Process for preparing a transition metal-silicate catalyst

• US 4,591,579 A
• Filed: 12/05/1984
• Issued: 05/27/1986
• Est. Priority Date: 12/06/1983
• Status: Expired due to Term

• Current Assignee: Johnson Matthey PLC
• Original Assignee: Internationale Octrooi Maatschappij "Octropa" BV
• Inventors: Lok, Cornelis M., Ganguli, Keshab L.
• Primary Examiner(s): Dees, Carl F.
• Application Number:
  US06/678,798
• Time in Patent Office: 538 Days
• Field of Search: 502/244, 502/259, 502/260
• US Class Current: 502/244
• CPC Class Codes: B01J 21/08 Silica
• CPC Class Codes: B01J 23/72 Copper
• CPC Class Codes: B01J 23/74 Iron group metals
• CPC Class Codes: B01J 23/75 Cobalt
• CPC Class Codes: B01J 23/755 Nickel
• CPC Class Codes: B01J 35/392 Metal surface area
• CPC Class Codes: B01J 35/393 Metal or metal oxide crystallite size
• CPC Class Codes: B01J 37/031 Precipitation
• CPC Class Codes: C07C 209/48 by reduction of nitriles

Abstract

The invention provides a process for the preparation of a transition metal-silicate catalyst in which an insoluble, basic compound of a transition metal having an atomic number between 26 and 30 (in particular nickel which has an atomic number of 28) is rapidly precipitated with an alkaline precipitation agent from an aqueous solution of such a metal salt, as a suspension, which precipitate is allowed to mature for a longer period in a suspended form, and, after the transition metal ions have been practically completely precipitated, soluble silicate is added to the suspension, after which the solids are separated from the liquid, optionally washed, dried and reduced.

Claims

1. A process for the preparation of a transition metal-silicate catalyst in which an insoluble, basic compound of a transition metal having an atomic number between 26 and 30 is precipitated with an alkaline precipitation agent from an aqueous solution of such a metal salt, as a suspension, which precipitate is allowed to mature in suspended form and is subsequently separated, dried and reduced, wherein, after the transition metal ions have been practically completely precipitated, soluble silicate is added.

2. A process according to claim 1, wherein the transition metal has atomic number 28 (nickel).

3. A process according to claim 1, wherein the soluble silicate is added to the suspension within 15 minutes after the precipitation of the metal has been completed.

4. A process according to claim 1, wherein the soluble silicate is added in an amount of 0.1 to 0.6 moles, preferably 0.2 to 0.4, of silicate per mole of metal in the suspension.

5. A process according to claim 1, wherein the added silicate is alkali silicate.

6. A process according to claim 5, wherein the added alkali silicate is sodium silicate.

7. A process according to claim 6, wherein the added alkali silicate is neutral sodium silicate (Na₂ O.3SiO₂).

8. A process according to claim 1, wherein the maturing is carried our for a period of 5 to 180 minutes, preferably between 10 and 90 minutes.

9. A process according to claim 1, wherein the maturing is carried out at a temperature lying between 60°

and about 105°

C., preferably between 70° and

90°

C.

10. A process according to claim 1, wherein the precipitation of the catalyst takes place within a period of between 0.1 second and 60 minutes, preferably between 0.2 sec. and 10 minutes.

11. A process according to claim 1, wherein the catalyst is dried by spray-drying.

12. A process according to claim 1, wherein, during the precipitation, stirring is carried out under input of mechanical energy of 5-2000 Watt per liter of solution.

13. A process according to claim 1, wherein the activation of the catalyst is carried out with the aid of hydrogen at a temperature between 150 and 500, preferably between 300°

and 450°

C.

14. A process according to claim 1, wherein the precipitation is carried out continuously by dosing a carrier suspension into an aqueous metal salt solution and an alkaline solution together in a small, vigorously rotating pump and thereafter pumping the suspension into one or more post-reactors.

15. A process according to claim 14, wherein two or more post-reactors are used, the temperature in the second and possibly following post-reactor being 5°

-15°

C. lower than that in the first post-reactor.

16. A transition metal/transition metal silicate catalyst, which contains 30 to 70% of active metal, calculated on the total weight of the catalyst, wherein the active metal surface area is between 100 and 160 m² /g in the case of nickel and between 1 and 25 m² /g in the case of cobalt and copper, and wherein the BET total surface area and the pore volume are at least 20% higher and the filtration speed from the hydrogenated mixture is at least 5×

that of a co-precipitated catalyst of the same composition.