This study synthesised dissolving pulp (DP) from Terminalia catappa L. (TC) wood and oil-palm empty fruit bunches (EFB) Elaeis guineensis Jacq. using a pre-hydrolysis kraft (PHK) process followed by elemental chlorine-free (ECF) bleaching. TC : EFB blends of 9 : 1, 8 : 2 and 7 : 3 were pre-hydrolyses at 160 °C for 3 hr and kraft-cooked at 170 °C for 180 min using active alkali (AA) charges of 19–21 %. Increasing the EFB proportion improved yield retention, likely because its lower hemicellulose content reduced alkali-labile carbohydrate loss. The novelty of this study lay in the integrated severity–composition mapping of TC : EFB blends and in the direct comparison of conventional and peroxymonosulfuric acid (Psa)-assisted ECF bleaching sequences. The conventional D0–Ep–D1 sequence produced pulp with 79.90 ± 0.25 % ISO brightness, 86.79 ± 0.77 % α-cellulose and 10.63 ± 0.22 cP viscosity, insufficient for rayon-grade DP requirements. In contrast, the Psa–D0–Ep–D1 sequence increased brightness to 88.16–88.36 % ISO and α-cellulose to 93.94–95.02 %, pentosan content ranged from 2.56–2.77 %, while maintaining viscosity at 9.49-10.12 cP, corresponding to a degree of polymerisation of approximately 730–760. The 9 : 1 and 8 : 2 TC : EFB blends satisfied the SNI 938 : 2017 requirements for rayon-grade dissolving pulp (DP), whereas the 7 : 3 blend was borderline for α-cellulose content. These results demonstrate that Psa-assisted ECF bleaching effectively produces rayon-grade DP from mixed hardwood–agro-residue feedstocks, while preserving pulp viscosity within the required range.