Despite increasing demand for dissolving pulps from raw material, production costs remain quite high compared to regular paper pulp. Research literature to date has focused on improving performance and quality but has not simultaneously explored how to improve yield, which typically falls below 35%. Dissolving pulp from bamboo, as a widely available, high-quality raw material, was investigated with dilute acetic acid pre-hydrolysis before cooking and cold caustic extraction prior to bleaching. It was found that dilute acetic acid in the pre-hydrolysis stage could speed up the degradation of hemicellulose in bamboo and improve the diffusion of the cooking liquor in bamboo fiber compared with hot-water treatment. The dissolving pulp from bamboo was produced with 93% α-cellulose, 90% ISO brightness, 959 mL/g viscosity, 5.23% xylans, and 0.17% ash. The overall yield on the basis of raw material was 37%, which was higher than other documented processes using other agents in prehydrolysis.