Preparation of polyamic acid and polyimide nanoparticles by compressed fluid antisolvent and thermal imidization

• Polyamic acid (PAA) was precipitated by compressed CO2 antisolvent.
• Increasing temperature increased PAA particle size.
• Increasing pressure reduced PAA particle size.
• Decreasing concentration of PAA in solution reduced PAA particle size.
• Polyimide was successfully produced from PAA via thermal imidization.

Polyamic acid (PAA) nanoparticles were generated by injection of an N-methyl-2-pyrrolidone (NMP) solution containing dissolved PAA into a high-pressure CO2 chamber in which the precipitation of PAA occurred by the antisolvent technique. Supercritical CO2 was then continuously fed into the chamber to dry the precipitated PAA. The effects of temperature, pressure and PAA concentration on PAA nanoparticle morphology and size were systematically examined. The results indicated that PAA size could be reduced by decreasing temperature or concentration and by increasing pressure. Spherical PAA nanoparticles with reduced coalescence could be generated at the condition of 313 K, 13.79 MPa and 1.0 wt% PAA in NMP. The resultant PAA nanoparticles and the corresponding polyimide (PI) nanoparticles obtained by thermal imidization treatment of PAA at the determined heating conditions were characterized by thermogravimetric analysis and Fourier transform infrared spectroscopy. With evidence of an imide ring structure and high thermal stability, PI was verified to be successfully produced.

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