Process for recovering base metals from used hydroprocessing catalyst
A hydrogenation treatment and catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that valuable metals cannot be recovered and catalysts cannot provide satisfactory And other issues
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Embodiment 1
[0113] Example 1 . The vacuum residue containing spent catalyst is processed in a microcoker and exposed to coking conditions of 850-950°F. Microcoker products include cracked gas streams, coke liquid product streams, and solid coke products. The coker liquid product stream is analyzed for metals, particularly molybdenum, nickel and vanadium. A single metal was not found either. The solid char product was similarly analyzed and determined to contain appreciable amounts of molybdenum, nickel and vanadium. The solid coke product was crushed in a ceramic ball mill to pass 100% through 325 mesh (44 μm), and then the ground sample was subjected to a pressure leaching test under the conditions taught in U.S. Patent Application Publication No. 2007 / 0025899A1, The contents of which are hereby incorporated by reference in their entirety. Molybdenum extraction was reported as 99.4%, nickel extraction was reported as 86.3%, and vanadium extraction was reported as 68.9%.
Embodiment 2
[0114] Example 2 : Vacuum residue containing spent catalyst was diluted with heavy naphtha at a solvent / resid volume ratio of 3 / 1. By separation in a centrifuge with a centrifugal force of 1600 g-force and a residence time of 2 minutes, 99.8% of the spent catalyst with a particle size below 10 microns was obtained.
[0115] The separated solids and asphaltenes (ie, 50 wt% asphaltenes in the feed) were heated to 950°F at atmospheric pressure with a residence time of 1 hour. The recovered solids (coke and catalyst) are ground or crushed to a particle size of about 1 micron to less than 50 microns, and the resulting crushed mass allows for metal recovery up to 99.8 wt% Mo and Ni. Specifically, the material is subjected to pressure leaching in ammonia solution to recover valuable metals such as Mo, Ni, V and other Group VA, VIA, VIIA and VIII metals.
Embodiment 3
[0116] Example 3 : The vacuum residue contains about 5 wt% MoS 2 and NiS catalysts. Using 2000 g-force and a residence time of 1 minute, the resid stream was contacted with heavy naphtha at a solvent / resid volume ratio of 2 / 1 to obtain a catalyst containing 99.9 wt% and 50 wt% virgin asphaltenes (based on Fresh feed to a hydrocracking unit, less than 1 wt%) of paste. The mash is processed in a microcoker and exposed to coking conditions of about 950°F. Products obtained from the microcoking operation included cracked gas stream (13 wt%), coke liquid product stream (26 wt%), and solid coke product (61 wt%). The solid coke product was analyzed and it was determined that the coke contained appreciable amounts of molybdenum, nickel and vanadium. The coke product was crushed in a ceramic ball mill to pass 100% through 325 mesh (44 μm), and then subjected to pressure leaching. Several trials were performed, and in each trial the extraction of molybdenum was over 99 wt%, nickel...
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Abstract
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