In this study, an approach for the preparation of heterogeneous acid catalysts based on asphaltenes isolated from vacuum residue is proposed. Varying the conditions for the sulfonation of asphaltenes made it possible to obtain materials with an acid value of 1.16 to 2.76 meq g–1 and a total sulfur content of 6.4 to 12.3 wt%. The samples obtained were characterized by acid-base titration, nitrogen adsorption, sulfur elemental analysis and transmission electron microscopy techniques, and were studied as potential acid catalysts in the ketalization reaction between glycerol and acetone. Sulfonated asphaltenes (SA) were characterized by a homogeneous distribution of sulfonic groups over the granule surface and an almost complete absence of a porous structure. The ketalization reaction in the presence of SA proceeded without intradiffusion restrictions; as a result of which, their activity was higher than for known heterogeneous catalysts. The most active SA sample (total acid value, 1.16 meq g–1) had an apparent activation energy of 18.0 kJ mol–1, which was lower than the value obtained for the zeolite BEA-40 (29–53 kJ mol–1) and the Amberlyst 36 resin (27 kJ mol–1), and was close to the value for the homogeneous p-TSA catalyst (14.5 kJ mol–1). The SA heterogeneous catalysts did not show any acid leaching and had no loss of activity after five catalytic cycles, with the total turnover number TON = 7247.
In this paper, we developed an effective method for purifying oil sludge using a sorbing electrochemical matrix and assessed the prospects of this method in comparison with conventional hydrocracking. We synthesized Ni-W supported hydrocracking catalysts with different morphology and studied their activity under various conditions, we compared the obtained catalysts with commercial catalyst SGK-5. We demonstrated that the introduction of a secondary mesoporous structure in the catalyst leads to an increase in the yield of light fractions to 52 wt.%. The possibility is demonstrated to obtain hydrocarbons from reservoir oil sludge, dispersed into an aqueous solution of detergent, by the method of low-temperature hydrogenation in sorbing electrochemical matrices. The obtained product was characterized by low viscosity, low content of transition metals (<320 ppm), and sulphur (<260 ppm).
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