Intrinsic nonsolvent polymerization

Akagi, K., Sakamaki, K., and Shirakawa, H., Intrinsic nonsolvent polymerization method for synthesis of polyacetylene films, Synth. Med., 55, 779-784 (1993). Catellani, M., Destri, S., and Bolognesi, A., New catalytic systems for acetylene polymerization, MakromoL Chem., 187, 1345-1349 (1986). 

Akagi, K. Sakamaki, K. Shirakawa, H. Intrinsic nonsolvent polymerization method for synthesis of highly stretchable and highly conductive polyacetylene films. Macromolecules 1992, 25, 6725-6726. 

POLYMERIZATION Solvent evacuation (SE) method and intrinsic nonsolvent (INS)... 

The intrinsic nonsolvent (INS) polymerization protocol [34], where solvent is never employed, is a technique that is closely related to the solvent evacuation method. In a typical experiment, neat AlEt3 was dropped into neat Ti(OBu)4 in a Schlenk flask at 0°C. The catalyst was aged for 1 h at room temperature and then further aged for another hour at 150° C. The flask was degassed and rotated to coat its walls with the catalyst solution. The system was then cooled to —78°C and acetylene was added. The reaction was allowed to proceed for 30-60 min before quenching. The resulting PA film was washed with toluene at — 78°C and dried under vacuum. 

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