Synthesis and Thermal Properties of Acrylonitrile/Butyl Acrylate/Fumaronitrile and Acrylonitrile/Ethyl Hexyl Acrylate/Fumaronitrile Terpolymers as a Potential Precursor for Carbon Fiber
Abstract
:1. Introduction
2. Results and Discussion
2.1. FTIR Spectroscopy
2.2. Conversions and Composition Analysis
Monomers feed (mol%), M AN/comonomer/FN | Monomers conversion (%) | Monomers composition (mol%), m AN/comonomer/FN | Reacted monomer (%) m/M × 100 AN/comonomer/FN | Actual composition (mol%) AN/comonomer/FN |
---|---|---|---|---|
100/0/0 | 85 | 85/0/0 | 85/0/0 | 100/0/0 |
AN/BA/FN | ||||
95/5/0 | 77 | 71.35/4.50/0 | 75/90/0 | 94.1/5.9/0 |
90/10/0 | 75 | 64.06/8.90/0 | 71/89/0 | 87.8/12.2/0 |
90/2/8 | 73 | 64.58/1.78/6.24 | 72/89/78 | 88.9/2.5/8.6 |
90/4/6 | 67 | 57.29/3.48/4.74 | 64/87/79 | 87.5/5.3/7.2 |
90/6/4 | 68 | 58.33/5.10/3.08 | 65/85/77 | 87.7/7.7/4.6 |
90/8/2 | 61 | 49.48/6.96/1.51 | 55/87/76 | 85.4/12/2.6 |
AN/EHA/FN | ||||
95/5/0 | 76 | 69.79/4.55/0 | 73/91/0 | 93.9/6.1/0 |
90/10/0 | 77 | 64.58/9.0/0 | 72/90/0 | 87.8/12.2/0 |
90/2/8 | 71 | 61.46/1.82/6.32 | 68/91/79 | 88.3/2.6/9.1 |
90/4/6 | 68 | 57.29/3.60/4.62 | 64/90/77 | 87.45/5.5/7.1 |
90/6/4 | 67 | 55.21/5.28/3.12 | 61/88/78 | 86.8/8.3/4.9 |
90/8/2 | 66 | 53.13/6.96/1.54 | 59/87/77 | 86.2/11.3/2.5 |
2.3. DSC Studies
2.3.1. Effect of Comonomer on Tg
AN/comonomer/FN (mol%) | Glass transition, Tg (°C) |
---|---|
100/0/0 | 210 ± 1 |
AN/BA/FN | |
90/2/8 | 69 ± 1 |
90/4/6 | 67 ± 2 |
90/6/4 | 67 ± 2 |
90/8/2 | 63 ± 1 |
90/10/0 | 70 ± 1 |
AN/EHA/FN | |
90/2/8 | 67 ± 1 |
90/4/6 | 65 ± 1 |
90/6/4 | 63 ± 1 |
90/8/2 | 60 ± 2 |
90/10/0 | 63 ± 1 |
2.3.2. Effect of Comonomer and Termonomer on Stabilization Temperature
AN/comonomer/FN (mol%) | Ti (°C) | Tf (°C) | ∆T (°C) | ∆H (J·g−1) | ∆H/∆t (J·g−1·min−1) |
---|---|---|---|---|---|
100/0/0 | 246 | 345 | 99 | 758 | 77 |
AN/BA/FN | |||||
90/10/0 | 264 | 321 | 57 | 590 | 104 |
90/2/8 | 228 | 309 | 81 | 371 | 46 |
90/4/6 | 233 | 317 | 84 | 392 | 47 |
90/6/4 | 241 | 331 | 90 | 437 | 49 |
90/8/2 | 260 | 353 | 93 | 489 | 53 |
AN/EHA/FN | |||||
90/10/0 | 263 | 306 | 43 | 523 | 122 |
90/2/8 | 250 | 321 | 71 | 321 | 45 |
90/4/6 | 221 | 291 | 70 | 345 | 49 |
90/6/4 | 220 | 304 | 84 | 356 | 42 |
90/8/2 | 241 | 327 | 86 | 381 | 44 |
2.4. TGA Studies
AN/comonomer/FN (mol%) | Weight loss (%) | Char yield (%) | |||
---|---|---|---|---|---|
Step 1 30–250 °C | Step 2 Part 1 250–350 °C | Step 2 Part 2 350–600 °C | Step 3 600–950 °C | ||
100/0/0 | 1.61 | 23.21 | 13.17 | 14.27 | 47.7 |
AN/BA/FN | |||||
90/10/0 | 0.18 | 34.62 | 20.14 | 7.06 | 38.0 |
90/2/8 | 0.15 | 29.99 | 14.69 | 10.04 | 45.1 |
90/4/6 | 0.18 | 32.52 | 15.01 | 8.43 | 43.9 |
90/6/4 | 0.17 | 34.21 | 15.98 | 9.53 | 40.1 |
90/8/2 | 0.19 | 33.76 | 17.01 | 9.06 | 40.0 |
AN/EHA/FN | |||||
90/10/0 | 0.45 | 35.80 | 15.0 | 11.67 | 37.1 |
90/2/8 | 1.67 | 30.18 | 14.14 | 10.12 | 43.9 |
90/4/6 | 0.24 | 33.21 | 15.73 | 8.34 | 42.5 |
90/6/4 | 0.78 | 35.01 | 16.23 | 7.79 | 40.2 |
90/8/2 | 1.12 | 38.65 | 14.29 | 6.84 | 39.1 |
3. Experimental Section
3.1. Synthesis and Characterization
3.2. Composition Analysis of Polymers
3.3. Differential Scanning Calorimetry (DSC)
3.4. Thermogravimetric Analysis
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Jamil, S.N.A.M.; Daik, R.; Ahmad, I. Synthesis and Thermal Properties of Acrylonitrile/Butyl Acrylate/Fumaronitrile and Acrylonitrile/Ethyl Hexyl Acrylate/Fumaronitrile Terpolymers as a Potential Precursor for Carbon Fiber. Materials 2014, 7, 6207-6223. https://doi.org/10.3390/ma7096207
Jamil SNAM, Daik R, Ahmad I. Synthesis and Thermal Properties of Acrylonitrile/Butyl Acrylate/Fumaronitrile and Acrylonitrile/Ethyl Hexyl Acrylate/Fumaronitrile Terpolymers as a Potential Precursor for Carbon Fiber. Materials. 2014; 7(9):6207-6223. https://doi.org/10.3390/ma7096207
Chicago/Turabian StyleJamil, Siti Nurul Ain Md, Rusli Daik, and Ishak Ahmad. 2014. "Synthesis and Thermal Properties of Acrylonitrile/Butyl Acrylate/Fumaronitrile and Acrylonitrile/Ethyl Hexyl Acrylate/Fumaronitrile Terpolymers as a Potential Precursor for Carbon Fiber" Materials 7, no. 9: 6207-6223. https://doi.org/10.3390/ma7096207