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Cellulose fibres were isolated from corn peel agricultural waste using NaOH extraction and converted to carboxymethyl cellulose (CMC) by carboxymethylation using monochloroacetic acid (MCA) in alkaline conditions. A Box-Behnken statistical design was used to evaluate the parameters (soaking time with NaOH solution, soaking time with MCA solution, and reaction time with MCA) affecting the degree of substitution (DS) of CMC. Optimization was carried out by using the response surface method. The optimized conditions for CMC production with a maximal DS of 0.90 were soaking with NaOH for 118 min, followed by soaking with MCA for 6.5 h, and reaction with MCA at 60°C for 84 min. FTIR and XRD confirmed the successful carboxymethylation. This work demonstrates the feasibility of using corn peel agricultural waste as an alternative raw material for the production of CMC with high DS.