MODIFICATION OF SURFACE PROPERTIES OF BIOPOWDERS BY DRY PARTICLE COATING

Elisabeth Dumoulin

Description

Niveau: Supérieur, Doctorat, Bac+8
THÈSE En vue de l'obtention du DOCTORAT DE L'UNIVERSITÉ DE TOULOUSE Délivré par Institut National Polytechnique de Toulouse Discipline ou spécialité : Génie des procédés JURY Mme. Elisabeth DUMOULIN Rapporteur M. Pierre GUIGON Rapporteur M. Denis PONCELET Examinateur M. Gérard THOMAS Examinateur M. John A. DODDS Directeur de thèse M. Olivier LECOQ Co directeur de thèse Ecole doctorale : Mécanique, Energétique, Génie civil et Procédés Unité de recherche : RAPSODEE (centre de Recherches d'Albi en génie des Procédés, des Solides Divisés, de l'Energie et de l'Environnement), UMR EMAC-CNRS 2392, École des Mines d'Albi Directeur(s) de Thèse : John A. DODDS et Olivier LECOQ Présentée et soutenue par M. Serkan OTLES Le 11 Décembre 2008 Titre : MODIFICATION OF SURFACE PROPERTIES OF BIOPOWDERS BY DRY PARTICLE COATING

• phd study


• génie des procédés, des solides divisés, de l'energie et de l'environnement


• directeur


• also scientific

Sujets

• Catherine Guigon
• Institut national polytechnique de Toulouse
• Thomas
• Serkan
• Université de technologie de Compiègne
• Poncelet
• Université de Toulouse
• École des Mines
• Dumoulin

Informations

• Publié par: profil-zyak-2012
• Publié le: 01 décembre 2008
• Nombre de lectures: 66
• Langue: Français
• Poids de l'ouvrage: 7 Mo

Extrait

THÈSE

En v u e d e l' ob t e n t ion d u

DOCTORATD EL’UNIV ERSITÉD ETOU LOUSE

D é liv r é p a rde ToulouseI nst it ut Poly t echnique Nat ional D iscip lin e ou sp é cia lit é :océdésGénie des pr

Pr é se n t é e e t sou t e n u e p a rk an OTLESM. Ser Le11 Décem br e 2 00 8

Tit r e :MODI FI CATI ON ES OF BI OF SURFACE PROPERTI CLEOPOWDERS BY DRY PARTI COATI NG

JU RY Mm e. Elisabet h DUMOULI N Rappor t eur M. Pier r e GUI GON Rappor t eur M. Denis PONCELET Ex am inat eur M. Gér ar d THOMAS Ex am inat eur M. John A. DODDS Dir ect eur de t hèse M. Oliv ier LECOQ Co dir ect eur de t hèse

Ecole d oct or a le :il et Pr Génie civ océdésgét ique, Mécanique, Ener U n it é d e r e ch e r ch e :de Recher ches d' Albi en génie des Pr océdés,RAPSODEE ( cent r e  des Solides Div isés, de l'Ener gie et de l'Env ir onnem ent ) ,  UMR EMAC- CNRS 2 3 9 2 , École des Mines d'Albi D ir e ct e u r ( s) d e Th è se :ier LECOQJohn A. DODDS et Oliv

Our true mentor in life is thescience

Acknowledgement I would like to express my sincere appreciation to my advisor, Prof. Dr. John A. Dodds, for his insight, encouragement and support throughout my doctoral study. Without his guidance and motivation, this research would not have been accomplished. I am grateful to Dr. Olivier Lecoq, my co–advisor, for the help and inspiration he has brought to this work. I would also like to thank Dr. Alain Chamayou and Dr. Laurence Galet for offering valuable advices. I would like to thank you Prof. Jacques Fages, Director of the RAPSODEE research centre, for his welcome to the laboratory. I am grateful to Prof. Dr. Elisabeth Dumoulin from Institut des Sciences et Industrie du Vivant et de l’Environnement (AgroParisTech), Prof. Dr. Pierre Guigon from Université de Technologie de Compiègne and Prof. Dr. Gérard Thomas from Ecole des Mines de St. Etienne for their participation to my PhD defence as the jury members. Special thanks go to our technicians Sylvie, Séverine, Laurent, Philippe and Christine in Albi and Anne Marie in St. Etienne and our secretary Anne Marie for their help, motivation and trust on me during this research. I would like to thank you my colleagues Mokrane, Chawki, Leslie, Brice and all PhD students whom I shared unforgettable 3 years for their support during my PhD study. And specially, my dear friend Yamina for her support, friendship, motivation and also scientific advices, thank you very much Yamina. I can not forget also my colleagues whom I spent just couple of weeks in St. Etienne but I got friends for life time. And of course Marie-France, my french teacher, who allowed me to express myself with a language that I have never used in my life and helped me to adapt myself to this lovely country and people. I am also grateful to two very special people, first of all, Nadia, without your support I wouldn’t be able to write these sentences, thank you very much for being next to me all the time. And Abdellah of course, thanks a lot for everything you did. I would like to express my endless gratitude to my parents, Salih and Oya, my sister Yesim and all of my family who have always helped me in everyway possible. And all of my friends, especially to Cem Cakiroglu and Emre Batir for their support and motivation. Last, but certainly not least, I want to thank you to the person who is my inspiration source, lighthouse in the academic ocean and always holds my hand to show the way, my uncle Prof. Dr. Semih Otles. Thank you Amca for everything, this is your achievement.

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TABLE OF CONTENTS Introduction Chapter I. Background on Dry Particle Coating 1.Introduction 2.Advantages of dry coating 3.Origin of dry coating 3.1.Ordered Mixture 3.2.Dry Coating Mechanism 4.Inter-particular Forces 4.1.Van der Waals Forces 4.2.Capillary Force 4.3.Electrostatic Force

5.Dry Particle Coating Equipments 5.1.Mechanofusion 5.2.Nara Hybridizer 5.3.Hosokawa Cyclomix 5.4.Magnetically Assisted Impaction Coater 5.5.Theta Composer 5.6.V–Blender 5.7.Rotating Fluidizer Bed Coater 6.Applications on Dry Coating 7.Conclusion Chapter II. Materials and Methods 1.Introduction 2.Dry Particle Coating Equipments 2.1.Nara Hybridizer 2.2.Hosokawa Cyclomix 2.3.Turbula Mixer 3.Characterization Methods 3.1.Environmental Scanning Electron Microscopy

4.4.Dependency of Inter-particular Forces on Different Parameters

Table of Contents

 Page  9  15  17  18  18  18  20  24  24  26  27  28  32  32  33  36  38  40  41  42  43  45  47  49  49  49  51  52  53  55

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3.2.Atomic Force Microscopy a)Tapping Mode b)Contact Mode c)Non – Contact Mode 3.3.Laser Diffraction Granulometer 3.4.Helium Pycnometer 3.5.Tapped Density Tester 3.6.Freeman Technology Powder Rheometer 3.7.Contact Angle Measurement 3.8.Dynamic Vapour Sorption 4.Materials 4.1.Poly(methyl methacrylate) 4.2.Cellets 4.3.Talc 5.Conclusion Chapter III. Effect of Equipment and Operating Conditions on the End-Use

 56  57  59  61  62  64  64  66  68  68  69  70  72  73  75  Properties of Composite Particles 77  79  80  80  81  82 2.2.2.Effect of Rotational Velocity on the Particle Size Distributions 82  84  86  87  87  89  90  91  96  102

1.Introduction 2.Dry Coating of Particles in Hybridizer 2.1.Hydrodynamic Properties of Hybridizer 2.2.Preliminary Study of Poly(methyl methacrylate) Particles 2.2.1.General Mass Balance

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2.3.Preliminary Study of Talc Particles 2.4.Dry Coating of Poly(methyl methacrylate) with Talc 2.4.1.General Mass Balance 2.4.2.Measurement of Solid Densities of the Dry Coated Particles 2.4.3.Characterization of Surface Morphology of the Particles 2.4.4.Characterization of Particles by Atomic Force Microscopy A) Topographical Analysis of the Particles B) Phase Contrast Analysis of the Particles C) Measurement of Adhesion Forces Between the Particles

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2.4.5.Calculation of Talc Particle Deposition on the Surface of the Coated  Particles 110 2.4.6.Characterization of Coating Strength of the Particles 112 A)Effect of Operating Velocity on the Coating Strength of the Particles 113 B)Effect of Mass Percentage of Talc on the Coating Strength of the Particles 116 C)118Effect of Equipment on Coating Strength of the Particles 2.4.7.120Characterization of the Flowability Properties of the Particle A)Effect of Operating Velocity on the Flowability Properties of the Particles 120 B)Effect of Mass Percentage of Talc on the Flowability Properties of the Particles 122 C)Effect of Equipment on the Flowability Properties of the Particles 125 2.5.Conclusion 126 3.130Dry Coating of Particles in Cyclomix 3.1.Preliminary Study of Poly(methyl methacrylate) Particles 130 3.1.1.131General Mass Balance 3.1.2.Effect of Rotational Velocity on Particle Size Distributions 131 3.2.133Dry Coating of Poly(methyl methacrylate) with Talc 3.2.1.133General Mass Balance 3.2.2.134Measurement of Solid Densities of the Dry Coated Particles 3.2.3.Characterization of Surface Morphology of the Particles 135 3.2.4.136Characterization of Coating Strength of the Particles A)136Effect of Operating Velocity on Coating Strength of the Particles B)Effect of Mass Percentage of Talc on Coating Strength of the  Particles 138 C)140Effect of Equipment on Coating Strength of the Particles 3.2.5.141Characterization of Flowability Properties of the Particle A)Effect of Operating Velocity on Flowability Properties of the Particles 141 B)Effect of Mass Percentage of Talc on Flowability Properties of the Particles 144

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C)Effect of Equipment on Flowability Properties of the Particles 145 3.3.Conclusions 146 4.148Dry Coating of Particles in Turbula 4.1.Preliminary Study of Poly(methyl methacrylate) Particles 148 4.2.Dry Coating of Poly(methyl methacrylate) with Talc 149 4.2.1.150Measurement of Solid Densities of the Dry Coated Particles 4.2.2.150Characterization of Surface Morphology of the Particles 4.2.3.151Characterization of Coating Strength of the Particles A)Effect of Mass Percentage of Talc on Coating Strength of the  Particles 151 B)Effect of Equipment on Coating Strength of the Particles 153 4.2.4.Characterization of Flowability Properties of the Particles 154 A)Effect of Mass Percentage of Talc on Flowability Properties of the  Particles 154 B)Effect of Equipment on Flowability Properties of the Particles 157 4.3.Conclusions 157 5.Conclusions 159 5.1.159Visual Analysis of The Dry Coated Particles in Different Equipments 5.2.Coating Strength of The Dry Coated Particles in Different Equipments 160 5.3.Modification of Flowability Properties of Dry Coated Particles in  Different Equipments 161 Chapter IV. Effect of Particle Size on the End–Use Properties of Composite  Particles 163 1.Introduction 165 2.Effect of Host Particle Size on the End – Use Properties of the Dry Coated  Particles 166 2.1.166Preliminary Study of Cellets 90 and Cellets 200 Particles 2.1.1.167General Mass Balance 2.1.2.Effect of Rotational Velocity on Particle Size Distributions 168 2.2.168Dry Coating of Cellets 90 and Cellets 200 with Talc 2.2.1.174Characterization of Surface Morphology of the Particles 2.2.2.Characterization of Particles by Atomic Force Microscopy 176

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A) Topographical Analysis of the Particles 177 B) Phase Contrast Analysis of the Particles 182 C) Measurement of Adhesion Forces Between the Particles 186 2.2.3.Calculation of Talc Particle Deposition on the Surface of the Coated Particles 189 2.2.4.Calculation of Van der Waals Forces Between the Particles 191 2.2.5.Characterization of Coating Strength of the Particles 192 A)192Particles in Hybridizer Trials B)Particles in Cyclomix Trials 195 C)198Particles in Turbula Trials D)Particles in Basic Mixing Trials 201 2.2.6.Characterizations of the Hydrophilic Properties of The Particles 205 A)206Characterization of the Wettability of the Particles B)207Characterization of Water Affinity of the Particles 2.3.Conclusions 210 3.Effect of Guest Particle Size on the End – Use Properties of the Dry Coated  Particles 213 3.1.Dry Coating of Cellets 200 Particles with Talc and Talc 16000 213 3.1.1.Characterization of Surface Morphology of the Particles 214 3.1.2.Characterization of Coating Strength of the Particle 216 A)217Particles in Hybridizer Trials B)218Particles in Cyclomix Trials C)Particles in Turbula Trials 220 D)Particles in Basic Mixing Trials 222 3.2.Conclusions 225 4.Conclusions 226 Conclusion & Perspectives 229 Appendices 239 References 277

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