Zirconium phosphate particles having improved adsorption capacity and method of synthesizing the same

Patent metadata

Field	Value
Publication number	US-9296611-B2
Application number	US-201414247261-A
Country	US
Kind code	B2
Filing date	Apr 8, 2014
Priority date	Oct 3, 2008
Publication date	Mar 29, 2016
Grant date	Mar 29, 2016

Abstract

Zirconium phosphate particles are synthesized by providing a solution of zirconium oxychloride in an aqueous solvent, adding at least one low molecular weight, oxygen containing, monofunctional, organic additive to the solution, and combining this solution with heated phosphoric acid or a phosphoric acid salt to obtain zirconium phosphate particles by sol gel precipitation.

First claim

What is claimed is:

1. A method of making zirconium phosphate particles comprising:
(a) combining zirconium oxychloride with at least one oxygen containing, monofunctional, organic additive having a molecular weight of 20-80 and in an amount of from 25 wt % to 70 wt % based on the weight of the zirconium oxychloride in an aqueous solvent to form a solution, and
(b) combining the solution obtained in (a) with phosphoric acid and removing the at least one oxygen containing, monofunctional, organic additive to obtain zirconium phosphate particles by sol gel precipitation.

2. The method of claim 1 , wherein the phosphoric acid in step (b) has a temperature of from about 90° C. to about 100° C.

3. The method of claim 1 , wherein the oxygen containing, monofunctional, organic additive forms a complex with zirconium ions in the solution.

4. The method of claim 1 , wherein zirconium oxychloride is dissolved in the aqueous solvent and then the oxygen containing, monofunctional, organic additive is added to form the solution of step (a).

5. The method of claim 1 , wherein the zirconium oxychloride is present in the aqueous solvent at a concentration of from about 1.1 to about 1.5 g/ml.

6. The method of claim 1 , wherein the zirconium oxychloride is present in the aqueous solvent up to a saturation concentration.

7. The method of claim 1 , wherein the oxygen containing, monofunctional, organic additive is present in the aqueous solvent and then the zirconium oxychloride is added to form the solution of step (a).

8. The method of claim 3 , wherein the oxygen containing, monofunctional, organic additive is present in the solution of step (a) in a molar amount sufficient so that substantially all of the zirconium ions in the solution are converted to the complex.

9. The method of claim 1 , wherein the oxygen containing, monofunctional, organic additive forms a soluble polymer complex with zirconium ions.

10. The method of claim 1 , wherein the oxygen containing, monofunctional, organic additive is an alcohol, a carboxylate, or combinations thereof.

11. The method of claim 1 , wherein the oxygen containing, monofunctional, organic additive is methanol, ethanol, propanol, isopropanol, acetic acid, propionic acid, or combinations thereof.

12. The method of claim 1 , wherein the phosphoric acid comprises orthophosphoric acid.

13. The method of claim 1 , further comprising:
(c) subjecting an aqueous slurry containing zirconium phosphate particles obtained from step (b) to a heat treatment carried out at a temperature of from about 90° C. to about 100° C.

14. The method of claim 13 , wherein the heat treatment of step (c) is carried out for at least one hour.

15. The method of claim 13 , wherein the aqueous slurry of step (c) is agitated during the heat treatment.

16. The method of claim 1 , wherein in step (b), the solution obtained in step (a) and a solution of phosphoric acid are combined so that zirconium ions and phosphate groups are present in a molar ratio of about 1 to about 3 of zirconium to phosphate.

17. The method of claim 1 , wherein the phosphoric acid has a molarity of from about 1.5 moles/L to about 3 moles/L.

18. The method of claim 1 , further comprising combining the solution obtained in (a) with HCl before step (b).

19. The method of claim 1 , further comprising isolating and drying the zirconium phosphate particles obtained in step (b) to obtain a free flowing powder.

20. A method of making zirconium phosphate particles having a controlled particle size comprising forming zirconium phosphate particles by sol gel precipitation by the method of claim 1 , wherein the zirconium phosphate particles have a particle size and particle size distribution obtained by controlling one or more of the following parameters: (a) the rate at which the solution of zirconium oxychloride and oxygen containing, monofunctional, organic additive is added to the reaction vessel, (b) the rate at which the solution of phosphoric acid is added to the reaction vessel, (c) the pH of the solution of phosphoric acid, (d) the concentration of zirconium oxychloride, oxygen containing, monofunctional, organic additive, or phosphoric acid in the reaction vessel, (e) the presence of HCl in the reaction vessel, (f) the speed of the agitator, or (g) any combination thereof.

Assignees

• Fresenius Med Care Hldg Inc

Inventors

• Wong Raymond June-Hin

Classifications

• B01J20/28083

  being in the range 2-50 nm, i.e. mesopores · CPC title

• B01J20/28057

  Surface area, e.g. B.E.T specific surface area · CPC title

• C01B25/372 Primary

  of titanium, vanadium, zirconium, niobium, hafnium or tantalum · CPC title

• C01B25/37

  Phosphates of heavy metals · CPC title

• B01J20/0211

  Compounds of Ti, Zr, Hf · CPC title