In this paper, the hydrolysis process of Dichlorohydroxytriazine (NHDT) under alkaline conditions are studied. A qualitative and quantitative method for the determination of HNDT and its hydrolysis products are established, which further clarified the hydrolysis mechanism of NHDT. Under alkaline conditions, the hydrolysis products are mainly compound 4, compound 6 and chloride (Cl−). The hydrolysis rate of NHDT at different NaOH concentration and temperature is studied. This research can be used to guide the high efficiency preparation of low fibrillation Lyocell fiber. According to the quantitative detection of wet abrasion numbers and the qualitative analysis of the fiber by SEM after slapping, it is concluded that the low fibrillation Lyocell fiber is less prone to fibrillation under the combined action of wet state and mechanical force. Due to hydrolysis of the unreacted second chlorine resulting in harmful products on the low fibrillation Lyocell fiber, the fibrillation propensity increased with the increase of storage time. The mechanical properties of low fibrillation Lyocell fiber prepared under different fiber states are studied. The tensile breaking strength of low fibrillation Lyocell fiber prepared in the form of sequentially arranged fiber bundles are better, which is closely related to the fiber surface.