Improvement in Char Strength with an Open Cage Silsesquioxane Flame Retardant
Abstract
:1. Introduction
2. Results and Discussion
2.1. Silsesquioxane Oligomers
2.2. Unsaturated Polyester Composite Materials
3. Materials and Methods
3.1. Materials
3.2. Preparation of Silsesquioxane Oligomers
3.3. Preparation of Polymer Composites
3.4. Silsesquioxane Oligomer Structural Characterisation
3.5. Polymer Composite Characterisation
4. Conclusions
Author Contributions
Conflicts of Interest
References
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Reference | Reaction Time | ||||
---|---|---|---|---|---|
t = 0 h | t = 24 h | t = 48 h | |||
Chemical Shifts (ppm) | Chemical Shifts (ppm) | Intensity Ratio | Chemical Shifts (ppm) | Intensity Ratio | |
α | 5.07 | 8.50 | --- | 8.50 | --- |
γ | 66.16 | 66.38 66.68 | 0.40 0.60 | 66.36 66.65 | 0.35 0.65 |
a | 124.64 | 125.31 125.44 | 0.32 0.68 | 125.29 125.42 | 0.34 0.66 |
c | 166.85 | 167.43 167.67 | 0.32 0.68 | 167.34 167.61 | 0.34 0.66 |
Species | Chemical Band Shift (ppm) |
---|---|
T1 | −47.4 to −49.3 |
T21(3c) | −52.7 to −54.2 |
T20(3c) | −54.2 to −55.4 |
T21(4c) | −55.4 to −56.1 |
T20(4c) | −56.1 to −57.3 |
T2(5c+6c+l) | −57.3 to −58.1 |
T3(3c) | − 58.1 to −59.2 |
T3(4c) | −59.2 to −60.7 |
T3(r) | −62 to −69 |
Experimental m/z Value | Integration | Species | Structures |
---|---|---|---|
417.1 | 20% | T2(OH)4Na+ (l) | |
433.1 | 6% | T2(OH)3(OCH3)Na+ (l) | |
604.8 | 15% | T3(OH)5Na+ (l) | |
618.9 | 8% | T3(OH)4(OCH3)Na+ (l) | |
774.7 | 11% | T4(OH)4Na+ (c) | |
788.7 | 8% | T4(OH)3(OCH3)Na+ (c) |
Experimental m/z Value | Integration | Species | Structures |
---|---|---|---|
1115.3 | 15% | T6(OH)2Na+ (3c) | |
945.5 | 13% | T5(OH)3Na+ (2c) | |
664.3 1303.7 | 9% | T7(OH)3Na2+2 (3c) T7(OH)3Na+ (3c) | |
578.5 1133.5 | 9% | T6(OH)4Na2+2 (2c) T6(OH)4Na2+2 (2c) | |
775.2 | 7% | T4(OH)4Na+ (c) | |
55.6 1285.0 | 6% | T7(OH)Na2+2 (4c) T7(OH)Na (4c) | |
587.0 1149.4 | 5% | T6(OH)6Na2+2 (1c) T6(OH)6Na+ (1c) | |
1491.2 | 4% | T8(OH)4Na+ (3c) |
Composite | Resin | ATH | MAPTMS (Synthesis Time) | POSS | Limiting Oxygen Index (LOI) | Mechanical Resistance of Combustion Char (kg/cm2) |
---|---|---|---|---|---|---|
R100 | 100% | 0% | 0% | 0% | 21% | --- |
R40A60 | 40% | 60% | 0% | 0% | 44% | --- |
R40A55M5-0 h | 40% | 55% | 5% (0 h) | 0% | 46% | 0.7 ± 0.3 |
R40A55M5-24 h | 40% | 55% | 5% (24 h) | 0% | 48% | 0.7 ± 0.2 |
R40A55M5-48 h | 40% | 55% | 5% (48 h) | 0% | 50% | 1.2 ± 0.1 |
R40A55M5-96 h | 40% | 55% | 5% (96 h) | 0% | 50% | 2.3 ± 0.2 |
R40A55M5-264 h | 40% | 55% | 5% (264 h) | 0% | 50% | 2.8 ± 0.2 |
R40A55P5 | 40% | 55% | 0% | 5% | 51% | 0.8 ± 0.1 |
Temperature (°C) | R100 | R + M |
---|---|---|
25 | ||
350 | ||
380 | ||
400 | ||
800 | --- |
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Bautista, Y.; Gozalbo, A.; Mestre, S.; Sanz, V. Improvement in Char Strength with an Open Cage Silsesquioxane Flame Retardant. Materials 2017, 10, 567. https://doi.org/10.3390/ma10060567
Bautista Y, Gozalbo A, Mestre S, Sanz V. Improvement in Char Strength with an Open Cage Silsesquioxane Flame Retardant. Materials. 2017; 10(6):567. https://doi.org/10.3390/ma10060567
Chicago/Turabian StyleBautista, Yolanda, Ana Gozalbo, Sergio Mestre, and Vicente Sanz. 2017. "Improvement in Char Strength with an Open Cage Silsesquioxane Flame Retardant" Materials 10, no. 6: 567. https://doi.org/10.3390/ma10060567