The Al-rich waste with aluminium and hydrocarbon as the major contaminant is generated at the wastewater treatment unit of a polymer processing plant. In this research, the heat treatment of this Al-rich waste and its use to adjust the silica/alumina ratio of the high calcium fly ash geopolymer were studied. To recycle the raw Al-rich waste, the waste was dried at 110°C and calcined at 400 to 1000°C. Mineralogical analyses were conducted using X-ray diffraction (XRD) to study the phase change. The increase in calcination temperature to 600, 800, and 1000°C resulted in the phase transformation. The more active alumina phase of active θ-Al2O3 was obtained with the increase in calcination temperature. The calcined Al-rich waste was then used as an additive to the fly ash geopolymer by mixing with high calcium fly ash, water glass, 10 M sodium hydroxide (NaOH), and sand. Test results indicated that the calcined Al-rich waste could be used as an aluminium source to adjust the silica/alumina ratio and the strength of geopolymeric materials. The fly ash geopolymer mortar with 2.5wt% of the Al-rich waste calcined at 1000°C possessed the 7-d compressive strength of 34.2 MPa. The Al-rich waste with aluminum and hydrocarbon as the major contaminant is generated at the wastewater treatment unit of a polymer processing plant. In this research, the heat treatment of this Al-rich waste and its use to adjust the silica / alumina ratio of the high calcium fly ash geopolymer were studied. To recycle the raw Al-rich waste, the waste was dried at 110 ° C and calcined at 400 to 1000 ° C. Mineralogical analyzes were conducted using X-ray diffraction (XRD) to study the The increase in calcination temperature to 600, 800, and 1000 ° C resulted in the phase transformation. The more active alumina phase of active θ-Al2O3 was obtained with the increase in calcination temperature. The calcined Al-rich waste was then used as an additive to the fly ash geopolymer by mixing with high calcium fly ash, water glass, 10 M sodium hydroxide (NaOH), and sand. Test results indicated that the calcined Al-rich waste could be used as an aluminum source to adjust the silica / alu mina ratio and the strength of geopolymeric materials. The fly ash geopolymer mortar with 2.5 wt% of the Al-rich waste calcined at 1000 ° C possessed the 7-d compressive strength of 34.2 MPa.