Solvent-Free Synthesis of Amidated Carboxymethyl Cellulose Derivatives: Effect on the Thermal Properties
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Acidification of NaCMC
2.3. General Procedure for Thermal Amidation Reaction on HCMC
2.4. Characterizations
2.4.1. Size Exclusion Chromatography (SEC)
2.4.2. Infrared Analysis (IR)
2.4.3. Nuclear Magnetic Resonance (NMR)
2.4.4. Thermogravimetric Analysis (TGA)
2.4.5. Differential Scanning Calorimetry (DSC)
2.4.6. Dynamical Mechanical Analysis (DMA)
3. Results
3.1. Thermal Amidation of Carboxymethyl Cellulose
3.2. Thermal Properties of Amidated CMC Derivatives
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Entry | Sample | R’ | DSCM | Mass Yield (%) | DSamide 1 | DSsub 1 | Substitution Efficiency (%) 2 | Tdonset (°C) 3 | Tdmax (°C) 4 | Tg (°C) 5 |
---|---|---|---|---|---|---|---|---|---|---|
1 | NaCMC | - | 1.2 | - | - | - | - | 225 | 288 | ND6 |
2 | HCMC | - | 1.2 | 86 | - | - | - | ND6 | 319 | ND6 |
3 | CMC1.2-Benz | | 1.2 | 75 | 0.95 | 1 | 83 | 190 | 323 | 129 |
4 | CMC0.9-Benz | | 0.9 | 68 | 0.6 | 0.7 | 78 | 185 | 312 | 138 |
5 | CMC0.7-Benz | | 0.7 | 66 | 0.5 | 0.6 | 85 | 190 | 309 | 140 |
6 | CMC-PE | | 1.2 | 76 | 0.5 | 0.85 | 71 | 190 | 312 | 122 |
7 | CMC-PP | | 1.2 | 70 | 0.55 | 0.9 | 75 | 180 | 313 | 105 |
8 | CMC-PB | | 1.2 | 57 | 0.5 | 0.8 | 67 | 185 | 319 | 90 |
9 | CMC-Und | | 1.2 | 69 | 0.7 | 0.8 | 67 | 140 | 334 | ND6 |
10 | CMC-Dod | | 1.2 | 67 | 0.65 | 0.8 | 67 | 150 | 332 | ND6 |
11 | CMC-Furf | | 1.2 | 68 | 0.75 | 0.95 | 79 | 180 | 318 | 147 |
12 | CMC-Thio | | 1.2 | 76 | 0.7 | 0.85 | 71 | 130 | 318 | 115 |
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Pettignano, A.; Charlot, A.; Fleury, E. Solvent-Free Synthesis of Amidated Carboxymethyl Cellulose Derivatives: Effect on the Thermal Properties. Polymers 2019, 11, 1227. https://doi.org/10.3390/polym11071227
Pettignano A, Charlot A, Fleury E. Solvent-Free Synthesis of Amidated Carboxymethyl Cellulose Derivatives: Effect on the Thermal Properties. Polymers. 2019; 11(7):1227. https://doi.org/10.3390/polym11071227
Chicago/Turabian StylePettignano, Asja, Aurélia Charlot, and Etienne Fleury. 2019. "Solvent-Free Synthesis of Amidated Carboxymethyl Cellulose Derivatives: Effect on the Thermal Properties" Polymers 11, no. 7: 1227. https://doi.org/10.3390/polym11071227