Ethylene → HCID 86584015, compound

Participants

Reaction Steps

In a terpolymerization reaction, 1-octene (80 mmol) and divinylbenzene (20 mmol) were mixed with 100 ml of hexane and 3 ml of methylaluminoxane (MAO) (2.5 M in toluene) in a sealed Parr 450 mL stainless autoclave equipped with a mechanical stirrer. The sealed reactor was then saturated with 10 psi ethylene gas at 50° C. before adding an ethyldiindenylzirconium dichloride catalyst solution (Et(Ind)2ZrCl2 (2.5 μmol) in toluene) to initiate the polymerization. Additional ethylene was fed continuously into the reactor by maintaining a constant pressure (10 psi) during the entire course of the polymerization. After 30 minutes, the reaction was terminated by adding 100 mL of dilute HCl solution in methanol. The polymer was precipitated in methanol and isolated by filtration. Further purification was carried out by redissolving the polymer in hexane and reprecipitating it in methanol twice. After vacuum drying for 8 h, 3.79 g of ethylene/1-octene/divinylbenzene terpolymer were obtained. The terpolymer was completely soluble in common organic solvents, such as hexane, toluene and tetrahydrofuran (THF). The terpolymer composition (69.4 mol % ethylene, 28.6 mol % 1-octene, and 2.0 mol % DVB) and molecular weight (Mw=92,900 and Mn=43,300) were analyzed by 1H NMR and gel permeation chromatography (GPC), respectively. The mole ratio of unsaturation/divinylbenzene moieties (TUS/DOU) is near unity. The glass transition temperature of the terpolymer (Tg=-57° C.), was measured by differential scanning calorimetry (DSC). The sharp Tg transition with flat baseline indicates homogeneous terpolymer microstructure.

Provenance & Evidence