Changing the Properties of Natural Fibres by Coating and of Synthetic Fibres by Infiltration

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1 Changing the Properties of Natural Fibres by Coating and of Synthetic Fibres by Infiltration Von der Fakultät für Mathematik, Informatik und Naturwissenschaften der RWTH Aachen University zur Erlangung des akademischen Grades eines Doktors der Naturwissenschaften genehmigte Dissertation vorgelegt von M.Sc. Amina Lotfy Owess Mohamed aus Kairo, Ägypten Berichter: Univ. Prof. Dr. Rer. Nat. Martin Möller Univ. Prof. Dr. rer. nat. Andrij Pich Tag der mündlichen Prüfung: Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfügbar.

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3 Changing the Properties of Natural Fibres by Coating and of Synthetic Fibres by Infiltration From the Faculty of Mathematics, Computer Science and Natural Sciences of the RWTH-Aachen University to obtain the academic degree of Doctor of Natural Science (Dr. rer.nat.) Approved thesis Submitted by M.Sc. Amina Lotfy Owess Mohamed From Cairo, Egypt Berichter: Univ. Prof. Dr. rer. nat. Martin Möller Univ. Prof. Dr. rer. nat. Andrij Pich Tag der mündlichen Prüfung: Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfügbar.

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5 Aachen University of Technology (RWTH) Institute of Technical and Macromolecular Chemistry (DWI/ITMC) GERMANY The undersigned certify that they have read, and recommend to the Aachen University of Technology (RWTH) for acceptance, a thesis entitled: Changing the Properties of Natural Fibres by Coating and of Synthetic Fibres by Infiltration Submitted by Amina Lotfy Owess Mohamed in total fulfilment of the requirements of the degree of Doctor Philosophy of Science Approved by thesis committee: Certified and Approved by (Advisor): Univ. Prof. Dr. rer. nat. Martin Möller Aachen University of Technology (RWTH-Aachen) Institute of Technical and Macromolecular Chemistry (DWI/ITMC) Certified and Approved by (Advisor): Univ. Prof. Dr. rer. nat. Andrij Pich Aachen University of Technology (RWTH-Aachen) Institute of Technical and Macromolecular Chemistry (DWI/ITMC) Accepted by (Further examiner): Univ. Prof. Dr. rer. nat. Bernhard Blümich Aachen University of Technology (RWTH-Aachen) Institute of Technical and Macromolecular Chemistry (ITMC) Accepted by (Chairman): Univ. Prof. Dr. rer. nat. Dieter Enders Aachen University of Technology (RWTH-Aachen) Institute of Organic Chemistry (IOC) Date:

6 Author s Declaration AUTHOR S DECLARATION I hereby declare that I am the sole author of this thesis. All the experiments in this thesis constitute work carried out by the candidate unless otherwise stated. The thesis's tables, figures, bibliography and appendices, and complies with the stipulations set out for the degree of Doctor of Philosophy by the RWTH-Aachen University of Technology (RWTH-Aachen). I further authorize RWTH-Aachen University of Technology (RWTH-Aachen) to reproduce this thesis by photocopying or by other means, in total or in part, at the request of other institutions or individuals for the purpose of scholarly research. Title of Thesis/Dissertation: Changing the Properties of Natural Fibres by Coating and of Synthetic Fibres by Infiltration Signature Author Mohamed, Amina Lotfy Owess DWI/ITMC, RWTH-Aachen University DWI an der RWTH-Aachen University vi

7 Abstract 2011 ABSTRACT The Thesis deals with the development of new concepts for improving the properties of natural and synthetic textile fibres. A natural fibre, cotton, has been chosen as fibrous material. The focus of the modification has been directed towards its handle properties, which usually are improved at the expense of moisture up-take. The silicon based compounds were used for this work. Polylactic acid and polypropylene have been chosen as synthetic fibres whose textile potential is hindered by their poor dyeability and low moisture sorption capacity and which can be modified at spinning stage with suitable additives. The focus here has been directed on using recyclable natural materials as additives for achieving an improved comfort property of the synthetic polymer. Two chemical processes, namely coating and infiltration, were considered for applying functional polymers on the fibre surface and, respectively, for modifying the bulk of a polymer via infiltration of particles into the matrix. The coating of cotton with two hydrophilic silicon softeners, a silanol compound and a PDMS compound, was carried out from water, as a classical method, and from supercritical CO2, respectively, as a new approach. The coating process and the change of the fabric properties were investigated by using Scanning Electron Microscopy (SEM), elemental identification Energy Dispersive X Ray Spectroscopy (EDX), Fourier Transform Infra-Red Spectroscopy (FTIR), X-Ray Photoelectron Spectroscopy (XPS), moisture analyser and Kawabata Evaluation System (KES-FB). The results allowed optimising the route of silicon product application and put into evidence the benefits of the treatment, independently of the fabric structure. The polylactic acid and polypropylene based composites were produced via melt infiltration of powders of chitosan, cotton or keratins into polymer matrix. The prepared powders were characterised using FTIR, NMR, Raman microscopy and amino acid analysis. The distribution of the powders into the matrix was investigated by SEM analysis. The composites show good thermal and mechanical properties demonstrated by Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA) and miniature material tester (MiniMat2000). The ability of absorbing and keeping the moisture was highly improved for all materials, as shown with IGA sorb moisture analyser. Polylactic acid based composites proved also an improved ability for dyeing with reactive and acid dyes at 100 C. Summing up the fibres properties can be controllable improved by selecting the appropriate synthetic polymer structure for coating natural fibres, or the appropriate natural additive for infiltrating the matrix of the synthetic fibre. vii Amina L. Mohamed

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9 Kurzfassung 2011 KURZFASSUNG Die Arbeit beschäftigt sich mit der Entwicklung neuer Konzepte zur Verbesserung der Eigenschaften von natürlichen und synthetischen Textilfasern. Eine natürliche Faser, Baumwolle, wurde als Fasermaterial ausgewählt. Der Schwerpunkt der Modifizierung wurde auf weichmachende Eigenschaften gerichtet, die in der Regel zu Kosten der Feuchtigkeitsaufnahme verbessert werden. Silizium basierende Verbindungen wurden für diese Arbeit verwendet. Als synthetische Fasern wurden Polymilchsäure und Polypropylen ausgewählt, deren textiles Potenzial durch ihre schlechte Färbbarkeit und niedrige Feuchtigkeitssorptionskapazität behindert und die beim Spinnen mit geeigneten Zusätzen modifiziert werden können. Der Schwerpunkt hier lag darin wieder verwertbare natürliche Materialien als Zusätze, zur Erzielung einer verbesserten Komforteigenschaft der synthetischen Polymere zu verwenden. Die Beschichtung der Baumwolle mit zwei hydrophilen Siliziumweichmachern, Silanverbindungen und PDMS Verbindungen wurde aus Wasser durchgeführt, eine klassische Methode, aus organischen Lösungsmitteln und aus überkritischem CO2 als neuer Ansatz. Die Beschichtung und die Veränderung der Gewebeeigenschaften wurden untersucht mit Hilfe von konfokaler Raman Mikroskopie (KRM), Rasterelektronenmikroskopie (REM), Energiedispersiver Röntgenspektroskopie (EDX), Fourier-Transform-Infrarotspektroskopie (FTIR), Röntgenphotoelektronenspektroskopie (XPS), Moisture Analyzer und Kawabata Auswertungs System (KES-FB). Die Ergebnisse ermöglichten die Optimierung der Route der Anwendung von Siliziumprodukten und bewiesen den Nutzen der Behandlung, unabhängig von der Gewebestruktur. Die Polymilchsäure und Polypropylen Komposite wurden durch Schmelzinfiltration von Pulvern aus Chitosan, Baumwolle oder Keratin in eine Polymermatrix hergestellt. Die hergestellten Pulver wurden mittels FTIR, NMR, FT-Raman-Mikroskopie und Aminosäure- Analyse charakterisiert. Die Verteilung des Pulvers in der Matrix wurde durch REM-Analyse untersucht. Die hergestellten Verbundwerkstoffe zeigen gute thermische und mechanische Eigenschaften, wie durch Differential Scanning Kalorimetrie (DSC), Thermogravimetrische Analyse (TGA) und Miniatur-Material-Tester (MiniMat 2000) nachgewiesen wurde. Die Fähigkeit Feuchtigkeit zu absorbieren und zu halten war für alle hergestellten Verbundwerkstoffe bei Raumtemperatur stark verbessert, wie mittels IGA Feuchtigkeitsanalyse gezeigt wurde. Polymilchsäure Komposite zeigten auch eine verbesserte Färbbarkeit mit reaktiven und sauren Farbstoffen bei 100 C. die als die Farbstärke von ix Amina L. Mohamed

10 Kurzfassung gefärbten Folien gemessen unter Verwendung von Daten Farbe Instrument vorgestellt verbessert werden muss. Zusammenfassend können die Fasereigenschaften kontrolliert verbessert werden, durch die Wahl der geeigneten synthetischen Polymerstruktur für die Beschichtung von Naturfasern, oder des geeigneten natürlichen Zusatzstoffes für die Infiltration der Matrix der synthetischen Faser. DWI an der RWTH-Aachen University x

11 2011 The road of life twists and turns and no two directions are ever the same. Yet our lessons come from the journey, not the destination (Don Williams) xi Amina L. Mohamed

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13 Acknowledgments 2011 ACKNOWLEDGMENTS First, I would like to thank God for all his blessings. Any success earned by this research deservedly belongs to almighty "God" Thanks God. It is pleasure to convey my gratitude to the following persons in my humble acknowledgment for their dedication and support. Grateful thanks to my supervisor Prof. Dr. rer. nat. Martin Möller head of the German Wool Research Institute/Institute of Textile Chemistry and Macromolecular Chemistry (DWI/ITMC), RWTH-Aachen University. For give me the opportunity to work under his supervision and for his academic guidance, scientific support, the interesting selection of topics and for giving me a large freedom in the organization of my work. I wish also to express my deep and sincere appreciation to Prof. Dr. Crisan Popescu, at (DWI/ITMC), who gave me his precious time and advice whenever I needed it. He has provided eminently helpful advice on everything from the methodological design to the writing process. His faith in me and his ability to bring me back to track at difficult times through four years have been a Godsend. I would like to thank Dr. Meriem Er-Rafik, at (DWI/ITMC), for her assistance, valuable advice and unfailing guidance thorough the application of silicone compounds and softeners on cotton fabric. I would like to convey my thanks to Dr. Ronlad Wagner, at (Momentive Performance Materials Co., Grermany), for valuable discussion thorough the application of silicone softeners on cotton fabric. I would like to extend my appreciation to Dr. Xiaomin Zhu for his valuable discussion in application of silicon compounds and for giving me the introduction of film extrusion. Thanks to Dr. Rostislav Vinokur for giving me the introduction of using the supercritical carbon dioxide in finishing process Also, I would like to thank all the Co-operation and technical assistance from my fellowcolleagues at (DWI/ITMC) who helped me to make this work possible are gratefully acknowledged. This work is a testimony to their professionalism and technical excellence. Thanks to all the fellow colleagues from lab 2.09, big office, DWI and the ITMC for the collegial environment and their friendship. xiii Amina L. Mohamed

14 Acknowledgments Very special thanks are recorded to, the Egyptian Governments, Egyptian ministry of higher education and scientific research, Missions Department, for giving me the opportunity to pursue my PhD degree in Germany, also, for the financial support. Special thanks to my mother, who took months out of her busy schedules to help me to take care of my children and for her encouragements and for her emotional support. Thank you to my husband Ahmed for sharing with me all the ups and downs of our life, for his support and love, patience and help in each and every part of my existence. Without his presence in my life this thesis would not be exist. Finally, thanks my wonderful Children, the joy of my life and my biggest accomplishment. Without my family s love and support, this work would have never been finished. No words can express my gratitude to them. Amina Mohamed July 2011 DWI an der RWTH-Aachen University xiv

15 Acknowledgments 2011 If you reach the summit, drew your eyes to the slope to see who help you to rise on it Then look at the sky, and thank Allah a lot for establishment of your feet on it. xv Amina L. Mohamed

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17 Dedication 2011 DEDICATION This dissertation is dedicated to God Almighty for his sufficient grace. Special dedication is to my beloved husband, AHMED, for providing helping, encouragement and constant supporting during all these years. Also I would like to dedicate my mother whose prayers & encouragement have been always with me. Dedication also to the soul of my father, I am indebted to him for his support, guidance and encouragement in all my life. Last, but by no means least, I would like to dedicated my beloved children Adam, Areej and Akram xvii Amina L. Mohamed

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19 2011 TABLE OF CONTENTS Author s Declaration...vi Abstract...vii Kurzfassung...ix Acknowledgments...xiii Dedication...xvii Table of Contents...xix List of Tables...xxvii List of Figures...xxx List of Schemes...xxxvi List of Equations...xxxvii List of Abbreviations and Symbols...xxxix A - Symbols Abbreviations...xxxix B - General Abbreviations...xl C - Chemical Abbreviations...xli 1. Introduction Cotton Fibre Distinctive Features Morphology of Cotton Molecular and Supramolecular Features of Cellulose Chemical Structure of Cellulose Physical Structure of Cellulose Crystalline and Amorphous Regions Cellulose Accessibility and Reactivity Chemical Treatments Diffusion into Cotton Fibre Chitosan Wool Fibre Morphology Chemical Composition Polymer Reinforced Composites Functional Chemical Finishing of Natural Polymer Infiltration of Silicone Compounds into Cotton Fibres Infiltration of Cotton and other Materials in the Matrix of Thermoplastic Polymers (Melt Infiltration) Polylactic acid...21 xix Amina L. Mohamed

20 DWI an der RWTH-Aachen University Polypropylene Monitoring the Penetration of Linear PDMS Compounds into Cotton Fibres Introduction Experimental Materials Methods Treatment in Aqueous Solution Treatment in Hexane Media Measurements Confocal Raman Microscopy (CRM) Scanning Electron Microscopy (SEM) Fourier Transform Infra-Red Spectroscopy (FT-IR) Results and Discussions Treatment with Silicon Oil Treatment with PDMS Compounds According to Molecular Weight Treatment with PDMS I (Mwt. = 1500) Treatment with PDMS II (Mwt. = 9600) Treatment with PDMS III (M.wt. = 69000) Studying the Effect of Storing Time on the PDMS Compounds Conclusions Supercritical Carbon Dioxide Assisted Silicon based Finishing of Cellulosic Fabric: a Novel Approach Introduction Experimental Materials Methods Treatment in SC-CO 2 Medium Treatment in Aqueous Solution Measurements Fourier Transform Infra-Red Spectroscopy (FT-IR) Confocal Raman Microscopy (CRM) Energy Dispersive X Ray Spectroscopy (EDX) Moisture Sorption and Desorption Mechanical Measurements Results and Discussion DWI an der RWTH-Aachen University xx

21 Characterisation of the Treated Fabrics Determination of the Silicon Concentration in the Fibre by ATR-FT-IR Distribution of the Silicone through the Cross-Section of the Fibre Study the Effect of Finishing with DMS Compounds on Moisture Regain Study of the Effect of Finishing with DMS Compounds upon the Physico- Mechanical Properties of the Finished Fabrics Bending stiffness properties Tensile properties Shearing properties Compression properties Surface properties Conclusions Improve Finishing Properties of Cotton Fabrics using Reactive Silicone Softeners Introduction Experimental Materials Methods Fabric extraction Preparation of Silicone Microemulsion Preparation of Magnasoft SilQ (Q or QF) containing microemulsions Preparation of aminosilicone TSF 4708 (A or AF) containing microemulsions Evaluation of the Adsorption and Desorption Adsorption kinetics Desorption kinetics and durability of the finishing The Kinetics of Adsorption Calculation of the Diffusion Coefficients Determination of the Adsorption Model Kinetic and Thermodynamic Analysis Measurements X-Ray Photoelectron Spectroscopy (XPS) Colour Measurements Energy Dispersive X Ray Spectroscopy (EDX) Confocal Raman Microscopy (CRM) Fourier Transform Infra-Red Spectroscopy (FT-IR) Fluorescence Microscopy...73 xxi Amina L. Mohamed

22 DWI an der RWTH-Aachen University 4.3. Results and Discussion Physicochemical Study of the Deposition of the siliconquat softener Magnasoft SilQ (QF ) onto Cotton Fibre Adsorption Study Kinetic study Thermodynamic analysis of adsorption process Chemical composition of the surface Effect of treatment time on the amount of adsorbed silicone compound Distribution of the silicone Q on the fabric surface Distribution of the silicone in the cross-section of the fibre Study of the Permanence of Silicone Compound on Cotton Fabric (Desorption Process) Desorption kinetics of QF Desorption of the non-covalently bounded silicone softener (Q) on the surface of cotton fabrics Physicochemical Study of the Adsorption of Aminosilicone Softener (TSF 4708) onto Cotton Fibre Adsorption Study Kinetic study Kinetics and thermodynamic analysis Effect of treatment time on the amount of adsorbed silicone softener compound Distribution of the silicone A on the fabric surface Study the desorption kinetics of (AF) Conclusions Development of Polylactic Acid and Polypropylene based Fibres with Improving Thermal, Mechanical and Dyeing Properties Introduction Polymer Composites from Cellulose based Materials Polymer Composites from Keratien based Materials Polymer Composites from another Natural Polymers Experimental Materials Methods Drying of PLA Granules DWI an der RWTH-Aachen University xxii

23 Chemical Preparation of Used Materials Preparation of N,O-carboxymethylated chitosan (N,O-CMC) Preparation of O-carboxymethylated chitosan (O-CMC) Preparation of α keratose (Keratose) Preparation of soluble keratin (SK) Preparation of N,N -1,4-butanediyl-bis[6-hydroxy-hexanamide(BIS-amide) Preparation of mono-6-hexylenediamino-6-deoxy-β-cd (CDEN) Preparation of Samples Powder Preparation of the PLA or PP Composites Films Dyeing of PLA Composite Films Measurements Differential Scanning Calorimetry (DSC) Thermogravimetric Analysis (TGA) NMR Measurements Colour Measurements Scanning Electron Microscopy (SEM) Fourier Transform Infra-Red Spectroscopy (FT-IR) Tensile Strength Moisture Sorption and Desorption Determination of the Degree of Substitution (DS) Amino Acid Analysis Result and Discussions Characterisation and Investigation of Prepared Materials and Powders Characterization of Cotton Powder Characterization of Chitosan Derivatives Characterization of chitosan derivatives using FT-IR analysis Characterization of chitosan derivatives using NMR analysis Characterization of Wool, Keratose and Soluble Keratin Characterization using raman microscopy Amino acid analysis Characterization of N,N-1,4-butanediyl-bis[6-hydroxy-hexanamide(BISamide) Characterization of Mono-6-hexylenediamino-6-deoxy-β-CD (CDEN) Characterization of the Micro Powders Scanning electron microscopy (SEM) xxiii Amina L. Mohamed

24 DWI an der RWTH-Aachen University Size distribution of produced particles Conclusions Polysaccharide based Materials in Thermoplastic Polylactic acid or Polypropelene Matrixes Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break Elongation at break Breaking Modulus Conclusions Keratin based Materials in Thermoplastic Polylactic acid or Polypropylene Matrixes Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break Elongation at break Breaking Modulus Conclusions Synthetic Materials in Thermoplastic Polylactic acid or Polypropelene Matrixes Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break Elongation at break Breaking Modulus Conclusion Improving the Dyeing Properties of PLA Composites Films DWI an der RWTH-Aachen University xxiv

25 Dyeing Uptake of PLA and its Composites Film with Polysaccharides based Materials Dyeing Uptake of PLA and its Composites Film with Keratinous based Materials Dyeing Uptake of PLA and its Composites Film with Synthetic Materials Conclusions Polypropylene Composites with N-Grafted Chitosan Derivatives with Improving Thermal and Mechanical Properties Introduction Experimental Materials Methods Preparation of the PP/modified chitosan Composite Films Measurements Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Tensile Strength Moisture sorption and desorption Result and Discussions Mono-N-grafted Amphiphilic Chitosan Derivatives into Polypropylene Matrix Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break Elongation at Break Breaking modulus Di-N-grafted Amphiphilic Chitosan Derivatives into Polypropylene Matrix Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break xxv Amina L. Mohamed

26 DWI an der RWTH-Aachen University Elongation at break Breaking modulus Melt Infiltration of tri N-grafted Amphiphilic Chitosan Derivatives into Polypropylene Matrixes Differential Scanning Calorimeter (DSC) Thermogravimetric Analysis (TGA) Scanning Electron Microscopy (SEM) Moisture Measurements Tensile Measurements Force at break Elongation at break Breaking modulus Conclusions Summary Zusammenfassung References Curriculum Vita List of Publications A - Publications Arising from This Thesis B - Other Publications C - Oral Lectures D - Poster DWI an der RWTH-Aachen University xxvi

27 2011 LIST OF TABLES Table 1: Chemical structure of major amino acids in wool keratin...14 Table 2: Chemical structure of silicon compounds...42 Table 3: Characteristic values in KES-F system (139)...45 Table 4: Silicon atomic concentration (atom %) from XPS results of in Knitwear and Terry before and after extraction...71 Table 5: Effect of the temperature on the adsorption of fluorescently labelled silicone (QF) onto Knitwear and Terry fabrics after 600 sec...74 Table 6: Comparison between the parameters of different kinetics models...76 Table 7: Effect of the initial bath concentration of fluorescently labelled silicone (QF) on the adsorption onto Knitwear and Terry fabrics after 600 sec...77 Table 8: Diffusion coefficients of silicone adsorption onto Terry and Knitwear fabrics...79 Table 9: Parameters of adsorption isotherm models of siliconquat (Q) onto Terry and Knitwear fabrics...80 Table 10: Thermodynamic parameters of the adsorption of Q onto both Terry and Knitwear fabrics...81 Table 11: Effect of the temperature on the desorption of fluorescently labelled silicone QF from Knitwear and Terry fabrics after 600 sec...89 Table 12: Effect of the temperature on the adsorption of fluorescently labelled (AF) onto Knitwear and Terry fabrics after 600 sec...94 Table 13: Comparison of the kinetic parameters calculated for different models...95 Table 14: Rate constants and diffusion coefficients of the adsorption of silicone product onto Terry and Knitwear fabrics...97 Table 15: Parameters of the adsorption isotherm models of AF onto Terry and Knitwear fabrics...98 Table 16: Thermodynamic parameters of the adsorption of A onto Terry and Knitwear fabrics99 Table 17: Comparison between the thermodynamic parameters of the adsorption of A and Q onto both Terry and Knitwear fabrics Table 18: Effect of the temperature on the desorption of fluorescently labelled silicone (AF) from Knitwear and Terry fabrics after 600 sec Table 19: Comparison of the desorption parameter of both silicone compounds (QF and AF)110 Table 20: Chemical structure of used dyes xxvii Amina L. Mohamed

28 DWI an der RWTH-Aachen University Table 21: Freezing shaking times for preparation of used additive powders Table 22: Amino acid analysis for keratinous-based materials Table 23: DSC data for PLA, PP and their composites with polysaccharides based materials140 Table 24: TGA data for PLA, PP and their composites with polysaccharides based materials143 Table 25: DSC data for PLA, PP and their composites films with keratinous-based materials151 Table 26: TGA and DTGA data for PLA, PP and their composites with keratinous-based materials Table 27: DSC data for PLA, PP and their composites films with synthetic materials Table 28: TGA and DTGA data for PLA, PP and their composites films with synthetic materials Table 29: Colour strength of PLA and its composites films with polysaccharides based materials Table 30: Colour strength of PLA film and its composites with keratinous-based materials. 171 Table 31: Colour strength of PLA film and its composites with synthetic materials Table 32: Chemical structure of the materials used in grafting onto chitosan Table 33: Chemical structure of mono-n-grafted chitosan Table 34: Chemical structure of di-n-grafted chitosan Table 35: Chemical structure of tri-n-grafted chitos Table 36: DSC data for PP and its composites with Ch/B in different grafting ratios Table 37: DSC data for PP and its composites with Ch/D-OH in different grafting ratios Table 38: DSC data for PP and its composites with Ch/O-OH in different grafting ratios Table 39: DSC data for PP and its composites with Ch/QI_I Table 40: TGA and DTGA data for PP and its composites with Ch/B in different grafting ratios Table 41: TGA and DTGA data for PP and its composites with Ch/D-OH in different grafting ratios Table 42: TGA and DTGA data for PP and its composites with Ch/O-OH in different grafting ratios Table 43: TGA and DTGA data for PP and its composites with Ch/QI_I 25 in different grafting ratios Table 44: DSC data for PP and its composites films with di-n-grafted chitosan in different grafting ratios DWI an der RWTH-Aachen University xxviii

29 2011 Table 45: TGA and DTGA data for PP and its composites with di-n-grafted chitosan in different grafting ratios Table 46: DSC data for PP and its composites films with tri-n-grafted chitosan in different grafting ratios Table 47: TGA and DTGA data for PP and its composites films with tri-n-grafted chitosan in different grafting ratios xxix Amina L. Mohamed

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