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Improved Superabsorbent Polymers Brunei University Improved Superabsorbent Polymers by Hossein Omidian A thesis submitted for the degree of Doctor of Philosophy September 1997 Department of Chemistry Polymer Research Centre of Iran Brunei University P.O. Box 14185/458 . Uxbridge Tehran . Middlesex, UB8 3PH,UK Iran , BEST COpy .. , . AVAILABLE , V,ariable print quality Abstract This work is devoted to the synthesis, characterization and modification of a class of acrylic-based superabsorbent polymers. The techniques of inverse suspension and solution polymerisations were used for synthesis. Each absorbent was mainly characterised by its equilibrium capacity of water absorption and by the rate of absorption. The swelling characteristics of the polymers were evaluated in terms of change in polymerisation variables which include, type and amount of crosslinker, monomer composition, process of polymerisation, temperature, initiator concentration, monomer concentration and particle size of the product. The swelling dependency on salinity was also examined. In some cases, the base polymer was blended with certain polymers in order to upgrade the swelling properties. A swelling model was devised based on a simple viscoelastic model, i. e. Voigt model, to obtain a better understanding of the effect of the above-mentioned variables on the swelling behaviour. Finally, our materials of choice were compared with some commercial analogues and some further comments have been made for continuing the work. Acknowledgments I wish to express my sincere appreciation to Prof. Peter. G. Sammes at chemistry department of the BruneI University who supervised me and offered valuable suggestions and discussions on the subject. I would like to record my gratitude to Dr. S. A. Hashemi for his support as my supervisor in Polymer Research Centre of Iran. Special thanks are due to Dr. I. G. Meldrum for his care to conduct me throughout the project, and for his helpful discussions which broadened my knowledge. I am also deeply indebted to my colleagues in Polymer Research Centre of Iran, specially Mrs. Askari, for their help in instrumental analysis. I also express my thanks to the Polymer Research Centre of Iran and the BruneI University for allowing me to use the facilities in the laboratories. At last but not at least, thanks are due to my family, Mojdeh and Alborz, who supported me by their patience during the years, and also to my friend, Mr. Reza Davari, who for the first time introduced me the superabsorbing polymers. Table of Contents An extended summary of the work 5 Chapter 1: INTRODUCTION ----------------------9 1.1 Definition 9 1.2 Analysis of superabsorbents 10 1.2.1 Absorption capacity 10 1.2.2 Absorption rate 11 1.2.3 Gel strength 11 1.3 Structural design of superabsorbent polymers 11 1.3.1 Polymer structure 11 1.3.2 Functional groups on polymer structure 12 1.3.3 Interaction with solvent 13 1.3.4 Approaches to increase chain expansion in solvent 14 a) Increase in number ofbonds II n ~ 14 b) Increase in bond length II I ". 14 c) Increase affinity to solvent 15 1.4 Crosslinking 15 1.4.1 In bulk 15 1.4.2 Crosslinking at surface 16 1.5 Swelling 17 1.5.1 Non-ionic gels 17 1.5.2 Ionic gels 18 1.6 Synthetic methods 19 1.6.1 Homogenous polymerization 19 1.6.2 Heterophase polymerization 20 1.6.2.1 Emulsion and Inverse-emulsion 21 1.6.2.2 Suspension and Inverse-suspension 21 1.7 Inverse suspension polymerization 22 1.8 Previous studies on hydrophilic polymers 23 1.8.1 Introduction 23 1.8.2 Natural polymers 24 1.8.3 Inorganic polymers 28 1.8.4 Synthetic polymers 28 1.8.4.1 Non-ionic polymers 28 1.8.4.2 Ionic polymers 30 1.8.4.3 Amphoteric polymers 33 1.8.4.4 Hydrophobically-modified polymers 35 1.8.4.5 Rod-like polymers 35 1. 9 Industry status 35 1.9.1 Applications 35 1.9.2 Price and main manufacturers 37 1.10 Aims 37 1.11 References 38 Chapter 2: EXPERThffiNTAL 46 2.1 General procedure for the synthesis of superabsorbent polymers 46 2.1.1 Inverse suspension polymerisation 46 2.1.1.1 Preparation ofthe dispersed phase 46 Lal Monomer solution 46 [kl Initiator solution 46 [c 1 Cross linker solution 46 [dl Neutraliser solution 46 2.1.1.2 Preparation ofthe continuous phase 47 [e 1 Surfactant solution 47 ill Cross linker solution 47 2.1.1.3 Sequence ofaddition 47 2.1.2 Solution polymerisation 47 2.2 Materials 48 2.3 Experiments 49 2.3.1 Inverse suspension polymerisations 49 ., 2.3.1.1 Preliminary trials {Expts. 1-17)-;-___--::---:=-_--:--:-- ________ 49 2.3.1.2 Effect ofthe oil-soluble cross linker concentration (Expts. 18-2]) 53 2.3.1.3 Effect ofthe water-soluble cross linker concentration (Expts. 22-25) 54 2.3.1.4 Effect ofthe comonomer replacement (Expts. 26-29) 54 2.3.2 Solution polymerisation 55 2.3.2.1 Effect ofthe change in the crosslinker concentration (Expts. 30-33) 55 2.3.2.2 Effect ofthe temperature in solution polymerisation (Expts. 34-47) 57 2.3.2.3 Effect ofthe initiator concentration in solution polymerisation (Expts. 48-56) 57 2.3.2.4 DSC studies on the effect oOnitiator concentration (Expts. 57-66) 57 2.3.2.5 DSC studies on the effect oftemperature (Expts. 67-72) 58 2.3.2.6 Change in initiator and neutralizer (Expt. 73) 58 2.3.2.7 Change in monomer concentration (Expt. 74) 58 2.3.2.8 Using PVC emulsion powder (Expts. 75-80) 59 2.4 Determination and characterization of polymers 60 2.4.1 Neutralisation 60 2.4.2 Assaying crosslink density, network chain density and Me 61 2.4.3 Density measurements - 63 2.4.4 Swelling measurements 63 2.4.5 Curve fitting 64 2.4.6 Sol content measurement by spectroscopy (Sec. 3.3, Table. 3.6) 64 2.4.7 Water content (bound water) measurement (Sec. 3.3, Table. 3.6) 65 2.4.8 Gel time measurement 65 2.4.9 Assaying particle size distribution (Sec. 3.6.2, Table. 3.17) 65 2.4.10 Gel content measurement by gravimetry (Sec. 3.4, Tables. 3.7-3.8) 65 2.5 References 66 Chapter 3: RESULTS AND DISCUSSIONS 67 3.1 Introduction 67 3.2 Polymerisations 68 3.2.1 Inverse suspension polymerisation 69 a) Ingredients for the dispersed phase 69 b) Ingredients for the continuous phase 70 c) Ingredients for the interface 70 d) Other provisions 71 3.2.1.1 Preliminary trials (Expts. 1-17) 73 3.2.1.2 Effect ofthe oil-soluble crosslinker concentration (Expts. 18-2]) 84 3.2.1.3 Effect ofthe water-soluble cross linker concentration (Expts. 22-25) 89 3.2.1.4 Effect ofthe comonomer (Expts. 26-29) 95 3.2.2 Solution polymerisation 100 3.2.2.1 Effect ofthe water soluble crosslinker concentration (Expts. 30-33) 101 3.3 A swelling model 103 3.3.1 Introduction 103 3.3.2 Swelling dependency on the crosslinkers 104 3.3.3 Comparing polymers in terms of their swelling characteristics 105 3.3.4 Mathematical relationships between swelling and crosslinker concentration 106 3.3.5 Viscoelastic models 108 3.3.5.1 Voigt model 109 3.3.6 Curve fitting 111 3.3.7 Swelling picture 114 3.3.8 Swelling in terms of expansion 114 3.3.9 Swelling in terms of diffusion 114 3.3.10 Discussion on swelling in terms of model parameters 116 3.3 .11 Increased permeability 11 7 3.3.12 Effect of the local water in the absorbents 118 3.3 .13 Effect of the extractable fractions in the absorbents 119 3.4 Effect of Temperature (Expts. 34-47) and Initiator (Expts. 48-56) 119 3.4.1 Introduction 119 3.4.2 General observations on the reaction 121 3.4.3 Results on water remained in undried product, after gel formation 122 3.4.4 Results on evaporative losses of water and monomer concentration 123 3.4.5 Results on swelling 124 3.4.6 Reaction kinetics 125 3 3.4.7 Discussions on the effects of changes in water content before and after reaction ----128 3.4.8 Discussions on the effect of drying on swelling 130 3.4.9 Application of Voigt model to rates of swelling 13 2 3.5 Monitoring the gel point through DSC studies (Expts. 57-66 and Expts. 67-72) 134 3.5.1 Introduction 134 3.5.2 DSC results (see Sec. 2.3.2.4 for the preparative procedure) 134 3.5.3 Discussion on DSC data 138 3.5.4 DSC data against bench-scale data 139 3.6 Effect of the external parameters 139 3.6.1 Introduction 139 3.6.2 Effect of the particle size 140 3.6.2.1 Dynamic swellings 140 3.6.2.2 Equilibrium swelling 143 3.6.2.3 Mean particle size and particle size distribution 144 3.6.2.4 An explanation for the swelling observations 147 3.6.2.5 Model interpretation 149 3.6.3 Effect of the ionic strength 152 3.6.3.1 Swelling-cross linker relationship in various swelling media 152 3.6.3.2 Swelling-salt relationship at different cross linker concentration 153 3.6.3.3 Expansion factor 154 3.6.3.4 An explanation for the swelling observations 155 3.7 Creating a porous structure 156 3.7.1 Increased monomer concentration 156 3.7.2 Effect of introducing filler (non-etched samples) 158 3.7.2.1 General observations on the reaction 159 3.7.2.2 Swelling observations 160 3.7.3 Effect of etching 160 3.8 Our samples against commercials 162 3.9 Validity of the two parameters model 164 Chapter 4: CONCLUSIONS 172 4.1 Preliminary trials 172 4.2 Crosslinking by ethylene glycol dimethacrylate and methylene bisacrylamide 173 4.3 Inclusion of acrylamide 173 4.4 The swelling model 173 4.5 Temperature and Initiator 175 4.6 DSC studies 176 4.7 Particle size 176 4.8 Ionic strength 177 4.9 Porous structure 177 4.10 Further works 178 4 An extended summary of the work The work presented here explores the effects of a number of variables on the swelling properties of a class of acrylic-based superabsorbent polymers.
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