Hydroprocessing catalyst prepared with waste catalyst fines and its use
US-9211536-B2 · Dec 15, 2015 · US
US9861963B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9861963-B2 |
| Application number | US-201314132741-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 18, 2013 |
| Priority date | Dec 27, 2012 |
| Publication date | Jan 9, 2018 |
| Grant date | Jan 9, 2018 |
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A process for preparing a hydrocarbon conversion catalyst that comprises a specially made silica-alumina composition and a metal or metal compound selected from Group VIB and Group VIII metals. The silica-alumina composition is made by preparing an aqueous mixture containing aluminum sulfate followed by adding alkali metal aluminate to the mixture to inhance the pH to within specified range and then adding aluminum sulfate to the mixture to lower the pH. Then alkali metal silicate is added followed by several other pH swings to provide a mixture containing silica-alumina. The resulting mixture is treated with an alkaline solution to provide a precipitate solid that is recovered to obtain a silica-alumina composition containing of from 30 to 70% wt silica and of from 70 to 30% wt of alumina.
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That which is claimed is: 1. A process for preparing a hydrocarbon conversion catalyst, which process comprises: (a) preparing an aqueous mixture containing aluminum sulfate and having a pH in the range of from 1.0 to 6.5; (b) adding alkali metal aluminate to the mixture obtained in step (a) to increase the pH of the mixture to within the range of from 7.1 to 12; (c) adding aluminum sulfate to the mixture obtained in step (b) to lower the pH of the mixture to within the range of from 1.5 to 6.5; (d) adding alkali metal silicate to the mixture obtained in step (c) to increase the pH of the mixture to within the range of from 6.5 to 11, wherein the final steps of the preparation process are (v) adding aluminum sulfate to the mixture obtained in a process comprising steps (a)-(d) to lower the pH of the mixture to within the range of from 2 to 8; (w) adding alkali metal silicate to the mixture obtained in step (v) to increase the pH of the mixture, (x) adding to the mixture obtained in step (w) (i) alkali metal aluminate to change the pH of the mixture to of from 7.8 to 12 and (ii) aluminum sulfate to change the pH of the mixture to within the range of from 1.5 to 7.7, wherein step (i) can precede or succeed step (ii), (y) treating the mixture obtained in step (x) with an alkali metal hydroxide solution having a pH of from 7.5 to 12, (z) recovering a precipitate solid from the mixture obtained in step (y) to provide a recovered precipitate; (zz) washing with water the recovered precipitate and drying the recovered and washed precipitate by flash drying, belt drying or spray drying to obtain a dried silica-alumina composition containing of from 30 to 70% wt silica and of from 70 to 30% wt of alumina, and having a surface area of from 320 m 2 /g to 450 m 2 /g, and subsequently shaping the dried silica-alumina composition to provide a shaped silica-alumina composition, and compositing the shaped silica-alumina composition with one or more metals or metal compounds which metals have been selected from the group consisting of Group VIB and Group VIII metals to obtain a hydrocarbon conversion catalyst. 2. A process according to claim 1 , which preparation process further comprises (e) adding aluminum sulfate to the mixture obtained in step (d) to lower the pH of the mixture to within the range of from 1.5 to 7.0; and (f) adding alkali metal aluminate to the mixture obtained in step (e) to increase the pH of the mixture to within the range of from 7.5 to 12. 3. A process according to claim 1 , wherein the alkali metal aluminate is sodium aluminate. 4. A process according to claim 1 , wherein the alkali metal silicate is sodium silicate. 5. A process according to claim 1 , which process comprises calcining the dried silica-alumina composition at a temperature of from 600 to 850° C. 6. A process according to claim 1 , which shaping step includes mixing the dried silica-alumina with water and acid to provide an extrusion mixture and subsequently extruding the extrusion mixture to yield the shaped silica-alumina composition. 7. A process according to claim 6 , in which process the acid is an inorganic acid. 8. A process according to claim 1 , which process further comprises drying and/or calcining the shaped silica-alumina composition. 9. A process according to claim 8 , which process comprises calcining the shaped silica-alumina composition at a temperature of from 600 to 850° C. 10. A process for hydrocracking a hydrocarbonaceous feedstock, which process comprises contacting gaseous feedstock at a reaction temperature in the range of 250 to 500° C. and a total pressure at the reactor inlet in the range of from 3×10 6 to 3×10 7 Pa in the presence of hydrogen with a catalyst prepared by a process according to claim 1 in which the gaseous feedstock contains less than 150 parts per million by weight of ammonia. 11. A process according to claim 1 , wherein the silica-alumina composition obtained in step (z) has a surface area of from 330 m 2 /g to 420 m 2 /g.
Tungsten · CPC title
Precipitation; Co-precipitation · CPC title
Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst · CPC title
to form a gel or a cogel · CPC title
Silica and alumina · CPC title
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