1. A device (1) for the selective granulometric separation of solid powdery materials, using centrifugal action, capable of separating the materials into two fractions, a fine material fraction and a coarse material fraction, comprising:
a housing (6);
a cylindrical rotor (2) which is rotatable relative to said housing on a vertical axis, internal to said housing, provided with blades (3) distributed over the periphery of said rotor (2);
means for supplying into said housing (6) a gaseous flow entering through said blades (3) into said rotor (2);
a set of vanes (7), internal to said housing (6) and surrounding said rotor (2), fixed with respect to said housing and optionally orientable, disposed coaxially facing the blades (3) so that said incoming gaseous flow passes through them;
means (8) for introducing the solid materials to be sorted into said housing (6), between the vanes (7) and said rotor (2);
an outlet (9) of the rotor (2), to enable said gas flow and the fine entrained materials to be discharged;
collection means (10), below said rotor (2), for the coarse non-entrained materials that fell, said collection means (10) comprising a peripheral fluidised bed system, the bed of which extends around the axis (A) of the rotor (2), at least below said cylindrical rotor, at least below said vanes (7) and the gap lying between said blades (7) and the rotor (2), the speed of the fluidisation gas in a horizontal section of the fluidised bed being less than 1 ms so as to produce a further separation between the fine materials and the coarse materials in which said fine materials are returned into the gap between said vanes and said rotor, said peripheral fluidised bed system comprising a trough (11) forming a peripheral conveyor, the bottom of said conveyor having air blowing means (16, 17, 18); and
a means for pouring the materials collected in said trough into one or more collectors (22).
2. The device according to claim 1, wherein the peripheral conveyor consists of a set of straight channels, put end to end, in a polygonal configuration.
3. The device according to claim 1, wherein the blowing means take the form of a porous wall (18), defining the bottom of said trough (11), downstream of a plenum chamber (17) provided with a gas supply (16).
4. The device according to claim 1, wherein a plurality of nozzles are distributed on the bottom of said trough, downstream of a plenum chamber provided with a gas supply.
5. The device according to claim 1, wherein said one or more collectors (22) discharges the material by means of a handling device (23).
6. The device according to claim 1, wherein the speed of the fluidisation gas in a horizontal section of the fluidised bed is between 30 and 50 mms.
7. The device according to claim 1, wherein said means of supplying a gaseous flow are formed by said housing (6) and a vertical sheath (5) extending said housing downwards, the housingvertical sheath assembly enclosing, from bottom to top, said collection means (10) and the vane (7)cylindrical rotor (2) assembly.
8. The device according to claim 1, wherein,
said means of supplying a gaseous flow are formed by said housing (6) that surrounds the vane (7)cylindrical rotor (2) assembly, with the exception of said collection means (10), the gas supply taking place laterally, and
said vanes (7) representing the lateral surface of a virtual cylinder coaxial with the axis (A) of said cylindrical rotor, the volume defined between the internal wall of said housing (6) and the lateral surface of said virtual cylinder forms a spiral.
9. The device according to claim 8, wherein said housing (6) forming the external wall of the spiral has a double inclination with a lower wall section (64) inclined by an angle with respect to the horizontal greater than or equal to 30\xb0 and a vertical upper wall section (65).
10. The device according to claim 8, wherein rotor driving means are positioned lower than said rotor.
11. The device according to claim 1, wherein the outlet (9) is higher than the rotor (2), arranged with respect to said means for supplying a gaseous flow so as to generate an ascending gas flow inside said rotor (2).
12. The device according to claim 2, wherein the blowing means take the form of a porous wall (18) defining the bottom of said trough (11), downstream of a plenum chamber (17) provided with a gas supply (16).
13. The device according to claim 2, wherein a plurality of nozzles are distributed on the bottom of said trough, downstream of a plenum chamber provided with a gas supply.
14. The device according to claim 9, wherein rotor driving means are positioned lower than said rotor.
15. The device according to claim 3, wherein the porous wall is a fabric.
16. The device according to claim 5, wherein the handling device is selected from the group consisting of an airslide, an Archimedes screw, a chain conveyor, a vibrating conveyor, and a belt conveyor.
17. The device according to claim 12, wherein the porous wall is a fabric.
The claims below are in addition to those above.
All refrences to claim(s) which appear below refer to the numbering after this setence.
1. A process for forming a bulk hydroprocessing catalyst with minimal amount of metals to waste treatment, the method comprises:
co-precipitating at reaction conditions at least one of a Group VIB metal precursor feed and at least a Promoter metal precursor feed selected from Group VIII, Group IIB, Group IIA, Group WA and combinations thereof, to form a mixture comprising a catalyst precursor;
isolating the catalyst precursor from the mixture, forming a supernatant containing at least a Promoter metal residual and at least a Group VIB metal residual in a total amount of at least 10 mole % of the metal precursor feeds;
mixing the supernatant with at least one of an acid, a sulfide-containing compound, a base, and combinations thereof under mixing conditions at a temperature from ambient to 90\xb0 C. for a sufficient amount of time to precipitate at least 50 mole % of metal ions in at least one of the metal residuals, wherein the precipitation is carried out at a pre-select pH;
isolating the precipitate to recover a first effluent containing less than 50 mole % of metal ions in at least one of the metal residuals in the supernatant;
converting the metal ions in the precipitate or the first effluent into at least a metal precursor feed;
recycling the at least a metal precursor feed to the co-precipitating step; and
sulfiding the catalyst precursor forming the bulk catalyst.
2. The process of claim 1, wherein an effluent stream from the process to waste treatment contains less than 50 ppm metals.
3. The process of claim 1, further comprising drying the catalyst precursors at a temperature of at least 150\xb0 C. before the sulfidation step.
4. The process of claim 3, wherein the catalyst precursor is dried at a temperature of at least 325\xb0 C. for the catalyst precursor to have the formula (X)b(Mo)c(W)d Oz; wherein X is Ni or Co, the molar ratio of b:(c+d) is 0.51 to 31, the molar ratio of c:d is >0.011, and z=2b+6 (c+d)2.
5. The process of claim 2, wherein the catalyst precursor is dried at a temperature of at most 200\xb0 C. and wherein the catalyst precursor has the formula Av(MP) (OH)x (L)nyz (MVIBO4))wherein
A is at least one of an alkali metal cation, an ammonium, an organic ammonium and a phosphonium cation,
MP is selected from the group of Group VIII, Group IIB, Group IIA, Group IVA and combinations thereof, P is oxidation state with MP having an oxidation state of either +2 or +4 depending on the selection of MP,
L is at least a ligating agent L having an charge n<=0;
MVIB is at least a Group VIB metal having an oxidation state of +6,
MP: MVIB has an atomic ratio of 100:1 to 1:100;
v\u22122 +P*z\u2212x*z+n*y*z=0; and
0<y\u2266\u2212Pn; 0<x\u2266P; 0<v\u22662; 0<z.
6. The process of claim 1, wherein the supernatant is mixed with at least an acid selected from the group of sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, acetic acid, oxalic acid, nitric acid, and mixtures thereof
7. The process of claim 6, wherein the acid is nitric acid and the precipitation is carried out at a pH of less than 3.
8. The process of claim 7, wherein the at least one of a Group VIB metal precursor feed comprises Mo and W compounds and the first effluent stream comprising less than 1000 ppm each of Mo and W.
9. The process of claim 8, wherein converting the metal ions in the precipitate comprises dissolving the precipitate in an aqueous ammonium hydroxide solution, forming at least one of ammonium molybdate and ammonium tungstate as Group VIB metal precursor feeds.
10. The process of claim 1, wherein the at least a Promoter metal precursor feed comprises a Ni compound and wherein converting the metal ions in the first effluent stream comprises treating the first effluent stream with a base for a sufficient amount of time to precipitate the Ni compound, wherein the precipitation is carried out at a pre-selected pH.
11. The process of claim 10, wherein the pre-selected pH is at least 7.
12. The process of claim 11, further comprising isolating and recovering the precipitate for a second effluent stream containing less than 20 ppm of Ni.
13. The process of claim 1, further comprising:
treating the first effluent in a reactor vessel having a plurality of electrodes having a positive or a negative charge provided by a power supply, and wherein the electrodes react with at least one of the metal residuals, forming a slurry containing insoluble metal compound;
recovering the insoluble metal compound from the slurry, forming a second effluent containing less than 2000 ppm of at least one of the metal residuals.
14. The process of claim 13, further comprising:
adding to the second effluent stream at least an additive selected from the group of an acid, a sulfide-containing compound, a base, and combinations thereof, under mixing conditions for a sufficient amount of time to precipitate at a first pre-selected pH at least a portion of at least one of the metal residuals, generating a third effluent stream containing less than 1000 ppm of metal ions in at least one of the metal residuals.
15. The process of claim 1, further comprising:
treating the first effluent with an exchange resin for a sufficient amount of time for at least 50 mole % of metal ions in at least one of the metal residuals in first effluent to be bound onto the resin, forming a second effluent stream containing unbound metal residuals.
16. The process of claim 15, further comprising:
eluting the resin to produce an eluate stream containing the metal ions previously bound onto the resin;
treating the second effluent stream or the eluate stream to recover at least 80 mol % of the metal ions in the stream to form at least a metal precursor feed;
17. The process of claim 16, wherein at least 80 mole % of metal ions in the second effluent stream is recovered by adding to the second effluent stream at least one of an acid, a sulfide-containing compound, a base, and combinations thereof, under mixing conditions for a sufficient amount of time to precipitate at a first pre-selected pH at least a portion of at least one of the metal residuals, generating a third effluent stream containing less than 1000 ppm of metal ions in at least one of the metal residuals.
18. The process of claim 1, further comprising:
running the first effluent through a filtering system having a plurality of filter having a successive decrease in sizes, forming a second effluent containing less than 2000 ppm of metal ions in at least one of the metal residuals.
19. The process of claim 1, wherein an effluent stream from the process to waste treatment contains less than 50 ppm of Group VIB and Promoter metals.
20. In a process for forming a bulk hydroprocessing catalyst, the process comprising: co-precipitating at reaction conditions at least a Group VIB metal precursor feed and at least a Promoter metal precursor feed selected from Group VIII, Group IIB, Group IIA, Group IVA and combinations thereof, to form a mixture comprising a catalyst precursor; isolating the catalyst precursor from the mixture, forming a supernatant containing at least a Promoter metal residual and at least a Group VIB metal residual in an amount of at least 10 mole % of the metal precursor feeds; calcining the catalyst precursor to form a catalyst precursor of the formula (X)b(Mo)c(W)d Oz; wherein X is Ni or Co, the molar ratio of b:(c+d) is 0.51 to 31, the molar ratio of c:d is >0.011, and z=2+6 (c+d)2; and sulfiding the catalyst precursor forming the bulk catalyst, the improvement comprising:
mixing the supernatant with at least one of an acid, a base, and combinations thereof under mixing conditions at a temperature from ambient to 90\xb0 C. for a sufficient amount of time to precipitate at least 50 mole % of metal ions in at least one of the metal residuals, wherein the precipitation is carried out at a pre-select pH;
isolating the precipitate to recover a first effluent containing less than 20 mole % of metal ions in at least one of the metal residuals in the supernatant;
dissolving the precipitate with at least a base to convert the metal ions in the precipitate into at least a metal precursor feed; and
recycling the at least a metal precursor feed to the co-precipitating step.
21. The process of claim 20, further comprising:
treating the first effluent in a reactor vessel having a plurality of electrodes having a positive or a negative charge provided by a power supply, and wherein the electrodes react with at least one of the metal residuals, forming a slurry containing at least a precipitate;
isolating the precipitate from the slurry to recover a second effluent containing less than 5000 ppm of metal ions in at least one of the metal residuals.
22. The process of claim 21, further comprising:
adding to the second effluent stream at least an additive selected from the group of an acid, a sulfide-containing compound, a base, and combinations thereof, under mixing conditions for a sufficient amount of time to precipitate at a first pre-selected pH at least a portion of at least one of the metal residuals, generating a third effluent stream containing less than 1000 ppm of metal ions in at least one of the metal residuals.
23. The process of claim 20, wherein the supernatant is mixed with at least an acid selected from the group of sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, acetic acid, oxalic acid, nitric acid, and mixtures thereof for a pre-select pH of less than 3.
24. The process of claim 20, wherein the at least one of a Group VIB metal precursor feed comprises Mo and W compounds and the first effluent stream comprising less than 1000 ppm each of Mo and W.