The decolorization and mineralization studies were performed under direct solar light using suspension photo catalyst (titanium dioxide). Plenty of research has been done on synthetic compounds used in many industries since last few years, using both UV and visible light. However the use of Advanced Oxidation Processes (AOP's) for live industry effluents and direct solar energy was not studied intensely. Live industry effluent was taken from textile industry and characterized. The effluent was of a non-biodegradable nature besides having intense color and Chemical Oxygen Demand (COD). In this chapter, the optimization of the process has been studied by varying catalyst concentration, variation of pH, addition of oxidant, and treatment under solar irradiation as pre and post treatment to the existing biological treatment for maximum degradation. The analysis of the products by measuring COD, BOD, TSS, TS, TDS, pH, Color and absorbance has been done. The results showed 96% color removal and 90-92% COD reduction along with enhancing the biodegradability of the effluent. This increase in biodegradability favor for further treatment of this effluent into cost effective secondary processes (biological), which were otherwise unsuccessful in the treatment of this effluent. The catalyst used in slurry mode was effectively recycled for 4-5 times to get the reliable results. So the chapter suggests the pretreatment of difficult wastewater with the AOP's to facilitate its treatment in cost effective biological processes. Average solar intensity was 26-30 W/m(2)during the experiment.