Thermal and Mechanical Characterization of EMA-TEGDMA Mixtures for Cosmetic Applications
Abstract
:1. Introduction
2. Experimental Section
2.1. Materials
2.2. Experimental Procedures
2.2.1. Procedure for Checking the Curing Process for Liquid Formulations
- In a vial, about 200 mg of a liquid formulation + about 2 mg of BPO were weighted and quickly dissolved at room temperature;
- When the solution was complete, the curing process started, so this vial needed to be kept in an ice/salt bath at –15 °C in order to stop this polymerization process;
- While the DSC device was equilibrated at –50 °C, a sample of the solution was prepared in the crucible in order to introduce it quickly into the DSC oven;
- Finally, after sample introduction into the DSC oven, it was equilibrated at –50 °C a few minutes more and then a dynamic experiment was performed up to 200 °C, in order to check the curing process of the liquid mixture.
2.2.2. Procedure for Preparing Samples of Final Materials for Mechanical Testing
- In a vial, around 10 mL of each liquid formulation was dropped with around 6 g of POW;
- This mixture was stirred quickly at room temperature with a glass bar;
- When the solution achieved the dough state, the mixture was poured over the silicone mold in order to fill it completely;
- The mixture was kept at room temperature overnight in the silicone mold in order to complete the curing process of the materials.
2.3. Measurement Techniques
3. Results and Discussion
3.1. Dynamic DSC Study of the Thermal Curing Process for Liquid Formulations:
3.2. Isothermal DSC Study of the Thermal Curing Process for Liquid Formulations
3.3. Thermal and Mechanical Characterization of Materials Prepared with Each Liquid Formulation
3.3.1. Thermal Stability Studies of the Cured Materials by TGA
3.3.2. Thermo-Mechanical Characterization of the Cured Materials by DMTA
3.3.3. Microindentation Hardness Characterization of the Cured Materials
3.3.4. Impact Strength Characterization of the Cured Material
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Formulation | EMA | TEGDMA | DMT | B-3 |
---|---|---|---|---|
A | 83.5 | 15 | 1 | 0.50 |
B | 88.5 | 10 | 1 | 0.50 |
C | 93.5 | 5 | 1 | 0.50 |
D | 83.63 | 15.13 | 0.75 | 0.50 |
E | 88.63 | 10.13 | 0.75 | 0.50 |
F | 93.63 | 5.13 | 0.75 | 0.50 |
G | 83.75 | 15.25 | 0.50 | 0.50 |
H | 88.75 | 10.25 | 0.50 | 0.50 |
I | 93.75 | 5.25 | 0.50 | 0.50 |
Formulation | Polymerization ΔH at 25 °C (10−2) (J/g) | Residual ΔH (10−2) (J/g) | t at α95 (min) |
---|---|---|---|
Commercial | 2.4 ± 0.1 | 0.21 ± 0.01 | 31 ± 1 |
A | 2.3 ± 0.1 | 0.23 ± 0.01 | 32 ± 1 |
B | 2.2 ± 0.2 | 0.24 ± 0.02 | 43 ± 2 |
C | 2.3 ± 0.1 | 0.26 ± 0.05 | 66 ± 2 |
D | 2.3 ± 0.1 | 0.27 ± 0.02 | 34 ± 1 |
E | 2.2 ± 0.1 | 0.28 ± 0.02 | 46 ± 1 |
F | 2.0 ± 0.3 | 0.22 ± 0.02 | 73 ± 1 |
G | 2.4 ± 0.1 | 0.30 ± 0.01 | 37 ± 1 |
H | 2.3 ± 0.1 | 0.25 ± 0.02 | 54 ± 1 |
I | 1.7 ± 0.3 | 0.24 ± 0.01 | 80 ± 1 |
Curing time at 25 °C (min) | Residual ΔH (J/g) |
---|---|
30 | 11 ± 1 |
60 | 9 ± 1 |
90 | 6 ± 2 |
180 | 2 ± 1 |
300 | 0.5 ± 0.2 |
Formulation | Onset TGA curve (5% Mass Loss) (°C) | Tmax (°C) |
---|---|---|
A | 273 | 390 |
B | 251 | 389 |
C | 256 | 389 |
D | 267 | 388 |
E | 236 | 388 |
F | 245 | 386 |
Formulation | Tg (°C) | E (MPa) |
---|---|---|
A | 95 ± 1 | 900 ± 34 |
B | 95 ± 1 | 743 ± 37 |
C | 94 ± 1 | 564 ± 29 |
D | 91 ± 1 | 436 ± 27 |
E | 91 ± 1 | 329 ± 22 |
F | 90 ± 1 | 259 ± 21 |
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Donoso, R.; Reina, J.A.; Giamberini, M.; De La Flor, S.; Ferrando, F.; Cerruti, P. Thermal and Mechanical Characterization of EMA-TEGDMA Mixtures for Cosmetic Applications. Polymers 2018, 10, 256. https://doi.org/10.3390/polym10030256
Donoso R, Reina JA, Giamberini M, De La Flor S, Ferrando F, Cerruti P. Thermal and Mechanical Characterization of EMA-TEGDMA Mixtures for Cosmetic Applications. Polymers. 2018; 10(3):256. https://doi.org/10.3390/polym10030256
Chicago/Turabian StyleDonoso, Ruben, Jose Antonio Reina, Marta Giamberini, Silvia De La Flor, Francesc Ferrando, and Pierfrancesco Cerruti. 2018. "Thermal and Mechanical Characterization of EMA-TEGDMA Mixtures for Cosmetic Applications" Polymers 10, no. 3: 256. https://doi.org/10.3390/polym10030256