Preparation Of Oil-soluble MoS₂ And Evaluation Of Its Activity On The Slurry-bed Hydrocraking For Heavy Oil

Heavy oil slurry-bed hydrocracking technology is one of effective way of handling the heavy oil with high metal、high sulfur and nitrogen and high carbon residue,and it combines the feature of high liquid yield and adaptability,exploitation of catalyst is an important part in the key technology of slurry bed hydrocracking.In this thesis,one kind of armorphous phase was preparatted by liquid phase method,the optimum preparation condition was screened out by regarding Mo metal conversion rate as index,and the product was analysed by X-ray diffraction and X-ray photoelectron spectroscopy.Four modifiers CTAB and SDBS,Tx-100and PEG were added in the preparation process in order to inhibit growth and agglomeration of nanoparticles and improve the lipophilic type of molybdenum disulfide.Obtained T-MoS₂,S-MoS₂,P-MoS₂ and C-MoS₂ catalysts were analysed by characterizatting means of infrared spectrum,thermal weight,scanning electron microscope and transmission electron microscope,finally,the catalyst suitable for slurry bed was screened out.Slurry bed hydrocracking technology was simulated in autoclave in order to investigate hydrogenation activity of catalyst with taking Karamay atmospheric residue（KLAR）and Qingdao refinery catalytic cracking oil slurry（FCCS）as raw materials.The results of optimization of preparation process of MoS₂ showed that sodium molybdate,sodium sulfide and hydroxylamine hydrochloride as raw material,reduction reaction of preparation process,curing reaction and acidizing optimization of reaction process was optimizatted for the preparation,successively,Under the optimum reaction conditions molybdenum metal transformation rate reached 82.84%.The result of XRD analysis shows that the product of preparation was molybdenum disulfide of amorphous structure,and the result of XPS analysis shows that the Mo element mainly exists as Mo⁴⁺,the S element mainly exists as S^2-in the product.By lipophilic test,infrared spectrum analysis,thermal gravimetric analysis,scanning electron microscope and transmission electron microscopy analysis,four kinds of modified molybdenum disulphide lipophilicity was increased,particle size decreases,reunion between the particles improved,In combination with suspended bed catalyst development experience and characterization results,screened T-MoS₂ was screened slurry bed hydrocracking technology for the catalyst.The screened T-MoS₂ shows higher ability hydrogenation of coke inhibition in the atmospheric residue of Karamay,and decreased the wall phase and liquid phase after the reaction,and T-MoS₂ had higher ability of hydrogenation saturation for FCCS raw.Compared T-MoS₂ and molybdenum naphthenate catalyst hydrogenation activity,molybdenum naphthenate hydrogenation of coke inhibition ability was higher than ability of T-MoS₂,the light aromatics ability of heavy oil of T-MoS₂ catalyst was higher than ability of molybdenum naphthenate.