The microfiltration process of wastewater containing high concentration of nickel ion was studied with a ceramic membrane of pore diameter 0.5 mm, and poly(acrylic acid) sodium (PAAS)-enhanced ultrafiltration used for advanced treatment of the permeation fluid of microfiltration process. The effects of mass ratio of PAAS to metal (rp/m) and pH value on membrane flux (J) and nickel rejection coefficient (RNi) were examined. Furthermore, ultrafiltration concentration, decomplexation, washing and reuse of PAAS were also studied. The results showed that in the process of microfiltration concentration, J decreased sharply first, then declined slowly, and finally decreased rapidly at pH 9. RNi was close to 1. When volume concentration factor increased from 1 to 10, nickel ion concentration in the retentate (Cr) increased from 5562.71 to 55507.76 mg/L, whereas nickel ion concentration in the permeate (Cp) remained about 13.26 mg/L. In the process of PAAS-enhanced ultrafiltration, J did not change with increasing of rp/m, and increased with pH value. RNi increased with rp/m or pH value. The ultrafiltration concentration experiment was carried out at pH=9 and rp/m=9. RNi was close to 1. Cr increased linearly, whereas Cp remained about 0.05 mg/L. The decomplexation experiment was done at pH=3 with the previous concentrated solution. It took 9 min to reach the decomplexation equilibrium. The decomplexation rate of nickel(II)-PAAS complex reached 81.9%. The washing experiment was done with the hydrochloric acid solution of pH=3. Nickel ion removal rate of 98.8% was obtained. After the washing process, the regenerated PAAS was recycled, and still had a good complexation capacity.