ABSTRACTAn alkali corn wet‐milling process was developed to evaluate the process as a method to produce high purity corn starch and coproducts with added value. Using a single hybrid (R1064 × LH59), the effects of alkali concentration (0.18–0.82% NaOH), time (29–61 min), and temperature (36–75°C) were investigated. Starch yield was not affected by steep time or temperature. Starch yield was optimal at 65.2% using 0.5% alkali. Increasing the concentration of alkali to 0.82% or decreasing it to 0.18% caused a decrease in starch yield of 8–10 percentage points. Other wet‐milling products (fiber, germ, and gluten) also were affected. Steep conditions of 0.5% NaOH, 60 min, and 45°C gave optimal starch yield. Comparisons between alkali and sulfur dioxide wet‐milling processes, using 1‐kg sample size, were performed on 10 commercial yellow dent corn hybrids. The alkali process averaged 1.7 percentage points more starch than the sulfur dioxide process. Each hybrid had a higher starch yield when wet‐milled with the alkali method. Alkali wet‐milling produced pure corn starch with <0.30% protein (db).