US 7,837,960 B2 · Process for separating and recovering base metals from used hydroprocessing catalyst

Abstract

A method is disclosed for separating and recovering base metals from a used hydroprocessing catalyst originating from Group VIB and Group VIII metals and containing at least a Group VB metal. In one embodiment, the method comprises the steps of: contacting the used catalyst with an ammonia leaching solution under conditions sufficient to dissolve the group VIB metal and the Group VIII metal into the leaching solution; forming a leached slurry containing at least a group VIB metal complex and at least a group VIII metal complex, ammonium sulfate and a solid residue containing at least a Group VB metal complex and coke; separating and removing from the leached slurry the solid residue and coke; precipitating from the remaining solution at least a portion of the Group VIB metal complex and at least a portion of the Group VIII metal complex by controlling the pH to form a liquid material substantially free of Group VB, Group VIB and Group VIII metals and another solid material comprising substantially Group VIB and Group VIII metal complexes. Said solid material is further processed by dissolution, means of separation, further means of precipitation and oxidative dissolution to produce, separately, a Group VIB metal product solution, a Group VIII metal product solution and a purified ammonium sulfate product solution.

Claims30

Dependent claims

A method of recovering metals from a used catalyst comprising the steps of:

(a) leaching a Group VB metal, a Group VIB metal and a Group VIII metal from the used catalyst with an ammonia containing leach solution at a temperature and a pressure sufficient to form a pressure leach slurry comprising at least a Group VIB soluble metal complex and at least a Group VIII soluble metal complex and a first solid residue;
(b) separating and removing the first solid residue from the pressure leach slurry to form a first pressure leach solution comprising the Group VIB soluble metal complex and the Group VIII soluble metal complex;
(c) precipitating from the first pressure leach solution, at a first pre-selected pH, a second solid residue comprising at least a portion of the Group VIB soluble metal complex to form a first slurry comprising the second solid residue and at least a portion of the Group VIII soluble metal complex;
(d) separating from the first slurry the second solid residue and a primary filtrate substantially free of Group VB, Group VIB and the Group VIII metals;
(e) dissolving the second solid residue at a second pre-selected pH to form a group VIB metal precipitate and a group VIII metal containing solution;
(f) separating the group VIB metal precipitate from the Group VIII metal containing solution of step (e);
(g) dissolving said Group VIB metal precipitate in a dilute base at a sufficient temperature to form a Group VIB soluble metal product.

4 more elements

A method of recovering metals from a used catalyst originating from a hydroprocessing catalyst having a general formula (X)a(M)b[(CH3CH2)cN(CH3)3]dOz and containing at least a group VB metal, wherein X is a Group VIII non-noble metal, M is a group VIB metal selected from Mo and W and combinations thereof, c is an integer from 10 to 40, the molar ratio of a:b is from 0.5/1 to 3/1, the method comprising the steps of:

(a) leaching a Group VB metal, a Group VIB metal and a Group VIII metal from the used catalyst with an ammonia containing leach solution at a temperature and a pressure sufficient to form a pressure leach slurry comprising at least a Group VIB soluble metal complex and at least a Group VIII soluble metal complex and a first solid residue;
(b) separating and removing the first solid residue from the pressure leach slurry to form a first pressure leach solution comprising the Group VIB soluble metal complex and the Group VIII soluble metal complex;
(c) precipitating from the first pressure leach solution, at a first pre-selected pH, a second solid residue comprising at least a portion of the Group VIB soluble metal complex to form a first slurry comprising at least a portion of the Group VIII soluble metal complex;
(d) separating from the first slurry the second solid residue and a primary filtrate substantially free of Group VB, Group VIB and the Group VIII metals;
(e) dissolving the second solid residue at a second pre-selected pH to form a group VIB metal precipitate and a group VIII metal containing solution;
(f) separating the group VIB metal precipitate from the Group VIII metal containing solution of step (e) and dissolving said Group VIB metal precipitate in a dilute base at a sufficient temperature to form a Group VIB metal product.

3 more elements

A method of recovering metals, including vanadium, from a used catalyst having a general formula (Mt)a(Xu)b(Sv)d(Cw)e(Hx)f(Oy)g(Nz)h containing at least a Group VB metal, wherein M is at least one group VIB metal, X is at least one of a non-noble Group VIII metal, a Group VIIIB metal, a Group VIB metal, a Group IVB metal, and a Group IIB metal, 0=<b/a=<5, (a+0.5b)<=d<=(5a+2b), 0<=e<=11(a+b), 0<=f<=7(a+b), 0<=g<=5(a+b), 0<=h<=0.5(a+b);

t, u, v, w, x, y, z, each representing total charge for each of:
M, X, S, C, H, O and N, respectively;
ta+ub+vd+we+xf+yg+zh=0 the method comprising the steps of:
(a) leaching a Group VB metal, a Group VIB metal and a Group VIII metal from the used catalyst with an ammonia containing leach solution at a temperature and a pressure sufficient to form a pressure leach slurry comprising at least a Group VIB soluble metal complex and at least a Group VIII soluble metal complex and a first solid residue;
(b) separating and removing the first solid residue from the pressure leach slurry to form a first pressure leach solution comprising the Group VIB soluble metal complex and the Group VIII soluble metal complex;
(c) precipitating from the first pressure leach solution, at a first pre-selected pH, a second solid residue comprising at least a portion of the Group VIB soluble metal complex to form a first slurry comprising the second solid residue and at least a portion of the Group VIII soluble metal complex;
(d) separating from the first slurry the second solid residue and a primary filtrate substantially free of Group VB, Group VIB and the Group VIII metals;
(e) dissolving the second solid residue at a second pre-selected pH to form a Group VIB metal precipitate and a Group VIII metal containing solution;
(f) separating the Group VIB metal precipitate from the Group VIII metal containing solution of step (e) and dissolving said Group VIB metal precipitate in a dilute base at a sufficient temperature to form a Group VIB metal product;
(g) recovering a secondary filtrate comprising substantially the Group VIII soluble metal complex and a trace amount of Group VB and Group VIB metals;
(h) combining the secondary filtrate with the primary filtrate of step (d) to form a combined filtrate comprising substantially the Group VIII soluble metal complex and a trace quantity of Group VB and Group VIB metals;
(i) precipitating from the combined filtrate the Group VB, Group VIB and Group VIII metals in a sulfidation process to form a third solid residue and a tertiary filtrate;
(j) separating the third of solid residue from the tertiary filtrate and dissolving the third solid residue to form a Group VIII metal product solution.

10 more elements

Dependencies are inferred from the claim text.

Process for separating and recovering base metals from used hydroprocessing catalyst

Life of this patent

Process for separating and recovering base metals from used hydroprocessing catalyst

Life of this patent

Abstract

Claims30