Study On The Preparation Of C9 Petroleum Resin Hydrogenation Catalyst By Co-precipitation Method

The C9 petroleum resin obtained by simple polymerization is filled with a large number of unsaturated bonds and heteroatoms,resulting in poor resin quality.The heteroatoms can be removed through hydrogenation reaction and the valence bond structure can be saturated.Its use range and added value are greatly However,the current industrialization of hydrogenated C9 petroleum resin is restricted by hydrogenation catalysts,and further research and development are needed.This article will prepare Ni-based C9 petroleum resin hydrogenation catalyst by co-precipitation method,investigate the influence of preparation method,raw material and additive doping on the catalyst performance,and analyze it in combination with the evaluation results and characterization of H2-TPR,XRD,etc.,and screen out the optimal catalyst is used in industrial production.The effects of different preparation methods,precipitation reaction process enhancement and Ni source,carrier and precipitant on the performance of the catalyst were investigated.Spray mixing is preferred as the process enhancement method and co-precipitation method as the preparation method.The optimized co-precipitation method was used to investigate the influence of Ni source,carrier and other raw materials on the catalyst.The optimal raw material was Ni(NO3)2·6H2O,the carrier was Al2O3,and the precipitation agent was Na2CO3.The specific surface area of the optimal catalyst is 289.2 m2/g,the mesoporous pore diameter is 3.9 nm,the color of the hydrogenated resin after hydrogenation evaluation is No.0,the softening point,wax fog point and other properties are excellent,and the hydrogenation rate of the initial sample can reach 97.5%,the accelerated deactivation evaluation life of the catalyst is up to 20 days(the life is based on the chromaticity of the hydrogenated resin as 0,and the chromaticity is greater than 0 to determine the catalyst deactivation).The effects of different types of additives,additives doping amounts and doping methods on the performance of the catalyst were studied.Based on the characterization results,it is known that the appropriate amount of Cu doping is helpful to the formation and dispersion of active NiO.The preferred additive is Cu(Cu source is Cu(NO3)2·XH2O),the additive doping amount is 3%,and the optimal doping method is a mixed solution of Cu salt and Ni salt to participate in the precipitation reaction.The catalyst prepared under the above conditions is the best pilot catalyst.The content and dispersion of the reducible active NiO component in the best pilot-scale catalyst are significantly higher than those of the catalyst without additives.The resin hydrogenation rate can reach 98.5%,the catalyst deactivation life can reach 25 days,and the hydrogenation depth and the catalyst life is further improved.Based on the optimal small-scale test,the catalyst industrial scale-up production is carried out in a step-by-step amplification method.The initial amplification is 1500 times for the optimal small-scale test.The maximum magnification is determined to be 6000 times based on the equipment conditions,and the total volume of the reaction liquid is 4m3,the maximum output of a single kettle is 300 kg,and then explore the influence of various factors such as the feed time(the same feed amount but different feed speed),washing process,molding process,reduction and passivation and other factors on the catalyst in the industrial production of catalysts.The optimal feeding time is determined to be 6h(feeding speed is 0.3 m3/h),and the optimal forming process is 10%aluminum sol forming.When the pH of the slurry at the end of washing is 8?8.5,the catalyst performance is the best.Under this condition,the catalyst will accelerate the loss the life span is 18.5 days.Industrial applications Due to the large catalyst loading and low space velocity,the expected service life can reach more than 240 days.The current catalyst has been loaded and used for 60 days and runs smoothly,and the catalyst hydrogenation activity and hydrogenated resin performance can meet the requirements of industrial applications.