Supercritical Fluid Extraction: Preparing a Superior Mesophase Precursor forCarbon Fibers

摘要

Supercritical fluid (SCF) extraction is being investigated for the production ofmesophase pitch, the liquid-crystalline precursor for the manufacture of high-performance carbon fibers. The mesophase pitch is produced by fractionation of an isotropic petroleum pitch with supercritical toluene in a region of liquid-liquid equilibrium that exists at pressures above 40 bar. Dramatic improvements in the reliability of our apparatus have recently been made, and mesophase pitch can now be produced on a routine basis. An experimental program was conducted to explore the effects of temperature, solvent-to-pitch (S/P) ratio, and solvent solubility parameter on the properties of the mesophase pitch produced. Temperatures of 320 and 360 deg C, solubility parameters of 3.7 and 5.0 (cal/cc)(1/2), and S/P ratios of 2.5 and 3.5 were chosen to conform to a two-level, augmented factorial experiment. A linear model correlated the data to a high degree of certainty. Results indicate that we can adjust SCF operating conditions and tailor-make a mesophase pitch for a given end use. We have discovered a semitheoretical method for predicting a priori the softening point and yield of mesophase pitch for a given set of SCF operating conditions. The SCF extraction process can be represented on a pseudoternary phase diagram, and good estimates of product yields and softening points can be made from a limited experimental data measured at other conditions.