The developments of monolithic materials rapidly in nowadays hold an impressively strong position in separation science as well as in other areas of chemistry. In this research are presented functionalization of PolyHIPE monolithic materials by tris(2-aminoethyl) amine. Monolithic polymer supports and scavengers were synthesized via nucleophilic displacement of chlorine in poly(4-vinyl benzyl chloride-co-divinylbenzene) as PolyHIPE materials. Porous copolymers of DVB/DVB were prepared by emulsion templating using high internal phase emulsions (HIPEs) as precursors for monoliths. The properties of the final products synthesized were functionalized with an amino group, at a different ratio of amine/chloromethyl groups, in different time refluxed were explored. PolyHIPE functionalized with tris(2-aminoethyl)amine to yield a product with high degrees of conversion. The extent of the functionalization reactions was investigated by a range of qualitative and quantitative techniques: FTIR, CHN analysis, potentiometric measurements, and (BET) measurements have been performed.