Cellulose nanocrystals (CNC) was successfully extracted from natural Calotropis gigantea fiber (CGF) by a combined ball milling defibrillation and SO₄²⁻/TiO₂ nano-solid superacid catalyst-assisted method. In the extraction process, natural Calotropis gigantea fibers were defibrillated layer by layer, subsequently, catalysis degraded by nano-solid superacid catalysis. The new extraction method avoids large amounts of acid pollution. The yield of CNC obtained from Calotropis gigantea fiber was 55.37 %. Rod-like CNC with an average length of 242.06 nm and width of 8.80 nm was obtained. The aspect ratio of the CNC (the length:width) was 27.5 times. The green method avoids the use of large amounts of sulfuric acid. The ball milling defibrillation combined with SO₄²⁻/TiO₂ nano-solid superacid catalyst-assisted provides an efficient and sustainable manner to make full use of natural Calotropis gigantea fiber resources.

通过球磨除颤和SO ₄ ^2- / TiO ₂纳米固体超强酸催化剂辅助方法，成功地从天然Calotropis gigantea纤维（CGF）中提取了纤维素纳米晶体（CNC）。在萃取过程中，天然Calotropis gigantea纤维逐层除颤，随后被纳米固体超强酸催化降解。新的提取方法避免了大量的酸污染。从Calotropis gigantea获得的CNC产量纤维为55.37％。获得平均长度为242.06nm且宽度为8.80nm的棒状CNC。CNC的纵横比（长度：宽度）是27.5倍。绿色方法避免了使用大量硫酸。球磨除颤结合SO ₄ ^2- / TiO ₂纳米固体超强酸催化剂辅助，提供了一种有效且可持续的方式，可以充分利用天然Calotropis gigantea纤维资源。