SYNTHESIS AND CHARACTERIZATION OF WATER SOLUBLE POLY(AMIC ACID) SALTS FROM ULTEM POLY(AMIC ACID)

Christy Sensenich and Dr. Judy Riffle, John Facinelli, Dr. Limin Dong
National Science Foundation and Technology Center:
High Performance Polymeric Adhesive and Composites, and
Department of Chemistry
Virginia Polytechnic Institute and State University
Blacksburg, Virginia

ABSTRACT

The synthesis of Ultem poly(amic acid), solution imidization, thermal imidization from the powder, preparation of water soluble poly(amic acid) salts and water soluble partially imidized poly(amic acid) salts, and molecular weight analysis of the imidized poly(amic acid) and the poly(amic acid) salts have been explored. NMR spectroscopy, IR spectroscopy, potentiometric titration, thermo-gravimetric analyze(TGA), and size exclusion gel permeation chromatography (GPC) were utilized to analysis the samples. The pre-calculated number average molecular weight of the poly(amic acid) was reached in 24 hours, but following subsequent precipitations in water to isolate the product the molecular weight dropped significantly. Thermal imidization from the powder showed advantages over the solution method. No precipitation in water was necessary, and hydrolysis was significantly reduced as the water was removed as soon as it was formed. Three partially imidized poly(amic acid) samples were prepared and converted to their salts. All poly(amic acid) salts were prepared from methanolic tetramethylammonium hydroxide (TMAH) and tetraethylammonium hydroxide (TEAH). The poly(amic acid) salts and partially imidized poly(amic acid) salts (up to 25% imidized), were water soluble. Molecular weight analysis by GPC showed that the molecular weights of the imidized poly(amic acid) and the poly(amic acid) salts increase with imidization at 250 deg. C. Also, the molecular weight of the final imidized material is unaffected by exposure of the salts to water.