Hydrogenation of neoprene (CR) latex was carried out by utilization of diimide with boric acid as a catalyst. Various hydrogenation conditions were studied and the hydrogenation degree could reach 48.1%. The most effective ratio of hydrogen peroxide/hydrazine hydrate was 0.8. The hydrogenation degree increased with increasing the temperature, the amount of boric acid and hydrazine hydrate. However, it decreased as prolonging the reaction time. The gel content was also investigated. Microstructure of hydrogenated neoprene (HCR) was characterized by IR and 1HNMR.