IP Library Granted Patent US 9,828,294
Granted Patent B2
US 9,828,294 · App. 15/109,538 · Granted Nov 28, 2017

Sintered clay mineral matrix doped with rare earth metals, transition metals, or post-transition metals

Inventors: Xinwei Chen (Singapore, SG); Liang Hong (Singapore, SG); Yi'en Zhou (Singapore, SG)
Assignee: National University of Singapore
C04B33/04B01D67/0041B01D67/0083B01D71/02B01D71/024C04B33/131C04B33/1305C04B33/1315C04B33/32C04B38/0064C04B2111/00801C04B2235/3227C04B2235/3284C04B2235/349C04B2235/602C04B2235/6021C04B2235/6025C04B2235/6027C04B2235/656C04B2235/661
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Quick Facts
Patent No.
US 9,828,294
App. No.
15/109,538
Granted
Nov 28, 2017
Kind
B2
Abstract

A porous sintered clay mineral matrix that contains aluminum and is doped with 0.1-20 mol %, based on the amount of the aluminum, one or more transition metals, one or more post-transition metals, one or more rare earth metals, or a combination thereof. An example is a kaolinite matrix. The matrix can be made from a calcined clay mineral powder that contains aluminum and is doped with at least one of these metals. Also disclosed are methods of preparing the above-described matrix and powder.

Claims (34)

1. A sintered clay mineral matrix, wherein the matrix is porous, contains aluminum, and is doped with 0.1-20 mol %, based on the amount of the aluminum, one or more transition metals, one or more post-transition metals, one or more rare earth metals, or a combination thereof, in which at least zinc or lanthanum is a dopant.

2. The sintered clay mineral matrix of claim 1 , wherein the transition metal is titanium, chromium, iron, cobalt, manganese or yttrium, the post-transition metal is zinc, and the rare earth metal is lanthanum.

3. The sintered clay mineral matrix of claim 2 , wherein the matrix is a membrane.

4. The sintered clay mineral matrix of claim 3 , wherein the matrix is doped with lanthanum or zinc.

5. The sintered clay mineral matrix of claim 4 , wherein the matrix is doped with lanthanum 5-15 mol %.

6. The sintered clay mineral matrix of claim 4 , wherein the sintered clay mineral matrix is a sintered kaolinite matrix.

7. The sintered clay mineral matrix of claim 6 , wherein the matrix is doped with lanthanum and the pores in the matrix have two distinctive diameter distributions, one in a range of 4 to 11 inn and the other less than 3 μm.

8. The sintered clay mineral matrix of claim 6 , wherein the matrix is doped with lanthanum and has a mechanical strength rate of greater than 5 MPa and a Darcy's permeability rate of greater than 5.00E-014 m 2 .

9. The sintered clay mineral matrix of claim 4 , wherein the matrix is doped with zinc 5-20 mol %.

10. The sintered clay mineral matrix of claim 6 , wherein the matrix is doped with zinc and has a mechanical strength rate of greater than 30 MPa.

11. A calcined clay mineral powder, wherein the powder contains aluminum and is doped with 0.1-20 mol %, based on the amount of the aluminum, one or more transition metals, one or more post-transition metals, one or more rare earth metals, or a combination thereof, in which at least zinc or lanthanum is a dopant.

12. The calcined clay mineral powder of claim 11 , wherein the transition metal is titanium, chromium, iron, cobalt, manganese or yttrium, the post-transition metal is zinc, and the rare earth metal is lanthanum.

13. The calcined clay mineral powder of claim 12 , wherein the powder is doped with lanthanum or zinc.

14. The calcined clay mineral powder of claim 13 , wherein the powder is doped with lanthanum 5-15 mol %.

15. The calcined clay mineral powder of claim 13 , wherein the powder is doped with zinc 5-20 mol %.

16. The calcined clay mineral powder of claim 13 , wherein the calcined clay mineral powder is a calcined kaolinite powder.

17. A method of preparing a clay mineral material, the method comprising:

dissolving one or more salts of transition metals, one or more salts of post-transition metals, one or more salts of rare earth metals, or a combination thereof in water to form a solution;

adding an organic solvent to the solution to form a second solution;

mixing clay mineral with the second solution to form a homogenous mixture;

heating the homogenous mixture at 50-150° C. for 12-72 hours to obtain a dried lump;

calcining the dried lump at 500-800° C. for 1-10 hours, and then cooling it to an ambient temperature, wherein both the heating and cooling are each conducted at a rate of 1-20° C./min; and

grinding the calcined lump to obtain a metal-doped clay mineral powder.

18. The method of claim 17 , wherein the transition metal is titanium, chromium, iron,

cobalt, manganese or yttrium, the post-transition metal is zinc, and the rare earth metal is lanthanum.

19. The method of claim 18 , wherein the clay mineral is kaolinite.

20. The method of claim 18 , wherein the salt is lanthanum nitrate or zinc nitrate.

21. The method of claim 17 , further comprising:

mixing the metal-doped clay mineral powder with a solution to form a second homogenous mixture, wherein the solution is prepared by dissolving 1-10 wt % polymeric binder in a pure or mixed organic solvent and includes 0.1 to 1 wt % additives that is a non-ionic surfactant, a deflocculating agent, and a plasticizer;

drying the second homogenous mixture at an ambient temperature for 1-10 hours to form a cake;

grinding the cake to obtain a powder;

molding the powder to form a ceramic green body by forming techniques of compression molding, extrusion, slip casting or tape casting; and

sintering the green body at 1000-1400° C. for 2-10 hours, and then cooling it to an ambient temperature, wherein both the heating and cooling are each conducted at a rate of 1-20° C./min, to obtain a metal-doped clay mineral matrix.

22. The method of claim 21 , wherein the clay mineral is kaolinite.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 12, 2016
From: CHEN, XINWEI; HONG, LIANG; ZHOU, YI'EN
To: NATIONAL UNIVERSITY OF SINGAPORE
Reel/Frame 039415/0020 →
Continuity (2)
Provisional Application 61928696 · Jan 17, 2014
Related Publication 20160326056A1 · Nov 10, 2016