Boric acid-containing B-10 is used in a nuclear reactor as a coolant and absorbs thermal neutrons generated during nuclear fission in the primary circuit. Boron-containing coolant water waste is generated from maintenance, floor drain, decontamination, and reactor letdown flows. There are two options for aqueous solution waste of boric acid. One is recycling and discharge through filtration, ion exchange, and reverse osmosis. The other is immobilization after evaporation and crystallization processes. The dry powder of boric acid waste liquid can be immobilized by cement, polymer, etc. Before the mid-1990s, concentrated boric acid waste was solidified with a cement matrix. To overcome the disadvantage of low waste loading of cement waste form, a method of solidifying with paraffin was adopted. However, paraffin solids were insufficient to be disposed of as final waste. Paraffin is a kind of soft solidified material and has low compressive strength and poor leaching resistance. As a result, it was decided as an unsuitable form for disposal. In KOREA, paraffin waste form was adopted for boric acid waste treatment in the 1990s. A large amount of paraffin waste forms about 20,000 drums (200 l drum) were generated to treat boric acid waste and were stored in nuclear power sites without disposal. In this study, we want to obtain high-purity boric acid waste by oxidizing and decomposing solid paraffin waste form through a boric acid catalytic reaction. In this reaction, paraffin is separated in the form of various by-products, which can then be treated through a liquid waste treatment device or an exhaust gas treatment device. The proper temperature for sample decomposition during the catalytic reaction was set through TGA analysis. Compositions of by-products and residues generated at each stage of the reaction could be analyzed to determine the state during the reaction. Finally, the boric acid waste powder was perfectly separated from paraffin waste form with disposable products through this pyrolysis process.