According to an embodiment, the pH of a diisocyanate composition and a diamine hydrochloride composition used in the preparation of an optical lens is adjusted to a specific range, whereby it is possible to enhance not only the yield and purity of the diisocyanate composition but also the optical characteristics of the final optical lens by suppressing the striae and cloudiness. Specifically, according to the process of the embodiment, the amount of an aqueous hydrochloric acid solution introduced to the reaction may be adjusted to control the pH of the diisocyanate composition to a desired range, thereby enhancing the yield and purity. Accordingly, the process for preparing a diisocyanate composition according to the embodiment can be applied to the preparation of a plastic optical lens of high quality.