This study examined a novel approach for converting waste water hyacinths into high-value chemicals under low temperature and low atmospheric pressure by using iron (III) chloride (FeCl3), an oxidant that has the unique properties of nontoxicity, low-cost, and abundance. The conversion process and transformation products of water hyacinths under different conditions were investigated and characterized. The results showed that the content of lignocellulose gradually decreased in the reaction solution. The chemical structure of lignocellulose in the water hyacinths was changed, and the glycosidic bonds of the water hyacinths were cleaved. The surface structure and crystalline regions of the water hyacinths were also damaged during the reaction. Furthermore, the hemicellulose and cellulose in the water hyacinths were dissolved and hydrolyzed to reducing sugars in the reaction solution, and then the reducing sugars were further dehydrated to hydroxymethylfurfural (HMF) and furfural. Lignin in the water hyacinths was depolymerized into aromatic and hydrocarbon compounds. The process presented in this study effectively alleviates environmental pollution by efficient utilization of aquatic wastes, and it produces high-value chemicals from biomass waste.