The purpose of this study is to optimize the processing conditions (temperature, pressure, process time, yield rate) for the conversion of biomass to a high-energy density biofuel. The hydrothermal polymerization (HTP) catalytic process has been developed for production of biofuel via hydrothermal processing using an acid-based catalyst. This study has shown that the HTP catalytic process for a reference feedstock lowered the temperature by 10 to 40 °C, reduced the pressure requirement by 1 to 2 MPa, increased the rate of yield by 22%, and shortened the total processing time by up to 3 h when compared to the conventional hydrothermal carbonization (HTC) process. FTIR spectrum analysis of the HTP catalytic biofuel has shown that lignin in the biomass is preserved, while the pure HTC process destroyed the lignin in the biomass. GC/MS analysis of the process liquid determined the changes of the intermediate soluble components as a function of time. By measuring the 2,5-hydroxymethyl furfuralde concentration in solution, an endpoint determination could be made. This study also determined the approximate analysis of the HTP biofuel from various organic wastes such as cotton, cow manure, wood waste, paper waste, sugarcane bagasse waste, and food waste.