Grouting materials are used frequently in grouting reinforcement projects, such as mining and coastal engineering. Double liquid grouting materials are mostly used because of the fast setting and high early strength properties when the two slurries are mixed together but high fluidity when the two slurries are separated. In our study, double liquid grouting materials were developed from CSA cement (slurry A), quicklime and fluorgypsum (slurry B). Aluminum sulfate was added in slurry B in order to counteract any adverse effects caused by the fluorgypsum, such as the decreased early compressive strength and the prolonged setting time. The effects of aluminum sulfate content and the quicklime/fluorgypsum ratio on the setting time, hydration heat, and compressive strength of the double liquid grouting materials were investigated, and the hydration products were characterized through thermogravimetry-differential thermal analysis (TG-DTA), X-ray Diffraction (XRD), and Scanning Electron Microscope (SEM) tests. The results show that the addition of aluminum sulfate can shorten the setting time and increase compressive strength at both early and later ages. Considering the setting time and compressive strength of double liquid grouting material at the same time, the optimum content of aluminum sulfate was found to be 2%, and the optimum ratio of quicklime/fluorgypsum was found to be 2:8. The values of the optimum content of aluminum sulfate and ratio of quicklime/fluorgypsum were verified from theoretical analysis.