Sepiolite is a clay mineral, a complex magnesium silicate, a typical formula for which is (OH2)4(OH)4Mg8Si12O30•8H2O. It is formed by blocks and cavities (tunnels) growing in the direction of the fibres. The tunnels, 3.7 x 10.6 Å in cross-section, are responsible for the high specific surface area and sorptive properties of sepiolite. The co-intercalation of 3-methyl cyclohex-2-en-1-one (MCH), the Douglas-Fir beetle anti-aggregation pheromone, with methanol, ethanol, acetone, or benzene into sepiolite tunnels was studied. The resulting nanohybrid materials were characterized by means of various techniques, such as multinuclear solid-state NMR spectroscopy, porosity studies and Thermal Gravimetric Analysis (TGA). This was done in the hope of obtaining slow and controlled release of MCH from the sepiolite tunnels. It was demonstrated by 13C MAS NMR (carbon-13 magic angle spinning nuclear magnetic resonance) that at room temperature there are two different MCH molecules: one MCH inside the tunnels and the other one outside the tunnels of the sepiolite. Heating nanohybrid materials at 60˚C for 20 hours removes the external MCH molecules from the sepiolite. 13C MAS NMR showed that by further heating nanohybrid materials at 120˚C for 20 hours, methanol, ethanol, or acetone peaks were greatly reduced; however, the benzene peak was not reduced. To better understand how benzene acts inside sepiolite, intercalation of d6-benzene, and co-intercalations of d6-benzene with MCH and d6-benzene with pyridine into sepiolite tunnels were carried out, and these samples were studied by the same techniques. Another technique was used in order to see whether the slow and controlled release of MCH from the sepiolite tunnels could be obtained: sepiolite-MCH nanohybrids were treated with 20 ml of 0.5 M HCl solution. It was found that when 1 gram of MCH-sepiolite sample was acid treated at room temperature, about 35% of intercalated MCH was removed from the sepiolite. The role of sepiolite clay was also studied in Maya-Blue representative structure sepiolite-indigo adduct. It is known that upon heating the sepiolite and indigo mixture, the stability that is present in Maya-Blue is achieved. It is still a mystery, however, how exactly indigo and sepiolite interact with each other.
| Identifer | oai:union.ndltd.org:uottawa.ca/oai:ruor.uottawa.ca:10393/20219 |
| Date | January 2011 |
| Creators | Blank, Katrin |
| Contributors | Detellier, Christian |
| Publisher | Université d'Ottawa / University of Ottawa |
| Source Sets | Université d’Ottawa |
| Language | English |
| Detected Language | English |
| Type | Thesis |
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