This paper presents a study on the removal of azo dyes [Methyl Orange (MO) and Trapaeolin 000 (TP)] from aqueous solution using new phthalonitrile and isoindoline substituted calix[n]arene derivatives into the organic phase in order to explore the potential use of these calixarenes as low-cost efficient extractants for removal of these azo dyes from wastewater. The effect of NaCl concentration, contact time, and pH on the extraction of these azo dyes was also investigated for all calixarene derivatives. The stoichiometric ratio between the calixarene derivatives (5 and 6) and selected azo dyes (MO and TP) was estimated through job's plot.