Spinnable mesophase pitch precursor containing more than 98% mesophase content was successfully prepared from FCC-DO (fluid catalytic cracking-decant oil) without hydrogenation or catalytic reaction. The preparation method involved thermal condensation, vacuum treatment, and annealing treatment. Petroleum mesophase pitch-based carbon fibers are produced by melt spinning of pitch precursors, followed by stabilization and carbonization. The resulting carbon fiber exhibited good mechanical performances up to tensile strength of 2.1 GPa and tensile modulus of 212 GPa, with strain-to-failure higher than 1.0%. These properties ensuring that the automotive grade carbon fibers can be successfully prepared from FCC-DO derived petroleum mesophase pitches through the cost-competitive processes.

We demonstrated an effective way of preparing melt spinnable mesophase pitches via catalytic hydrogenation of petroleum residue (fluidized catalytic cracking-decant oil) and their subsequent thermal soaking. The mesophase pitches thus obtained were analyzed in terms of their viscosity, elemental composition, solubility, molecular weight, softening point and optical texture. We found that zeolite-induced catalytic hydrogenation under high hydrogen pressure contributed to a large variation in the properties of the pitches. As the hydrogen pressure increased, the C/H ratio decreased, and the solubility in n-hexane increased. The mesophase pitch with entirely anisotropic domains of flow texture exhibited good meltspinnability. The mesophase carbon fibers obtained from the catalytically hydrogenated petroleum residue showed moderate mechanical properties.

Taguchi’s experimental design was employed in the melt spinning of molten mesophase pitch to produce carbon fibers. The textures of the obtained carbon fibers were radial with varied crack angles, as observed by scanning electron microscopy and polarized optical imaging. The diameter, crack angle, preferred orientation, and tensile modulus of the produced samples were examined to investigate the influence of four spinning variables. The relative importance of the variables has been emphasized for each characteristic. The results show that thicker carbon fiber can be obtained with a smaller entry angle, a higher spinning temperature, a reduced winding speed, and an increased extrusion pressure. The winding speed was found to be the most significant factor in relation to the fiber diameter. While it was observed that thicker carbon fiber generally shows improved preferred orientation, the most important variable affecting the preferred orientation was found to be the entry angle. As the entry angle decreased from 120° to 60°, the shear flow was enhanced to induce more ordered radial alignment of crystallite planes so as to obtain carbon fibers with a higher degree of preferred orientation. As a consequence, the crack angle was increased, and the tensile modulus was improved.

The C-type mesophase pitch-based carbon fiber (C-MPCF) was prepared throuch C-type spinnerette and compared the mechanical properties to those of round type mesophase pitch fiber (R-MPCF) and C-type isotropic pitch fiber (C-iPCF). The tensile strength and modulus of C-MPCF were about 18.6% and 35.7% higher than those of R-MPCF. The tensile strength of C-MPCF was 62% higher than that of C-iPCF of the same 8μm thickness because of more linear transverse texture, which could be easily converted to graphitic crystallinity during heat treatment. The torsional rigidity of C-MPCF was 2.37 times higher than that of R-MPCF. The electrical resistivity of C-MPCF was 8μΩ·m. The C-iPCF shows far lower electrical resistivity than R-iPCF as well as the mesophase carbon fiber because of better alignment of texture to the fiber axis.