In this study, we tried to prepare an isotropic spinnable pitch which can be useful to prepare the general purpose carbon fiber through the co-carbonization of biomass tar with ethylene bottom oil under two different preparation methods (atmospheric distillation, pressurized distillation). The results showed that the ethylene bottom oil added co-carbonization was very effective to decrease of the oxygen contents for obtaining a stable spinnable pitch. The pressurized distillation was more effective to reduce the oxygen functional groups of pitches than atmospheric distillation. The obtained spinnable pitch by the pressurized distillation showed higher pitch yield of 42% and lower oxygen content of 9.12% than the spinnable pitch by the atmospheric distillation. The carbon fiber derived from the pressurized distillation spinnable pitch by carbonization at 800ºC for 5 min showed that the higher tensile strength of carbon fiber was increased up to 800 MPa.

Isotropic pitch-based fibers produced from coal tar pitch with the melt-blowing method were carbonized at temperatures ranging from 800 to 1600oC to investigate their crystalline structure and physical properties as a function of the carbonization temperature. The in-plane crystallite size (La) of the carbonized pitch fiber from X-ray diffraction increased monotonously by increasing the carbonization temperature resulting in a gradual increase in the electrical conductivity from 169 to 3800 S/cm. However, the variation in the d002 spacing and stacking height of the crystallite (Lc) showed that the structural order perpendicular to the graphene planes got worse in carbonization temperatures from 800 to 1200oC probably due to randomization through the process of gas evolution; however, structural ordering eventually occurred at around 1400oC. For the carbonized pitch powder without stabilization, structural ordering perpendicular to the graphene planes occurred at around 800–900oC indicating that oxygen was inserted during the stabilization process. Additionally, the shear stress that occurred during the melt-blowing process might interfere with the crystallization of the CPF.

In this work, thermal treatment accompanied with different acid treatments was applied to a commercial coal tar pitch (CTP) to obtain a spinnable precursor pitch for carbon fiber. In the case of thermal treatment only, a relatively high reaction temperature of between 380˚C and 400˚C was required to obtain a softening point (SP) range of 220˚C-260˚C and many meso-phase particles were created during the application of high reaction temperature. When nitric acid or sulfuric acid treatment was conducted before the thermal treatment, the precursor pitch with a proper SP range could be obtained at reaction temperatures of 280˚C-300˚C, which were about 100˚C lower than those for the case of thermal treatment only. With the acid treatments, the yield and SP of the precursor pitch increased dramatically and the formation of meso-phase was suppressed due to the lower reaction temperatures. Since the precursor pitches with acid and thermal treatment were not spinnable due to the inhomogeneity of properties such as molecular weight distribution and viscosity, the CTP was mixed with ethanol before the consecutive nitric acid and thermal treatments. The precursor pitches with ethanol, nitric acid, and thermal treatments were easily spinnable, and their spinning and carbon fiber properties were compared to those of air blowing and thermal treated CTP.

Isotropic pitch fibers were stabilized and carbonized for preparing carbon fibers. To optimize the duration and temperature during the stabilization process, a thermogravimetric analysis was conducted. Stabilized fibers were carbonized at 1000, 1500, and 2000℃ in a furnace under a nitrogen atmosphere. An elemental analysis confirmed that the carbon content increased with an increase in the carbonization temperature. Although short graphitic-like layers were observed with carbon fibers heat-treated at 1500 and 2000℃, Raman spectroscopy and X-ray diffraction revealed no significant effect of the carbonization temperature on the crystalline structure of the carbon fibers, indicating the limit of developing an ordered structure of isotropic pitch-based carbon fibers. The electrical conductivity of the carbonized fiber reached 3.9×10⁴S/m with the carbonization temperature increasing to 2000℃ using a four-point method.

A petroleum-based isotropic pitch fiber spun by melt-blown method was oxidized in air flow at various conditions. The oxidized pitch fiber obtained was tested for its infusibility and its elemental composition during the process of stabilization. The structural changes were traced by using solvent solubility, FT-IR spectroscopy, and elemental analysis. The samples showed a gradual increase in weight with increasing the oxidization temperature. The weight gain of sample oxidized at 320℃ for 10 min was about 4.5%. The concentration of the pyridine and toluene soluble fraction decreased with an increase in stabilization temperatures. The oxygen uptaken in the stabilization process converted aliphatic side chains into the carbonyl groups. As stabilization proceeded, the more ether and carboxylic acid groups were formed through the oxidations of aldehyde and primary alcohol, and then the carboxylic acid was dehydrated to be aromatic anhydride.