本實驗利用農業廢棄物-椰殼為原料，以氯化銅與硫酸亞鐵雙金屬觸媒作為活化劑，製備成高孔隙活性碳觸媒並應用於染料之降解。探討金屬活化劑(CuCl2/FeSO4)含浸對於活性碳觸媒於濕式氧化反應中甲基藍溶液中COD去除率之影響，利用溫度變化、雙氧水變化、活性碳變化及pH值變化探討反應條件對氧化效果之影響，研究中探討活性碳金屬比例濃度的不同對活性碳觸媒表面特性之影響。研究中發現以適當比例的金屬濃度及活化條件可有效控制活性碳的孔洞體積；而甲基藍之氧化效率則受系統中觸媒劑量與雙氧水濃度之影響甚鋸，觸媒劑量與雙氧水濃度越高其氧化效率越快，顯示活性碳的有效吸附及氧化處理為帶色染料廢水處理之重要關鍵。 The purpose of this investigation is to prepare the porous activated carbon catalyst for dye degradation with discarded coconut shells by using the copper chloride and iron sulfate as the chemical activation agent. The influent factors on the COD removal of methyl blue in oxidation were considered by reaction temperature, dosage of catalyst, and pH. The metal ratios of Cu to Fe strongly affect the pore properties and surface area of activated carbon. It also indicated the importance of dye adsorption capacity and activity of oxidation in wastewater treatment. It was found that optimum bimetal ratio dominated the pore volume of activated carbon. On the other hand, the increase in pore size and BET surface area on activated carbon benefited the methyl blue adsorption in carbon matrix and the dye diffusion in the pore structure. The efficiency of oxidation was mainly limited by the dosage of catalyst and the oxidant concentration. Increase of the dosage of catalyst and the oxidant concentration could increase the reaction rate of oxidation. It was concluded that the pore properties of activated carbon significantly affected the adsorption behavior of dye in carbon matrix, and the dosage of catalyst and the oxidant concentration played the important roles to determine the oxidation rate of dye in wastewater.