Performance of wastewater treatement sludge-carbon (SC) can be evidently improved by removing the inorganic fractions. A novel investigation for recovery of Al from acid leaching of SC and synthesis of nano-Al(OH)(3) has been conducted. Results show that the sodium aluminates with high purity can be obtained by effectively dissolving the inorganic fractions from SC and by further removing the impurities (Fe(3+), Ca(2+), Mg(2+), S(4+), and P(3+)). Highly dispersed Al(OH)(3) with high S(BET) is obtained at pH = 6. The peaks of -CH(2)- vibration and the C1s peaks (binding energies of 284.6 eV) imply that polyethylene glycol 1000 (PEG-1000) is chemically adsorbed on the surface of Al(OH)(3) samples, which is propitious to reduce the hydrogen bonds between water molecules and surface -OH groups to prevent hard agglomeration. The stretching vibration peaks of [AlO(2)](-) and the Na1s peaks confirm that a trace of sodium aluminate (NaAl(OH)(4), Na(+)(H(2)O)(4)[Al(OH)(4)(-)], or the dehydrated monomers) is retained in the prepared Al(OH)(3). The main phase transformation for calcination (≤800 °C) of the SC-derived Al(OH)(3) is from amorphous Al(OH)(3) to amorphous A1(2)O(3). Here we highlight that production of Al(OH)(3) and SC from sludge provides the potential application in significant quantities that can revolutionize the handling of such kinds of harmful waste.