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One of the current challenges is to add value to agro-industrial wastes, and the cocoa industry generates about 10 tons of cocoa pod husks in Colombia for each ton of cocoa beans, which are incinerated and cause environmental damage. This study characterized the Colombian cocoa pod husk (CPH) and to isolate and characterize cellulose microfibers (tCPH) extracted via chemical treatment and pressure. Chemical and physical analyses of CPH were performed, and a pretreatment method for CPH fibers was developed, which is followed by a hydrolysis method involving high pressure in an autoclave machine with an alkaline medium (6% NaOH), and finally, bleaching of the fiber to obtain tCPH. The tCPH cellulose microfibers were also chemically and physically analyzed and characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermo-gravimetric analysis (TGA). Chemical and physical characterization showed a decrease in lignin content in tCPH. FTIR analysis showed the absence of some peaks in tCPH with respect to the CPH spectrum; XRD results showed an increase in crystallinity for tCPH compared to CPH, due to a higher presence of crystalline cellulose in tCPH. SEM images included a control fiber treated without high pressure (tCPHnpe), and agglomerated fibers were observed, whereas cellulose microfibers with a mean diameter of 10 ± 2.742 μm were observed in tCPH. Finally, with TGA and DTGA it was confirmed that in tCPH, the hemicellulose and lignin were removed more successfully than in the control fiber (tCPHnpe), showing that the treatment with pressure was effective at isolating the cellulose microfibers from cocoa pod husk.