This study aims to improve the economic efficiency of the pitch synthesis reaction on the pilot plant by optimizing the pitch synthesis reaction and utilization of the byproduct. The pitch was synthesized using a 150 L pilot plant with pyrolyzed fuel oil as a precursor. The pitch synthesis reaction is carried out through volatilization and polycondensation, which occur at 300 and 400 °C. Volatilization is terminated during heating; thus, additional soaking time is meaningless and reduces the process efficiency. Soaking time is a major variable when the synthesis temperature exceeds 400 °C. The byproduct is generated through volatilization; thus, its chemical characteristics are only influenced by the reaction temperature. The byproduct consists of various polycyclic aromatic hydrocarbons. The average molecular weight and yield of the byproduct increase with the reaction temperature. Carbon black was synthesized using chemical vapor deposition from the byproduct. The particle size of carbon black was controlled by the used precursor (byproduct), and the electrical conductivity of prepared carbon black has a maximum of 58.0 S/cm. Therefore, carbon black, which is synthesized from the byproduct of pitch synthesis, is expected to be used as a precursor for conductive material used in lithium-ion batteries or supercapacitors.