Original Basic Activation for Enhancing Silica Particle Reactivity: Characterization by Liquid Phase Silanization and Silica-Rubber Nanocomposite Properties
Abstract
:1. Introduction
2. Materials and Methods
2.1. Silica Pre-Loading of the Base Catalyst
2.2. Silica Silanization
2.3. Preparation of 1H NMR Samples
2.4. Silica-Rubber Composite Fabrication
2.5. Characterization
3. Results and Discussion
3.1. Impact of Basic Activation on Silica Particles
3.2. Silica Reactivity Enhancement Evaluation
3.3. Thermogravimetric Analysis
3.4. 1H Liquid State NMR
- nsilane is the amount of silane in solution (mmol),
- ACH3 is the area of the CH3 peak at 0.88 ppm,
- AOMCTS is the area of the OMCTS peak at 0.09 ppm,
- NOMCTS is the number of hydrogen nuclei generating the signal,
- NCH3 is the number of hydrogen nuclei generating the signal,
- nOMCTS is the amount of OMCTS internal standard in the CDCl3 solution (mmol).
3.5. Evaluation of Silica Reactivity Enhancement in Rubber-Silica Composites
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Components | phr | Mixing Conditions | |
---|---|---|---|
Step 1 | Polystyrene-butadiene | 80 | 80 °C for 10′ |
Polybutadiene | 20 | ||
TDAE Oil | 25 | ||
Zinc oxide | 0.5 | ||
Stearic acid | 3 | ||
Silica | 65 | ||
Step 2 | Step 1 compound | - | 80 °C for 7′ |
Silica | 15 | ||
Silane (TESPD) | 8 | ||
6PPD | 2.5 | ||
Step 3 | Step 2 compound | - | 60 °C for 1′45″ |
Zinc oxide | 2 | ||
Sulfur | 1.1 | ||
MBT | 0.3 | ||
DPG | 3.2 | ||
CBS | 2.3 |
C6 | C12 | C18 | TEA-C6 | TEA-C12 | TEA-C18 | DBU-C6 | DBU-C12 | DBU-C18 | NaH-C6 | NaH-C12 | NaH-C18 | |
---|---|---|---|---|---|---|---|---|---|---|---|---|
TGA | 0.418 | 0.165 | 0.128 | 0.383 | 0.381 | 0.3 | 0.582 | 0.508 | 0.447 | 0.271 | 0.314 | 0.301 |
1H NMR | 0.274 | 0.176 | 0.186 | 0.185 | 0.198 | 0.173 | 0.299 | 0.289 | 0.206 | 0.188 | 0.149 | 0.165 |
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Moretto, E.; Yan, C.; Dieden, R.; Steiner, P.; Duez, B.; Lenoble, D.; Thomann, J.-S. Original Basic Activation for Enhancing Silica Particle Reactivity: Characterization by Liquid Phase Silanization and Silica-Rubber Nanocomposite Properties. Polymers 2022, 14, 1676. https://doi.org/10.3390/polym14091676
Moretto E, Yan C, Dieden R, Steiner P, Duez B, Lenoble D, Thomann J-S. Original Basic Activation for Enhancing Silica Particle Reactivity: Characterization by Liquid Phase Silanization and Silica-Rubber Nanocomposite Properties. Polymers. 2022; 14(9):1676. https://doi.org/10.3390/polym14091676
Chicago/Turabian StyleMoretto, Enzo, Chuanyu Yan, Reiner Dieden, Pascal Steiner, Benoît Duez, Damien Lenoble, and Jean-Sébastien Thomann. 2022. "Original Basic Activation for Enhancing Silica Particle Reactivity: Characterization by Liquid Phase Silanization and Silica-Rubber Nanocomposite Properties" Polymers 14, no. 9: 1676. https://doi.org/10.3390/polym14091676