In the paper,cassava starch was modified by two treatment with three sodium hexametaphosphate as crosslinking agent and acetic anhydride as esterifying agent. The first treatment was cassava starch was esterified after cross-linked. The second treat-ment was cassava starch was cross-linked after esterified. The cassava starch acetate were micronized treatment also. IR,SEM,XRD and TGA were used to characterize the synthetic product. The results show the ideal synthetic route of cassava starch acetate is first esterified,then the cross-linked. Cassava starch can be refined effectively by mechanical ball milling,and particle size and morphol-ogy can be controlled by ball milling time. The test shows that the heat resistance,fine cross-linking and the crystallinity of cassava starch acetate are decreased,and cold viscosity increased but the heat viscosity decreased.%本文以三偏磷酸钠为交联剂，醋酸酐为酯化剂，采用先交联、后酯化，先酯化、后交联，两种方案对木薯淀粉进行改性，并对木薯淀粉醋酸酯进行微细化处理。利用IR、SEM、XRD和TGA对合成产物进行表征；并对其冷热粘度进行了研究。结果表明，理想合成路线为：先酯化，后交联合成交联木薯淀粉醋酸酯。通过机械球磨，能有效地将木薯淀粉颗粒微细化，并可通过球磨时间控制淀粉颗粒的粒度和形貌。测试表明，微细化交联木薯淀粉醋酸酯的耐热性下降、结晶度下降；冷粘度增高，但热粘度性质有所下降。
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