory Sweep Measurements Examples of the Application of Rheology for Assessment and Prediction of Flocculation Flocculation and Restabilisation of Clays Using Cationic Surfactants Flocculation of Sterically Stabilised Dispersions Flocculation of Sterically Stabilised Emulsions 458

12 XVI 21.3 Assessment and Prediction of Emulsion Coalescence Using Rheological Techniques Introduction Rate of Coalescence Rheological Techniques Viscosity Measurements Measurement of Yield Value as a Function of Time Measurement of Storage Modulus G as a Function of Time Correlation between Elastic Modulus and Coalescence Cohesive Energy E c 463 References 463 Index 465

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