Some Investigation Of Comprehensive Utilization Of Oil Shale Residue

Glass-ceramics, foam glass-ceramics and alumina were prepared with oil shale residue from shale oil factory as start material. Crystallization phase identification, microstructure and functional group of bond were analyzed by modern test technique XRD,SEM and FT-IR.Firstly, decorative glass-ceramics with high value-added and low-cost were made from oil shale residue adopting sintered method. Compositions of glass-ceramics and selection of main crystallization and nucleating agents were discussed. Utilizing the orthogonal experiment, the optimal heat treatment schedule of glass-ceramics was decided. The results showed that composite nucleating agents(TiO2+P2O5) can efficiently induced crystallization. The optimal heat treatment showed as follows:the nucleating temperature was 850℃and held for 100min, and the crystallization temperature was 980℃and held for 80min. The main crystallization phase of the glass-ceramics was hedenbergite, and anorthite was the minor crystallization phase. These crystals formed fibrous structure and complected one another. The effect of each heat treatment factors on the properties and microstructure of glass-ceramics was discussed. With increasing of heat treatment temperature, the results showed that the crystal size and crystallization rate increased first, then decreased and finally ascended. The micro-hardness and compressive strength had the same variational trend. It further confirmed the optimal heat treatment schedule at the same time. The crystallization process of glass-ceramics was investigated. With increasing of heat treatment temperature, the results showed that the FT-IR absorption bands appeared obvious split. The aluminum-oxide polyhedron in the glass network was changed from [AlO4] to [AlO6] and played break network role in promoting crystallization. The titanium ion in the network was gradually transformed from 4-coordinated to 6-coordinated, moreover formed nanometer spherical grain of MgTi2O5 and Fe2TiO4 which provided the position of heterogeneous nucleation for the growth of crystal.Secondly, foam glass-ceramics were prepared with oil shale residue using powder sintered process. Components of foam glass-ceramics and selection of additives were discussed. The effect of various factors on the properties of foam glass-ceramics was analyzed. Utilizing the orthogonal experiment, the optimal formula and heat treatment schedule of foam glass-ceramics were decided. The results showed that the optimal content of foaming agent calcium carbonate, stabilizing agent sodium phosphate and flux borax were 4%,6% and 4% respectively. The optimal process of heat treatment showed as follows:the foaming temperature of 1080℃, the foaming time of 15min, and the heating rate of 14℃/min. Foaming agent and temperature had greatest effect on the properties of foam glass-ceramics. The foaming and crystallization process of samples were completed after heat treatment including preheating, sintering, foaming, stabilizing and annealing process. In addition, the foaming process demanded higher temperature and held in a short time.Finally, alumina was prepared through acidic leaching method with oil shale residue as start material. The effect of activated roasting, leaching temperature, the dosage of hydrochloric acid and leaching time on the extraction rate of alumina was discussed. The results showed that alumina was able to extract by acidic leaching from oil shale residue which did not need activation. The optimal process conditions showed as follows:the dosage of hydrochloric acid and oil shale residue were 40.0mL and 15.0g respectively, and the treated condition was at 100℃for 2.0h. The extraction rate and purity of alumina were 90.6% and 91.7% respectively.