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Felipe N. Linhares
Development of Biodiesel-Resistant Nitrile Rubber Compositions
Introduction
28
1 Literature Review
31
1.1 Biodiesel: an alternative to fossil fuels
31
1.1.1 Overview on biodiesel
31
1.1.2 Biodiesel synthesis and possible feedstock
33
1.1.3 Physicochemical properties and oxidation stability
35
1.2 Compression-ignition engines
38
1.2.1 The compression-ignition engine and its composing materials
38
1.2.2 Compatibility of biodiesel with some compression-ignition engine parts
38
1.3 Compatibility of biodiesel with elastomers
39
1.4 Nitrile rubber
44
1.4.1 Main properties
44
1.4.2 Curing systems
45
1.4.3 Vulcanisation kinetics
51
1.4.4 Degradation process
53
2 Aims
56
2.1 General aims
56
2.2 Specific aims
56
3 Materials and Equipment
57
3.1 Part I – Preliminary studies: The influence of acrylonitrile content and different types of crosslink networks
57
3.1.1 Materials
57
3.1.2 Equipment
57
3.2 Part II – Formulation development: The influence of binary sulphur-based curing systems
58
3.2.1 Materials
58
3.2.2 Equipment
58
4 Methods
60
4.1 Part I – Preliminary studies: The influence of acrylonitrile content and different types of crosslink networks
60
4.1.1 Compounding
60
4.1.2 Vulcanisation
61
4.1.3 Vulcanisation kinetic
61
4.1.4 Crosslink density
61
4.1.5 Immersion tests
62
4.1.6 Change in mass
62
4.1.7 Mechanical tests
63
4.1.7.1 Strain-stress
63
4.1.7.2 Tear strength
63
4.1.7.3 Hardness
63
4.1.8 Scanning Electron Microscopy (SEM)
63
4.2 Part II – Formulation development: The influence of binary sulphur-based curing systems
64
4.2.1 Compounding
64
4.2.2 Vulcanisation
65
4.2.3 Crosslink density
65
4.2.4 Ageing tests
66
4.2.4.1 Ageing in air
66
4.2.4.2 Ageing in biodiesel
66
4.2.5 Gravimetric tests
66
4.2.6 Stress-strain
67
4.2.7 Hardness
67
4.2.8 Differential scanning calorimetry (DSC)
67
4.2.9 Dynamic mechanical thermal analysis (DMTA)
67
4.2.10 Scanning electron microscopy (SEM)
68
4.2.11 Confocal Laser Scanning Microscopy (CLSM)
68
4.2.12 Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy
68
4.2.13 Nuclear magnetic resonance (NMR)
68
4.2.14 Statistical analyses
69
4.3 Experimental scheme
70
4.3.1 Part I – Preliminary studies: The influence of acrylonitrile content and differenttypes of crosslink networks
70
4.3.2 Part II – Formulation development: The influence of binary sulphur-based curingsystems
71
5 Results and Discussion
72
5.1 Part I – Preliminary studies: The influence of acrylonitrile content and different types of crosslink networks
72
5.1.1 Characterisation of the compositions
72
5.1.1.1 Vulcanisation kinetics
72
5.1.1.2 Crosslink density
74
5.1.2 Ageing tests
75
5.1.2.1 Gravimetric tests
75
5.1.2.2 Physical mechanical resistance
77
5.1.2.3 Scanning Electron Microscopy (SEM)
81
5.1.3 Overall performance
83
5.2 Part II – Formulation development: The influence of binary sulphur-based curing systems
84
5.2.1 Characterisation of the compositions
84
5.2.1.1 Crosslink density and differential scanning calorimetry (DSC)
84
5.2.1.2 Mechanical properties
86
5.2.1.3 Dynamic mechanical thermal analysis (DMTA)
90
5.2.1.4 Scanning electron microscopy (SEM)
91
5.2.1.5 Confocal Laser Scanning Microscopy (CLSM)
95
5.2.1.6 Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy
96
5.2.1.7 Nuclear magnetic resonance (NMR)
97
5.2.2 Ageing tests
98
5.2.2.1 Gravimetric tests
98
5.2.2.2 Differential scanning calorimetry (DSC)
101
5.2.2.3 Strain-stress
103
5.2.2.4 Hardness
109
5.2.2.5 Confocal Laser Scanning Microscopy (CLSM)
110
5.2.2.6 Scanning electron microscopy (SEM)
111
Conclusions
114
Suggestions for Future Work
117
References
118
Appendix A
131
Appendix B
132
Appendix C
133
Appendix D
135
Appendix E
139
Annexe A
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