HD -chitosan was produced with basic material -mantis shrimp shell which was removed inorganic salt with chlorhydric acid, proteins with dilute alkali solution, then dislodged acetyl group with concentrated alkaline solution. Next, the above -mentioned HD -chitosan was degraded with H2O2 for producing soluble COS. With adjusted conditions, the soluble COS was added to ferric chloride solution for complexing. It was confirmed by series of experiments that the optimized conditions of preparing HD-chitosan was 45%NaOH, the ratio of material to solvent(g/ml)1 : 300, and at constant temperature 85 ℃ for 9 h. The yield of HD-chitosan to chitin was 73.1%with other excellent quality index. The optimized conditions of preparing soluble oligosaccharide was 4.0% acetic acid, 4.0% H2O2 and at constant temperature 65 ℃ for 6 h. The viscosity average molecular weigh of products was 2.9 ku. In addition, it was also observed that the products of oligosaccharide was desirable faint yellow powder and had fine solubility. According to analysis of FT-IR and UV spectrum, the formation of soluble COS-Fe (Ⅲ) complex was certified.%以皮皮虾壳作基本原料，分别采用稀盐酸、稀碱溶液浸泡，除去虾壳中的钙质等无机质和蛋白等有机成分，以浓碱脱除甲壳素上的乙酰基，制得壳聚糖.再以其为原料，采用 H2O2氧化降解法得到水溶性壳寡糖.将所制水溶性壳寡糖加入到氯化铁溶液中，设定各项条件，使二者进行配位反应.经系列实验证实，得出制备高脱乙酰度壳聚糖最适宜条件为：温度85℃，时间9 h，NaOH 质量分数45%，料液比1：300.所得产品脱乙酰度为89.6%，收率（壳聚糖/甲壳素）为73.1%，其他各项指标也均为优良级.制备水溶性壳寡糖最适宜条件为：温度65℃，时间6 h，醋酸质量分数4.0%，H2O2质量分数4.0%，产品平均粘均分子质量为2.9 ku，外观为淡黄色粉末，溶解性能优良.通过对 FT-IR 和 UV 谱图的分析，证实了水溶性壳寡糖 Fe（Ⅲ）配合物的生成.
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