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TITLE
DEDICATION
CERTIFICATE
DECLARATION
ACKNOWLEDGEMENT
PREFACE
ABBREVIATIONS
CONTENTS
1. INTRODUCTION
1.1. Synthesis of different types of epoxy resins
1.1.1. Epoxidation using epichlorohydrain
1.1.2. Epoxidation of olefins
1.2. Cure reaction and curatives of epoxy resins
1.3. Modified epoxy resins
1.3.1. Epoxy resins modified with reactive rubbers
1.3.2. Epoxy resins modified with siloxanes
1.3.3. Epoxy resins modified with thermoplastics
1.4. Epoxy-imide resins
1.4.1. Epoxy-imide resins from conventional epoxy resins and imide group containing curatives
1.4.2. Epoxy-imide resins obtained by the modification of backbone epoxy resin with imide groups
1.4.3. Epoxy-imide resins obtained by blendingepoxy resins with polyimides
1.5. End-uses of modified epoxy resins
1.6. Objective and scope of the present investigation
2. EXPERIMENTAL
2.1. Materials
2.1.1. Solvents
2.1.2. Aminoacids / diamines
2.1.3. Other reagents and materials
2.1.4. Anhydrides
2.1.5. Epoxy resins
2.2. Synthesis of imide-diacids
2.3. Synthesis of diimicle-diacids
2.3.1. From aromatic diamines
2.3.2. From aliphatic diamines
2.3.3. From siloxane linkages containing diamine
2.4. Synthesis of monoitaconamic acid
2.5. Synthesis of maleimidobenzoic acids
2.6. Pre-reaction of epoxy resins with CTBN-L or CTBN-S
2.7. Synthesis of siloxane-imide- epoxy resin
2.8. Pre-reaction of siloxane-imide-epoxy resins
2.9. Preparation of epoxy-imide polymers
2.10. Characterization
2.10.1. IR spectral studies
2.10.2. NMR spectral studies
2.10.3. Elemental analysis
2.10.4. Chemical analysis
2.10.4.1 Determination of epoxy value
2.10.4.2 Determination of acid value
2.10.4.3 Determination of hydroxyl value
2.10.5 Determination of molecular weights
2.10.6 Thermal analysis
2.10.6.1 Differential scanning calorimetry
2.10.6.2 Therrnogravimetric analysis
2.10.7 X-ray clifferaction studies
2.10.8 Morphological Studies
2.11. Evaluation of adhesive properties
2.11.1. Surface preparation of stainless steel coupons
2.11.2. Evaluation of lap shear strength (LSS) of bonded coupons
2.12. Evaluation of epoxy-imides as matrix resins for composites. 2.12.1. Preparation of unidirectional composites
2.12.1 Preparation of unidirectional (U.D.) composites
2.12.2. Testing of unidirectional composites
2.13. Evaluation of siloxane containing epoxy-imide polymers as atomic oxygen resistant coatings
2.13.1. Preparation of coatings
2.13.2 Exposure of uncoated and coated samples to atomicoxygen
2.13.3. Surface analysis
3. RESULTS AND DISCUSSION
3.1. Epoxy-imide resins obtained from imide-diacids
3.1.1. Background
3.1.2. Synthesis of epoxidized hydroxyl terminated polybutadiene (EHTPB)
3.1.3. Synthesis and characterization of imide-diacids
3.1.4. Synthesis and characterization of epoxy-imide resins from GY 250 / EPN 1138 / EHTPB and imide-diacids
3.1.5. Thermal properties of epoxy-imide resins
3.1.6. X-ray diffraction studies of epoxy-imide resins
3.1.7. Adhesive strength of epoxy-imide resins
3.1.7.1 Adhesive lap shear strength of GY 250-IDA-[/IDA-11systems
3.1.7.2 Adhesive lap shear strength of EPN 1138-IDA-I/IDA-11systems
3.1.7.3 Adhesive lap shear strength of EHTPB-IDA-YIDA-I1systems
3.1.7.4. Comparative evaluation of adhesive strength of epoxy-irnideresins obtained from GY 250, EPN 1138 and EHTPB
3.1.8. Effect of carboxyl to epoxy equivalent ratio on adhesive lap shear strength and thermal property of epoxy-imide resins
3.1.8.1. Thermal stability of epoxy-imide resins obtained usingdifferent carboxyl eqv to epoxy eqv ratios
3.1.8.2. Adhesive lap shear strength of GY 250-IDA-UIDA-I1systems
3.1.8.3 Adhesive lap shear strength of EPN 1138-IDA-MDA-I1systems
3.1.8.4 Adhesive lap shear strength of EHTPB-IDA-YIDA-I1systems
3.1.8.5 Comparative evaluation of adhesive strength of epoxyimideresins obtained from GY 250-IEPN 1138-IEHTPBIDA-I/IDA-I1 for varying carboxyl eqv to epoxy eqv ratio.
3.1.9. Conclusions
3.2. Epoxy-imide resins obtained from diimide-diacids
3.2.1. Background
3.2.2. Synthesis of 2, 2-bis[4- (4-trimellitimidophenoxy) phenyl] propane (DIDA-V)
3.2.3. Synthesis and characterization of epoxy-imide resins from GY 250 / EPN 1138 and diimide-diacid (DIDA-V)
3.2.4. Thermal properties of epoxy-imide resins (GY 250 / EPN 1138-DIDA-V)
3.2.5. Adhesive lap shear strength of GY 250-DIDA-V and EPN 1138-DIDA-V systems
3.2.6. Epoxy-imides obtained from EHTPB and DIDA-V
3.2.7. Glass fibre reinforced unidirectional composites obtained from GY 250-/ EPN 1138-DIDA-V systems
3.2.8. Comparison of adhesive and thermal properties of DIDA-V based epoxy-imides with that of IDA-based epoxy-imides
3.2.9. Comparison of adhesive and thermal properties of epoxy-imide resins based on DIDA-V with other epoxy-imide resins obtained from different aromatic and aliphatic diamines
3.2.10. Thermal stability of GY 250-/ EPN 1138-DIDA systems
3.2.11. Conclusions
3.3. Epoxy-imide resins modified with reactive liquid rubbers
3.3.1. Background
3.3.2. Epoxy-imide resins modified with EHTPB
3.3.2.1 Effect of addition of EHTPB on the adhesive strength of GY250-IEPN 1138-IDA-UIDA-I1 systems
3.3.2.2 Thermal stability of EHTPB-modified epoxy-imide systems
3.3.2.3 Morphological studies of the EHTPB-modified epoxy-imidesystems
Fig. 3.3.9. SEM of GY 250-IDA4 system (unrnod1jie4
Fig. 3.3.10 SEM of EPN f 138-IDA4 system (i s d @ e g
Fig.3.3.12. SEM of EHTPB (10 wt. %) mod@&EPN 1138-IDA-- I system
3.3.3. Epoxy-imide resins modified with CTBN-L and CTBN-S 3.3.4. Conclusions
3.3.3.1 Effect of addition of CTBN-L on the adhesive strength ofGY 250-/EPN 1138-IDA-[/IDA-I1 systems
3.3.3.2 Thermal stability of epoxy-imide systems modified withCTBN-L
3.3.3.3 Morphological studies of epoxy-imide systems modified withCTBN-L
3.3.3.4 Effect of addition of CTBN-S on the adhesive strength of GY250-/EPN 1138-IDA-IIIDA-I1 systems
Fig. 3.3.18. SEM of CTBN-L (10 phr) -modifiedGY 250-IDA-I system
Fig. 3.3.1 9. SEM of CTBN-L (I 0 phr) -modgedEPN 1138-IDA-I system
3.3.3.5 Thermal st: thility of CTBN-S-modified epoxy-imide resins
3.3.3.6 Morphology studies of epoxy-imide resins modifiedwith CTBN-S
Fig. 3.3.25. SEM of CTBN-S (I0 ph) -mudfiedGY 250-IDA-1 system
Fig. 3.3.26. SEM of CTBN-S (I 0 phr) n~oclijriedEPN 1 138-IDA-1 system
3.3.3.7 Comparison of adhesive strength of epoxy-imides modifiedwith EHTPB, CTBN-L and CTBN-S
3.3.4. Conclusions
3.4. Epoxy-imide resins containing siloxane linkages
3.4.1. Background
3.4.2. Synthesis of 1, 3-bis (3-trimellitimidopropyl) 1, 1, 3, 3-tetramethyldisiloxane (DIDA-XII)
3.4.3. Synthesis of epoxy-imide resins containing siloxane linkages
3.4.3.1 Thermal stability of epoxy-imide resins containing siloxanelinkages
3.4.3.2 Adhesive lap shear strength of epoxy-imide resinscontaining siloxane linkages
3.4.4. Synthesis of siloxane-imide-epoxy resin
3.4.5. Siloxane-epoxy-imide resin based atomic oxygen resistant coatings
3.4.5.1 Preparation of siloxane-epoxy-imide coatings
3.4.5.2 Evaluation af A0 resistance of siloxane-imide-epoxy-basedcoating
3.4.5.3 Siloxane-imide-epoxy based A0 resistant coating forpolyimide film
Fig. 3.4.1 4. SEM of uncoated aluminized Kapiour$lm {tMcknr!ss: 25 pm) exposed lo AO, flumce of 4.4xldb aomdm2
Fig. 3.4.15. SEM of coated aluminized Kupton flm thickness: 6th ickness: 25, ug] exposed to A0 jluence of20xl d atoms/cm2
Fig 3.418. SEM of coated aluminized Kapton film (1 25) exposed to A 0 fluence of 20xld0 atoms/cm r
3.4.5.4 Siloxane-imide-epoxy based A0 resistant coating forC-polyimide and glass-polyimide composites
Fig. 3.4.20. SEM of urlcoated C-PI composite exposed to A 0fruence of 9.6x1do ~oms/cm2
Fig. 3.4.21. SEM of coated C-PI composite exposed AO fluence of 23x10 28 atoms/cm2
Fig. 3.4.23. SECi of uwuated glw-potyrmi& compositeexposed to A0 fluence of 9.6r10ae otoms/cd
Fig. 3.4.2 4. SEM of coaled glas.v-polyinzid e composireexposed to AO.j[uence of 23x1 0 aloms/cm2
3.4.6 Conclusions
3.5. Addition-type epoxy-imide resins
3.5.1 Background
3.5.2 Synthesis of monoitaconamic acid (MIA)
3.5.3. Background
3.5.4 Synthesis of addition-type epoxy-imide resins
3.5.5. Thermal stability of addition-type epoxy-imides
3.5.6. Adhesive strength of addition-type epoxy-imide resins
3.5.7. Conclusions
4. SUMMARY AND CONCLUSIONS
Scope for further work
REFERENCES
Research Publications & Patents
Epoxy-lmide Resins from N- (4- and 3-carboxyphenyl) trimellitimides. I. Adhesiveand Thermal Properties