| Literature DB >> 32012769 |
Bolesław Szadkowski1, Anna Marzec1, Przemysław Rybiński2, Witold Żukowski3, Marian Zaborski1.
Abstract
Perlite and vermiculite are naturally occurring minerals, commonly used by industry to obtain highly thermoisolative and/or non-flammable materials. However, there has been little research into the preparation and application of rubber compounds containing these inexpensive mineral fillers. Here, we show the benefits of perlite and vermiculite minerals as fillers for ethylene-propylene rubber (EPM) composites. To obtain more uniform dispersion and improved compatibility between the minerals and the elastomer matrix, 1-allyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (AMIMTFSI) and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (BMIMTFSI) imidazolium ionic liquids (ILs) were added. The mineral fillers were found to be attractive semi-reinforcing fillers, which also act as flame retardants in the elastomer composites. Furthermore, a higher content of vermiculite mineral significantly reduced the air permeability of the composites. The incorporation of ionic liquids into the EPM-filled systems had a considerable effect on the torque increment, crosslink density, and more importantly the flammability of the studied compounds. The application of 2.5 parts per hundred parts of rubber (phr) BMIMTFSI, in particular, reduced the flammability of the EPM composite, as the maximum heat release rate (HRRmax) decreased from 189.7 kW/m2 to 170.2 kW/m2.Entities:
Keywords: composite properties; ethylene–propylene rubber; ionic liquids; perlite; vermiculite
Year: 2020 PMID: 32012769 PMCID: PMC7040615 DOI: 10.3390/ma13030585
Source DB: PubMed Journal: Materials (Basel) ISSN: 1996-1944 Impact factor: 3.623
Composition of EPM-filled mixtures (in phr—parts per hundred parts of rubber).
| Compound | Neat EPM | DCP | TTT | Perlite | Vermiculite | AMIMTFSI | BMIMTFSI |
|---|---|---|---|---|---|---|---|
| EPM | 100 | 1 | 0.25 | 0 | 0 | 0 | 0 |
| EPM/5PT | 100 | 1 | 0.25 | 5 | 0 | 0 | 0 |
| EPM/10PT | 100 | 1 | 0.25 | 10 | 0 | 0 | 0 |
| EPM/20PT | 100 | 1 | 0.25 | 20 | 0 | 0 | 0 |
| EPM/20PT/AMIMTFSI | 100 | 1 | 0.25 | 20 | 0 | 2.5 | 0 |
| EPM/20PT/BMIMTFSI | 100 | 1 | 0.25 | 20 | 0 | 0 | 2.5 |
| EPM/5VMT | 100 | 1 | 0.25 | 0 | 5 | 0 | 0 |
| EPM/10VMT | 100 | 1 | 0.25 | 0 | 10 | 0 | 0 |
| EPM/20VMT | 100 | 1 | 0.25 | 0 | 20 | 0 | 0 |
| EPM/20VMT/AMIMTFSI | 100 | 1 | 0.25 | 0 | 20 | 2.5 | 0 |
| EPM/20VMT/BMIMTFSI | 100 | 1 | 0.25 | 0 | 20 | 0 | 2.5 |
Figure 1Digital photographs of EPM vulcanizates filled with different contents of perlite and vermiculite.
Rheometric parameters and crosslink density values of EPM-filled compounds.
| Compound | Mmin (dNm) | ΔM (dNm) | t02 (min) | t90 (min) | υe (mol/cm3) |
|---|---|---|---|---|---|
| EPM | 0.81 | 4.80 | 1.07 | 18.84 | 3.4 |
| EPM/5PT | 0.91 | 5.41 | 1.09 | 17.29 | 4.5 |
| EPM/10PT | 0.98 | 6.08 | 1.03 | 17.20 | 5.3 |
| EPM/20PT | 1.14 | 7.19 | 0.91 | 15.76 | 5.9 |
| EPM/20PT/AMIMTFSI | 0.96 | 5.37 | 0.83 | 14.16 | 5.0 |
| EPM/20PT/BMIMTFSI | 0.97 | 5.42 | 0.90 | 15.28 | 4.8 |
| EPM/5VMT | 0.87 | 4.83 | 1.16 | 14.76 | 3.5 |
| EPM/10VMT | 0.93 | 4.86 | 1.03 | 13.29 | 3.6 |
| EPM/20VMT | 0.99 | 4.45 | 1.06 | 12.76 | 2.8 |
| EPM/20VMT/AMIMTFSI | 0.96 | 5.90 | 1.01 | 11.57 | 4.3 |
| EPM/20VMT/BMIMTFSI | 0.96 | 5.62 | 1.02 | 11.58 | 4.9 |
Mmin—minimum torque moment, ∆M—increment of torque, t02—scorch time, t90—optimum curing time, υe—crosslink density.
Figure 2Mechanical curves of the studied EPM composites: (a) tensile test; (b) tear resistance.
Figure 3Mechanical parameters of the EPM composites with 20 phr (parts per hundred parts of rubber) of filler and 2.5 phr of ionic liquids: (a) tensile strength; (b) tear resistance.
Figure 4Gas permeability coefficient values for EPM composites filled with different contents of perlite and vermiculite.
Figure 5Thermogravimetric curves of the perlite and vermiculite minerals.
Figure 6Thermogravimetric curves of the unfilled EPM elastomer and EPM composites with 20 phr of perlite and vermiculite fillers.
Thermogravimetric data for EPM composites.
| Compound | T5 | T50 | TRMAX1 | TRMAX2 | dm/dt1 | dm/dt2 | P600 |
|---|---|---|---|---|---|---|---|
| EPM | 298 | 423 | 350 | 442 | 4.85 | 5.36 | 18.82 |
| EPM/5PT | 271 | 400 | 300 | 403 | 1.95 | 23.53 | 1.17 |
| EPM/10PT | 272 | 405 | 305 | 401 | 1.38 | 17.3 | 6.63 |
| EPM/20PT | 278 | 410 | 270 | 407 | 1.50 | 34.76 | 12.61 |
| EPM/5VMT | 288 | 405 | 292 | 398 | 1.33 | 30.34 | 10.42 |
| EPM/10VMT | 262 | 404 | 260 | 402 | 1.24 | 39.71 | 4.18 |
| EPM/20VMT | 296 | 410 | 261 | 403 | 0.93 | 20.16 | 15.65 |
T5, 50—temperature of sample 5% and 50% mass loss, TRMAX—temperature for maximum rate of thermal decomposition of tested vulcanizates, P600—residue after thermal decomposition of the composites.
Flammability parameters of EPM composites.
| Compound | TTI | HRR | HRRmax | THR | EHC | EHCmax | MLR |
|---|---|---|---|---|---|---|---|
| EPM | 70 | 202.7 | 576.0 | 92.9 | 51.0 | 79.0 | 0.206 |
| EPM/5PT | 68 | 204.1 | 445.9 | 57.7 | 31.8 | 77.5 | 0.257 |
| EPM/10PT | 70 | 195.5 | 390.5 | 49.8 | 38.1 | 79.2 | 0.212 |
| EPM/20PT | 90 | 66.34 | 189.7 | 16.6 | 10.4 | 64.2 | 0.224 |
| EPM/20PT/AMIMTFSI | 120 | 61.23 | 179.3 | 17.0 | 8.9 | 62.1 | 0.200 |
| EPM/20PT/BMIMTFSI | 110 | 63.52 | 170.2 | 16.2 | 9.3 | 60.2 | 0.265 |
| EPM/5VMT | 70 | 185.3 | 560.1 | 70.1 | 46.6 | 72.1 | 0.211 |
| EPM/10VMT | 73 | 171.8 | 529.6 | 47.9 | 75.8 | 78.2 | 0.014 |
| EPM/20VMT | 80 | 177.3 | 435.8 | 53.9 | 29.8 | 77.2 | 0.023 |
| EPM/20VMT/AMIMTFSI | 105 | 145.7 | 401.6 | 51.5 | 26.9 | 74.2 | 0.245 |
| EPM/20VMT/BMIMTFSI | 75 | 120.5 | 380.5 | 49.7 | 21.3 | 69.5 | 0.213 |
TTI—time to ignition; HRR—heat release rate; HRRmax—max heat release rate; THR—total heat release; EHC—effective heat of combustion; EHCmax—max effective heat of combustion; MLR—mass loss rate.
Figure 7Cone calorimetry test results showing flammability parameters of the EPM composites: (a) HRR vs. time and, (b) THR vs. time curves.
Figure 8SEM microphotographs of: (a) perlite; (b) vermiculite; (c) EPM composite filled with 10 phr of perlite; (d) EPM composite filled with 10 phr of vermiculite.