Starch nanocrystals (SNCs) are insoluble platelet particles with multifunctional properties. SNCs production is mainly based on acid hydrolysis of cornstarch with low yield. This study focuses on investigating the effect of pretreatments (heat‐moisture‐treatment [HMT], annealing [ANN], and sonication [SNT]) on unconventional pinhão starch to produce SNCs by acid hydrolysis to improve the yield and SNCs properties. All starches hydrolysis is described by a first‐order model reaction and shown two phases related at k values. The faster hydrolysis is from SNT (k = 0.61 day−1) and the slower one is at ANN (k = 0.40 day−1). Furthermore, the acid hydrolysis is described by a rapid (0–2 days) phase, followed by a slow phase lasing 3–7 days. The HMT increases the yield of the SNCs (14.7%) but promotes losses in the RC (47.34%) as compared with the native starch (yield 10.23%; RC 52.23%). The ANN improves crystallites perfection, protecting them from acid attack. The pretreatments allow pinhão starch to be used as promising feedstock to produce SNCs with good yield and RC. In addition, ANN can be useful to improve the thermal stability and SNT to speeding up the hydrolysis for SNCs production, while HMT can increase the hydrolysis yield.

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