Preparation Of C9 Petroleum Resin Catalyst By Impregnation Precipitation Method

With the continuous development of the domestic ethylene industry,the output of C9 distillate is increasing year by year.Polymerizing it into petroleum resin and then performing hydrogenation modification is currently the most economical treatment method.The core of increasing the added value of C9 petroleum resin lies in the performance of the h(?)drogenation catalyst.In this paper,the preparation process of the Ni-based petroleum resin hydrogenation catalyst prepared by the impregnation precipitation method is studied,and the influencing factors of the preparation process and the hydrogenation process are optimized and analyzed respectively.This article first explores the effects of different carriers on the activity of impregnation precipitation,and investigates the different treatments of macroporous alumina,magnesia,and diatomaceous earth as carriers,and also conducts research and testing on the different proportions and mixing methods of mixed carriers.Experiments have found that after the macroporous alumina support is calcined at 800? for 8 h,when the catalyst is prepared at an atomic ratio of 1:1 with nickel,the catalytic activity is excellent,and the C9 resin can be hydrogenated to zero color,and the resin is softened.Point 108.3? up to the standard.Other magnesia and diatomaceous earth carriers only meet the color index,but their softening point is as high as 120?,and the overall hydrogenation performance is not as good as that of treated alumina.Subsequently,the optimal carrier impregnation precipitation method was used to prepare the process,and the influence of different impregnation precipitation preparation conditions was analyzed.The influence of the impregnation precipitation temperature of 60?90? was explored.The precipitants were respectively NaOH,urea,and Na2CO3,and the forward direction was adopted.It is prepared by feeding,reverse feeding,parallel feeding,and parallel fluctuating feeding.After immersion and precipitation,the washing water quantity,washing time,washing temperature,and washing times are tested and analyzed.It is finally determined that soda ash is used as the precipitant,nickel nitrate and additives are prepared as a mixed salt solution,the reaction temperature is controlled to 80?,while the feed is fluctuated,the pH is controlled to fluctuate between 6 and 9 twice,and deionized water is used after the reaction.Wash 3 times at 60? with a volume ratio of 3:1.After drying the filter cake,it is roasted in a muffle furnace at 450? for 4 h,then shaped and reduced.A colorless C9 petroleum resin that can be obtained by hydrogenation.The influence of Mg,Ca,Sr,La and other additives on the preparation of catalysts by the impregnation precipitation method was explored.The additives were added before the roasting,impregnation and precipitation of the support,and the addition amount was from 1%to 5%.Finally,it was found that the promoter activity was Sr>Mg>La>Ca.The addition of Sr promoter before the impregnation and precipitation can increase the specific surface area and pore volume of the catalyst the most.When the addition amount of Sr is 3%,the specific surface area of the catalyst can be increased to 124.4 m2/g,the pore volume reaches 0.671 cm3/g.Finally,in this study,the catalyst molding formula and hydrogenation process conditions were extruded separately for molding agent 5-30%,water-to-powder ratio 0.4-0.65,nitric acid dosage 0-20%,sesame powder auxiliary agent 1-5%,etc.The strip is formed,the mechanical strength is tested,and the formula is determined:remember that the quality of the original powder is 100%,then add 20%SB powder,3%sesame powder,60%water,and 10%concentrated nitric acid.After molding,it can still maintain good catalytic activity,and the mechanical strength is greater than 80 N/cm.The main explorations for process optimization during catalyst hydrogenation include:resin concentration 10-40%,reaction temperature 220-280?,pressure 6-9 MPa,liquid space velocity 0.5-1.5 h-1,hydrogen-oil ratio 200-600,etc.factor.It is determined that the catalyst hydrogenation process C9 petroleum resin solution has a concentration of 20%,a temperature of 250?,a pressure of 9 MPa,a hydrogen-to-oil ratio of 300:1,and a space velocity of 0.9 h-1.Under these conditions,the long-term evaluation of the catalyst for 240 h can result in a good C9 resin with a color number of less than 1,a softening point of 100?,and a wax mist point of 70?.