aims: Synthesis of organic-inorganic hybrids as 3D adsorbents for heavy metal removal background: Synthesis of organic-inorganic hybrids objective: Study of heavy metal removal with porous nanocomposite scaffolds based on hybrid organic/inorganic nanoparticles (MSN@COF) method: Using soluthermal methods for the synthesis of organic-inorganic hybrids and studying the removal of heavy metals in them result: Precise and defect-free synthesis of organic-inorganic hybrids Removal of over 90% of heavy metals conclusion: In this research work, in order to achieve the desired product, mesoporous silica nanoparticles were first synthesized based on TEOS, and then the surface modification of these nanoparticles was done with APTES in order to achieve MSN-NH2. Next, organic covalent frameworks based on cyanuric chloride were synthesized. The main goal in this research work was the synthesis of porous nanocomposites based on MSN and COF, so that it is possible to synthesize hybrid organic/inorganic porous nanocomposites by in situ growth of COF on porous silica nanoparticles. Therefore, after synthesizing both hybrid organic/inorganic porous nanocomposites (COF and MSN) and examining their morphology and how to identify them, porous nanocomposites (MSN@COF) resulting from the growth of COF on MSN were synthesized. To achieve a proper comparison of the porosity and nature of these nanocomposites, once this nanocomposite was synthesized using MSNs whose surfactant was not removed, the CTAB surfactant was removed after COF growth on it. In another synthesis, the nanocomposite was synthesized from the growth of COF on MSN-NH2 whose surfactant was removed. This nanocomposite, due to the open pores of the MSNs, the growth of COF started by connecting to the amino groups obtained from APTES from within the MSN-NH2 themselves. The nanocomposite had less porosity than the other composite due to the growth of COF inside it. But the remarkable thing was the growth and presence of COF with its constituent atoms inside the MSN cavities. Due to the fact that porous nanomaterials have their own unique morphology, nature, function, and application according to their constituents and porosity category, both porous nanoparticles used in the preparation of these nanocomposites are well-known and widely used porous nanomaterials. They are in industry and medicine, so we decided to synthesize porous nanocomposites that have the special characteristics, behavior, and ability of both MSN and COF. Relevant analyses confirmed the synthesis of these porous nano absorbents. The growth of COF on MSNs, according to the data obtained from BET, has reduced the surface area and volume of pores in porous nanocomposites, but on the other hand, the presence of COF with its constituent atoms definitely gives a special characteristic and ability to nanocomposites. Porous materials will give in exchange for a decrease in the surface area and volume of the initial MSN cavities. The results of this study demonstrated that MSN@COF(WC) absorbs a higher percentage of zinc and cadmium metal ions than other adsorbents at various levels of adsorbent consumption, demonstrating that hybrid adsorbents are more effective than COF and MSN in removing these heavy metals from the primary solution. Also, the evaluation of the equilibrium time showed that the adsorption of heavy metals zinc and cadmium by MSN, COF adsorbents has a greater speed, while the MSN@COF(NC) hybrid adsorbent needs the greatest time to reach equilibrium conditions. When hybrid absorbents and two other absorbents were compared at various pollution levels, it became clear that hybrid absorbents at low pollution levels and other absorbents at high pollution levels are more effective in removing metals heavier than the original solution. In conclusion, the results of this study showed that the hybrid adsorbents have a larger absorption amount and the other two adsorbents have a higher absorption speed to reach equilibrium conditions in the process of removing zinc and cadmium metals from the stock solution. other: All the necessary information is available inside the text.