Method of making pyrochlores

Patent metadata

Field	Value
Publication number	US-9126189-B2
Application number	US-201414311925-A
Country	US
Kind code	B2
Filing date	Jun 23, 2014
Priority date	Jul 11, 2013
Publication date	Sep 8, 2015
Grant date	Sep 8, 2015

Abstract

Disclosed is a method of making a pyrochlore comprising, obtaining a solution comprising a solvent and a metal precursor or salt thereof capable of forming a pyrochlore, wherein the metal precursor or salt thereof is dissolved in the solvent, subjecting the solution to a drying step to obtain a non-gelled or non-polymerized pyrochlore precursor material in powdered form, and subjecting the pyrochlore precursor material to a calcination step to obtain a pyrochlore.

First claim

The invention claimed is:

1. A method of making a pyrochlore comprising:
(a) obtaining a solution comprising a solvent and metal precursors capable of forming a pyrochlore, wherein the metal precursors are dissolved in the solvent;
(b) subjecting the solution to a drying step to obtain a non-gelled or non-polymerized pyrochlore precursor material in powdered form; and
(c) subjecting the pyrochlore precursor material to a calcination step to obtain a pyrochlore,
wherein a gelled or polymeric matrix is not formed in any of steps (a) to (c).

2. The method of claim 1 , wherein the solvent is water, methanol, ethanol, propanol, isopropanol, butanol, acetone, or mixtures thereof.

3. The method of claim 2 , wherein the solvent is water or methanol.

4. The method of claim 1 , wherein the metal precursors are metal salts or metal oxides or a combination thereof.

5. The method of claim 1 , wherein the metal precursors include a trivalent ion of La, Ce, Nd, Bi, Sc, or Y or a tetravalent ion of an element of Zr, Pt, Pd, Ni, Mo, Rh, Ru, or Ir, or a bivalent, trivalent or tetravalent ion of Ba, Ca, Cu, Mg, Ru, Rh, Pt, Pd, Ni, Co, Ir, or Mo.

6. The method of claim 5 , wherein the pyrochlore has a structure of:
A x B y−z C z O 7 ,
wherein
A is a trivalent ion of an element of La, Ce, Nd, Bi, Sc, or Y, where 0≦x≦2,
B is a tetravalent ion of an element of Zr, Pt, Pd, Mo, Rh, Ru, or Ir, where 0≦y−z≦2, and
C is a bivalent, trivalent or tetravalent ion of Ba, Ca, Cu, Mg, Ru, Rh, Pt, Pd, Ni, Co, Ir, or Mo, where 0≦z≦2.

7. The method of claim 1 , wherein the pyrochlore has a structure of La 2 Zr 2 O 7 , La 2 R 0.11 Zr 1.89 O 7 , La 2 Ir 0.11 Zr 1.89 O 7 , La 2 Ni 0.11 Z 1.89 O 7 , La 2 Pt 0.11 Zr 1.89 O 7 , or La 2 Pd 0.11 Zr 1.89 O 7 .

8. The method of claim 1 , further comprising adding a chelating agent to the solution.

9. The method of claim 8 , wherein the chelating agent is citric acid, EDTA, disodium EDTA, trisodium EDTA, EGTA, phosphoric acid, or succinic acid.

10. The method of claim 9 , wherein the chelating agent is citric acid.

11. The method of claim 9 , wherein the molar ratio of the chelating agent to the total amount by weight of metal within the metal precursors ranges from 1:0.1 to 1:1.5.

12. The method of claim 1 , wherein the drying step (b) comprises subjecting the solution to a temperature range of 60 to 100° C. for a sufficient amount of time to substantially remove or evaporate the solvent from the solution to obtain the pyrochlore precursor material in powdered form.

13. The method of claim 12 , wherein the drying step (b) is performed under atmospheric conditions.

14. The method of claim 13 , wherein the drying step (b) comprises using a water bath or a hot plate.

15. The method of claim 12 , wherein the drying step (b) comprises using vacuum evaporation.

16. The method of claim 15 , wherein the vacuum evaporation is performed within a rotary evaporator.

17. The method of claim 12 , further comprising subjecting the pyrochlore precursor material to a temperature range of 100° C. to 150° C. for 1 to 3 hours.

18. The method of claim 1 , wherein the calcination step (c) comprises subjecting the pyrochlore precursor material to a temperature range of 800° C. to 1500° C. for sufficient amount of time to produce the pyrochlore.

19. The method of claim 18 , wherein the calcination step (c) comprises subjecting the pyrochlore precursor material to a temperature range of 900° C. to 1100° C. for 7 to 9 hours.

20. The method of claim 1 , wherein the drying step (b) and calcination step (c) are not performed in a reducing or nonoxidizing atmosphere.

21. The method of claim 1 , wherein the pyrochlore precursor material is not precipitated out of the solution in step (a) and step (b), and wherein ammonium carbonate is not added to the solution in step (a) and step (b).

22. The method of claim 1 , wherein the solution in steps (a) and (b) does not include a ployhydroxy alcohol.

23. The method of claim 1 , wherein a support material is dispersed in the solution.

24. The method of claim 23 , wherein the support material comprises a clay mineral or an alkaline earth metal/metal oxide compound.

25. The method of claim 1 , wherein the pyrochlore is capable of catalyzing the production of a gaseous mixture comprising hydrogen and carbon monoxide from a hydrocarbon gas.

Assignees

• Sabic Global Technologies Bv

Inventors

• D Souza Lawrence
• Viswanath Vinu

Classifications

• B01J35/735

  Pyrochlore-type A2B2O7 · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J35/30

  characterised by their physical properties · CPC title

• C01B3/326

  characterised by the catalysts · CPC title