Sulfonated polymers are used in the oil field for scale inhibition. In this study, Al-sulfonated polycarboxylic acid (Al-SPCA) hybrid nanoparticles (NPs) were prepared by taking an environmentally friendly approach. The particle size of these materials was controlled at approximately 80 nm by applying hydrothermal synthetic methods with urea as a slow-neutralization agent. Reaction parameters (e.g., concentration of salt solution, reaction time, urea concentration, and ionic strength) were investigated to optimize NP synthesis. The mobility of Al-SPCA hybrid NPs decreases dramatically in a 1% (wt/wt) KCl solution. With phosphinopolycarboxylic acid (PPCA) as a dispersant, NPs were well-suspended in a 1% KCl solution. Absorption of PPCA by hybrid NPs increases their negative surface charge and decreases particle deposition. The retention and flowback performance of hybrid NPs was compared with the neat-chemical-squeeze simulation in ground-core-column experiments. The results show that the slow release of sulfonated polymer from solid hybrid NPs in a porous medium may have potential inhibitor-treatment application in the oil field.