In this paper, cellulose nanocrystals (CNCs) were isolated from the cellulose extracted from cocoa pod husk waste, followed by characterization using XRD, FT-IR, TGA, SEM and TEM to determine its crystallinity, structural properties, thermal characteristics, morphology and dimensions respectively. The result revealed that the cocoa pod husk amorphous segments containing hemicelluloses and lignin were extensively removed with increasing chemical treatments leading to increased purity, crystallinity index and thermal stability of the extracted materials. The diameter, length and crystallinity index of the CNC isolated from the CPH are 10–60 nm, 41–155 nm and 67.60% respectively.

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The synthesis of mesoporous silica materials was reviewed with a view to discuss the reaction mechanism and the various attempts made at enhancing the materials' properties by utilizing varieties of templating agents and silica frameworks from pure synthetic chemicals. This chapter also reviewed studies in which either the template or the framework was synthesized from benign reagents obtained from renewable sources, to achieve enhanced material properties. The view was to encourage the development of mesoporous silica materials in which both the template and the silica framework are from biomass origin. This approach may promote the large-scales synthesis of mesoporous silica for commercial purposes, which had previously been hampered by the toxic nature, cost of synthetic chemical reagents, and unsustainable synthetic routes.