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Title
DEDICATION
CERTIFICATE
DECLARATION
ACKNOWLEDGEMENT
ABBREVIATIONS
CONTENTS
1. Introduction and Objectives
1.1 Organisation of the Thesis
2. Polymer Metal Complexes: A Retrospective Survey
2.1 Polymer-metal complexes: Synthesis and classification
2.1.1 Pendant complexes
(a) Monodentate pendant complexes
(b) Polydentate pendant complexes
2.1 2 Intro and inter-molecularly bridged complexes
2.1.3 Polymerisation of coordinated monomers
(a) Polymerisation of vinyl compounds containing metal complexes
(b) Polycondensation of metal complexes containing free functional groups
(c) Ring opening polymerisation
2.1.4 Polymers formed by the reaction of peripheral functional groups in metal complexes with polymers
2.1.5 Coordination Polymers
(i) Linear coordinated polymers
(a) Bifunctional ligands
(b) Simple compound or ion as ligands
(ii) Network-coordinated polymers
2.2 Applications of polymer-metal complexes
2.2.1 Natural chelating polymers
2.2.2 Ion selectivity
2.2.3 Catalytic activity
2.2.3.1. Basis of catalytic action
(i) Oxidative addition and reductive elimination
(ii) lnsertion reaction
2.2.3.2 Macromolecular effect on catalytic activities of polymer-metal complexes
a) Porosity and surface area
b) Nature of polymer support and extent of crosslinking
c) Spacer effects
d) Swelling and solvation of the macromolecular matrix
2.2.3.3 Types of reactions catalysed by polymer-anchored catalysts
a) Oxidative reactions
b) Hydrogenation reactions
c) Hydroformylation
d) Hydrosilysation
e) Polymerisation initiation
f) Hydrolysis
3. Synthesis and Characterisation of NNMBA-Cross linked Polyacrylic Acids and their Metal Complexes
3.1 Synthesis of 4-20 mol% NNMBA-cross linked polyacrylic acids
3.2 Preparation of sodium salt of NNMBA-cross linked polyacrylic acids
3.3 Metal ion complexation of NNMBA-cross linked polyacrylic acids
3.4 Influence of pH on metal ion binding
3.5 Swelling studies of 4-20 mol% NNMBA-cross linked polyacrylic acids
3.6 Characterisation of 4-20 mol% NNMBA-cross linked polyacrylic acids and their metal complexes
3.6.1 FT-IR spectra
3.6.2 13C CP-MAS NMR spectra
3.6.3 UV visible spectra
3.6.4 EPR spectra
3.6.5 Thermogravimetric analysis
3.6.6 Scanning electron microscopy
4. Synthesis and Characterisation of Acrylic Acid-N-Vinyl-2-Pyrrolidone Copolymers and their Metal Complexes
4.1 Synthesis of linear and 4 mol% TTEGDMA-, BDDMA- and NNMBA-cross linked acrylic acid-N-vinyl-2-pyrrolidone copolymers
4.1.1 Linear copolymer
4.1.2 TTEGDMA-, BDDMA-, and NNMBA-cross linked copolymers
4.2 Derivatisation of AA-NVP copolymers
4.3 Metal ion complexation of acrylic acid-N-vinyl-2-pyrrolidone copolymers
4.4 Influence of pH on metal ion complexation of AA-NVP copolymers
4.5 Swelling studies of various cross linked acrylic acid-N-vinyl-2-pyrrolidone copolymers
4.6 Characterisation of polymeric ligands and derived polymer-metal complexes
4.6.1 FT-IR spectra
4.6.2 12C CP-MAS NMR spectra
4.6.3 Nitrogen analysis
4.6.4 UV-vis. spectra
4.6.5 EPR spectra
4.6.6 Thermogravimetric analysis
4.6.7 Scanning electron microscopy
5. Catalytic Activity of Acrylic Acid Based Polymer-Metal Complexes in the Hydrolysis of p-Nitrophenyl Acetate
5.1 Catalytic activity of 4-20 mol% NNMBA-cross linked polyacrylic acid metal complexes
5.1.1 Effect of degree of NNMBA cross linking on the catalytic activity of metal complexes 4-20 cool% polyacrylic acids
5.1.2 Kinetics of hydrolysis of p-nitrophenyl acetate catalysed by Co (II) complex of 4 mol% NNMBA-cross linked polyacrylic acid
5.2 Acrylic acid-N- vinyl-2-pyrrolidone copolymer systems
5.2.1 Catalytic activity of linear AA-N VP copolymer-metal complexes
5.2.2 Catalytic activity of 4 mol% TTEGDMA-cross linked AA-NVP copolymer-metal complexes (1 1 system)
5.2.3 Catalytic activity of 4 mol % BDDMA-cross linked AA-NVP copolymer-metal complexes (1: 1 system)
5.2.4 Catalytic activity of NNMBA-cross linked AA-NVP copolymer metal complexes (1: 1 system)
5.2.5 Kinetics of hydrolysis of p-nitrophenyl acetate catalysed by Co (II) complex of 4 mol% TTEGDMA-cross linked AA-NVP copolymer system (1: 1)
5.2.6 Effect of the nature of cross linking agent on the catalytic activity of copolymer metal-complexes in the hydrolysis of p-nitrophenyl acetate
5.3 Effect of various parameters on the catalytic activity of acrylic acid based polymer-metal complexes in the hydrolysis of p-nitrophenyl acetate
5.4 Comparison between cross linked polyacrylic acid system and cross linked AA-NVP copolymer system
5.5 Comparison between linear and cross linked AA-NVP copolymer systems
6. Experimental
6.1 General
6.1.1 Materials
6.1.2 Instrumental
6.2 Synthesis of 4-20 mol % of NNMBA-cross linked polyacrylic acid
6.3 Synthesis of acrylic acid-N-vinyl-2-pyrrolidone copolymers
6.3.1 Linear copolymer
6.3.2 Cross linked copolymers
6.3.2.1 Synthesis of 4 mol% TTEGDMA-cross linked acrylic acid-N-vinyl-2 pyrrolidone copolymers
6.3.2.2 Synthesis of 4 mol% BDDMG4-cross linked acrylic acid-N-vinyl-2 pyrrolidone copolymers
6.3.2.3 Synthesis of 4 mol% NNMBA-cross linked acrylic acid-N-vinyl-2 pyrrolidone copolymers
6.4 Derivatisation of NNMBA-cross linked polyacrylic acids and acrylic acid-N-vinyl-2-pyrrolidone copolymers
6.5 Estimation of carboxyl capacity of polyacrylic acids and AA-NVP copolymers
6.6 Preparation of polymer-metal complexes: General procedure
6.7 Effect of pH on metal ion binding
6.8 Swelling studies
6.9 Recyclability of complexed resins
6.10 Catalytic activity of polymer-metal complexes: General procedure
7. Summary and Outlook
References