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Nowadays, using fly ash for zeolites production has become a well-known strategyaimed on sustainable development. During zeolite synthesis in a hydrothermal conversion largeamount of post-reaction solution is generated. In this work, the solution was used as a substratefor Na-A and Na-X zeolites synthesis at laboratory and technical scale. Obtained materials werecharacterized using particle size analysis, X-ray diffraction (XRD), X-ray fluorescence spectroscopy(XRF), transmission electron microscopy (TEM), Fourier transformed infrared spectroscopy (FTIR),and nitrogen adsorption/desorption isotherm. Produced zeolites revealed high purity (>98%) andmonomineral zeolitic phase composition. The SiO2content was in the range 39–42% and 40–38%,whereas Al2O3content was 23–22% and 25–26% for Na-X and Na-A, respectively. TEM and BETanalyses revealed Na-X zeolite pores were almost identical to commercial 13X with SBETin therange 671–734 m2/g. FTIR indicated slight differences between materials obtained at laboratory andtechnical scale in Si-O-(Si/Al) bridges of the zeolitic skeleton. The results showed good replicability ofthe laboratory process in the larger scale. The proposed method allows for waste solution reusabilitywith a view to highly pure zeolites production in line with circular economy assumptions.