Alumina (Al
2
O
3
) extraction from circulating
fluidized bed (CFB) fly ash (CFBFA) is one of the most important pathways
for value-added utilization. However, in CFBFA, impurity iron (Fe)
normally coexists, resulting in complicated separation processes,
low Al
2
O
3
extraction efficiency, and substandard
Al
2
O
3
-based products. How to remove Fe impurity
effectively from CFBFA has become an important issue. For an effective
Fe removal from CFBFA, spinel ferrite transformation by carbothermal
reduction at a low temperature was discussed in the paper. The effects
of the reduction temperature and reduction time on the removal efficiency
of Fe and the recovery of aluminum (Al) as well as the removal of
other metals were systematically investigated, and the transformation
mechanisms of Fe-containing phases were investigated by X-ray diffraction,
X-ray photoelectron spectroscopy, and a scanning electron microscope–energy
dispersive spectrometer. The results showed that Fe in CFBFA was present
in the form of weakly magnetic α-Fe
2
O
3
, leading to a Fe removal of about 17.1% after magnetic separation;
however, the recovery efficiency of Al reached 97.4%. Weakly magnetic
hematite (α-Fe
2
O
3
) could be converted
to strongly magnetic spinel-type ferrite (MFe
2
O
4
) after carbothermal reduction at 700 °C for 60 min, and the
Fe removal efficiency could reach 62.8% after magnetic separation;
however, the recovery of Al was 81.2%, which was decreased compared
to the recovery of Al under the condition without carbothermal reduction
treatment. However, the carbothermal reduction–magnetic separation
process did not have a major effect on the existing form and leaching
behavior of Al, Li, and Ga. Simultaneously, it could be observed that
some transition metal elements such as Mn, Cr, and so forth could
be enriched in spinel-type MFe
2
O
4
and removed
after magnetic separation, which also provided a way for transition
metal enrichment and extraction of transition metals from other tailings.