Preparation of suspensions

Patent metadata

Field	Value
Publication number	US-10167203-B2
Application number	US-201514960926-A
Country	US
Kind code	B2
Filing date	Dec 7, 2015
Priority date	Dec 24, 2004
Publication date	Jan 1, 2019
Grant date	Jan 1, 2019

Abstract

A method for preparing a suspension of LDH particles comprising the steps of: preparing LDH precipitates by coprecipitation to form a mixture of LDH precipitates and solution; separating the LDH precipitates from the solution; washing the LDH precipitates to remove residual ions; mixing the LDH precipitates with water; and subjecting the mixture of LDH particles and water to a hydrothermal treatment step by heating to a temperature of from greater than 80° C. to 150° C. for a period of about 1 hour to about 144 hours to form a well dispersed suspension of LDH particles in water, wherein said LDH particles in suspension comprise platelets having a maximum particle dimension of up to 400 nm.

First claim

The invention claimed is:

1. A method for preparing a suspension of LDH particles comprising the steps of:
a) preparing LDH precipitates by coprecipitation to form a mixture of LDH precipitates and solution, wherein the LDH precipitates and the solution formed in step (a) are left in contact with each other for a period not exceeding 30 minutes;
b) separating the LDH precipitates from the solution;
c) washing the LDH precipitates to remove residual ions;
d) mixing the LDH precipitates with water; and
e) subjecting the mixture of LDH particles and water from step (d) to a hydrothermal treatment step by heating to a temperature of from greater than 80° C. to 150° C. for a period of about 1 hour to about 144 hours to form a dispersed suspension of non-aggregated LDH particles in water, wherein said LDH particles in suspension comprise platelets having a maximum particle dimension of up to 400 nm.

2. A method as claimed in claim 1 wherein step (e) comprises subjecting the mixture of LDH particles and water from step (d) to a hydrothermal treatment step by heating to a temperature of from greater than 80° C. to 150° C. for a period of about 1 hour to about 2 hours.

3. A method as claimed in claim 1 wherein the platelets exhibit a particle size distribution of no more than about ±27%, based upon the peak value and the peak width at half maximum from the particle size distribution of an intensity average using photon correlation spectroscopy (PCS) measurement.

4. A method as claimed in claim 1 wherein the LDH precipitates and the solution formed in step (a) are left in contact with each other for a period not exceeding 20 minutes.

5. A method as claimed in claim 1 wherein the LDH precipitates and the solution formed in step (a) are left in contact with each other for a period not exceeding 10 minutes.

6. A method as claimed in claim 1 wherein the LDH precipitates and the solution formed in step (a) are left in contact with each other for a period not exceeding 5 minutes.

7. A method as claimed in claim 1 wherein the LDH precipitates and the solution formed in step (a) are left in contact with each other for a period not exceeding 1 minute.

8. A method as claimed in claim 1 wherein the LDH precipitates and solution formed in step (a) are stirred.

9. A method as claimed in claim 1 wherein the hydrothermal treating step is carried out while suppressing boiling.

10. A method as claimed in claim 1 wherein in step (a) a mixed metal ion solution and an alkaline solution are rapidly mixed together.

11. A method as claimed in claim 10 wherein the mixed metal ion solution and the alkaline solution are added together within a time period of less than 1 minute.

12. A method as claimed in claim 1 wherein precipitation in step (a) takes place at a temperature ranging from room temperature up to about 50° C.

13. A method as claimed in claim 1 wherein the LDH precipitates are washed one or more times with deionized water following separation from the solution.

14. A method as claimed in claim 1 wherein the mixture of water and LDH precipitates is held at the elevated temperature for a period of from 2-48 hours in step (e).

15. A method as claimed in claim 13 wherein the mixture of water and LDH precipitates is held at the elevated temperature for a period of from 1-24 hours.

16. A method as claimed in claim 1 wherein the largest dimension of the platelets in the suspension predominantly falls within the range of 20-400 nm.

17. A method as claimed in claim 1 wherein the largest dimension of the platelets in the suspension predominantly falls within the range of 40-300 nm.

18. A method as claimed in claim 1 wherein the suspension contains up to 10% w/w LDH platelets.

19. A method as claimed in claim 1 wherein the suspension contains up to 5% w/w LDH platelets.

20. A method as claimed in claim 1 wherein the suspension contains up to about 1% w/w LDH platelets.

21. A method as claimed in claim 1 wherein the suspension contains less than 1% w/w LDH particles.

22. A method as claimed in claim 1 further comprising the step of removing at least some of the water from the suspension to concentrate the particles to form a more concentrated suspension.

23. A method as claimed in claim 1 wherein step (d) comprises mixing the LDH precipitates with water in order to disperse the LDH precipitates in the water and to break up any loose aggregates of LDH precipitates into platelets.

24. A method for forming LDH particles comprising forming a suspension as claimed in claim 1 and separating the LDH particles from the suspension.

Assignees

• Univ Queensland

Inventors

• Lu Gaoqing
• Xu Zhiping

Classifications

• C01F7/784 Primary

  Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions · CPC title

• B82Y30/00 Primary

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01G49/009

  Compounds containing iron, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2004/53

  bimodal size distribution · CPC title