A pyrolysis process was used to prepare char from the coarse guard hair droppings from cashmere dehairing processes. Three preparation variables were examined in this study, namely the heating rate, holding temperature, and holding time. The morphological evolution from hair to char, char yield, and uptake of methylene blue by the resultant char were investigated. Different morphological structures were observed for the char, including lotus-type, honeycomb-like, solid, bamboo-like, gourd-shaped, hollow and fragment structures. Based on the Box–Benkhen Design, two quadratic models were developed to correlate the preparation variables on two responses of the yield and the uptake value of methylene blue for cashmere guard hair char. From the analysis of variance, the char yield from cashmere guard hair is significantly affected by holding temperature and time. The uptake value of methylene blue is significantly influenced by holding temperature, holding time, and quadratic terms of the heating rate and the holding temperature.