Method of purifying barium nitrate aqueous solution

• US 7,648,687 B1
• Filed: 06/15/2006
• Issued: 01/19/2010
• Est. Priority Date: 06/15/2006
• Status: Expired due to Fees

• Current Assignee: Eestor Inc. (FuelPositive Corp.)
• Original Assignee: Eestor Inc. (FuelPositive Corp.)
• Inventors: Nelson, Carl W., Weir, Richard D.
• Primary Examiner(s): Lorengo; Jerry
• Assistant Examiner(s): Smith; Jennifer A
• Application Number:
  US11/453,581
• Time in Patent Office: 1,314 Days
• Field of Search: 423/395, 423/397, 423/396, 423/394.2, 423/409
• US Class Current: 423/157
• CPC Class Codes: B01D 11/043 with stationary contacting elements, sieve plates or loose contacting elements
• CPC Class Codes: B01D 11/0434 comprising rotating mechanisms, e.g. mixers, rotational oscillating motion, mixing pumps
• CPC Class Codes: C01F 11/36 Nitrates
• CPC Class Codes: C01P 2006/60 Optical properties, e.g. expressed in CIELAB-values
• CPC Class Codes: C22B 26/20 Obtaining alkaline earth metals or magnesium
• CPC Class Codes: C22B 3/44 by chemical processes treatment or purification of solutions by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42
• CPC Class Codes: Y02P 10/20 Recycling

Abstract

Purification techniques have been developed for ceramic powder precursors, e.g., barium nitrate. These techniques can be performed using one or more of the following operations: (1) removal of impurities by precipitation or coprecipitation and separation using a nonmetallic-ion-containing strong base, e.g., tetraalkylammonium hydroxides; (2) reduction of higher oxidation-state-number oxymetal ions and subsequent precipitation as hydroxides that are separated from the solution; and (3) use of liquid-liquid exchange extraction procedures to separate certain impurities.

Claims

1. A method of purifying a barium nitrate aqueous solution, the method comprising:

providing the barium nitrate aqueous solution;

combining the barium nitrate aqueous solution with a precipitant solution to cause precipitation of first impurities, the first impurities comprising at least one of magnesium hydroxide, aluminum hydroxide, or iron hydroxide, the precipitant solution comprising tetraalkylammonium hydroxide;

separating the first impurities from the barium nitrate aqueous solution; and

following separating the first impurities, combining the barium nitrate aqueous solution with a separation solution using a liquid-liquid extraction column to remove second impurities from the barium nitrate aqueous solution, the second impurities comprising strontium ions.

2. The method of claim 1 wherein the precipitant solution further comprises a pH in the range of approximately 7.5 to nearly but below 8.5.

3. The method of claim 1 the combining the barium nitrate aqueous solution with the precipitant solution further comprises:

metering the precipitant solution into the barium nitrate aqueous solution; and

mixing the barium nitrate aqueous solution and the precipitant solution using at least one of a mechanical mixer and a recirculating pump.

4. The method of claim 1 wherein the separating uses at least one of colloidal filtration, pressure filtration, vacuum filtration, dead-end filtration, crossflow filtration, centrifugation, sedimentation, membrane separation, a pleated all-polypropylene filter, and a hydrophilic polyethersulfone (PES) membrane filter.

5. The method of claim 1 further comprising:

reducing oxymetal ions in the barium nitrate aqueous solution to cause the precipitation of third impurities.

6. The method of claim 5 further comprising:

increasing barium nitrate aqueous solution pH before the reducing oxymetal ions.

7. The method of claim 6 wherein the increasing barium nitrate aqueous solution pH further comprises:

combining a nonmetal-ion-containing strong base with the barium nitrate aqueous solution.

8. The method of claim 7 wherein the combining the nonmetal-ion-containing strong base with the barium nitrate aqueous solution further comprises:

combining a tetraalkylammonium hydroxide solution with the barium nitrate aqueous solution to increase barium nitrate aqueous solution pH to approximately 10.

9. The method of claim 5 wherein the reducing further comprises:

reducing oxymetal ions in the barium nitrate aqueous solution using a nonmetallic-ion-containing reducing agent.

10. The method of claim 9 wherein the reducing agent is hydrogen peroxide.

11. The method of claim 5 wherein the reducing further comprises:

reducing oxidation-state numbers for oxymetal ions in the barium nitrate aqueous solution to four or lower in oxidation state number.

12. The method of claim 5 further comprising:

separating the third impurities from the barium nitrate aqueous solution.

13. The method of claim 1 wherein the separation solution further comprises at least one of decanoic acid and kerosene.

14. The method of claim 1 wherein the combining the barium nitrate aqueous solution with the separation solution using the liquid-liquid extraction column further comprises:

using at least one of a static liquid-liquid extraction column, an agitated liquid-liquid extraction column, a sieve tray column, a random packed column, a structured packed column, a Karr column, a Scheibel column, a rotating disk contactor column, and a pulsed column.

15. The method of claim 1 wherein the combining the barium nitrate aqueous solution with the separation solution using the liquid-liquid extraction column further comprises:

reaching a near-emulsion state between the barium nitrate aqueous solution and the separation solution.

16. The method of claim 1 further comprising:

removing the barium nitrate aqueous solution from the liquid-liquid extraction column.

17. The method of claim 1 wherein the first impurities further comprise at least one of:

a magnesium hydroxide;

an aluminum hydroxide;

an iron hydroxide;

a hydrated metal ion of at least one of groups IIIB, IVB, VB, VIIB, VIIB, VIII, IB, IIB, IIIA, IVA, and VA;

a hydrated metal ion of at least one of the lanthanides and actinides;

a beryllium hydrated metal ion;

a magnesium hydrated metal ion;

an oxymetal ion of at least one of groups IVB, VB, VIIB, VIIB, IVA, and VA; and

an oxymetal ion of at least one actinide.

18. The method of claim 1 wherein the second impurities further comprise at least one of sodium ions, potassium ions, strontium ions, and calcium ions.

19. The method of claim 1 further comprising:

neutralizing the barium nitrate aqueous solution before the combining the barium nitrate aqueous solution with the separation solution using the liquid-liquid extraction column.

20. A method of purifying a barium nitrate aqueous solution, the method comprising:

providing the barium nitrate aqueous solution;

combining the barium nitrate aqueous solution with a precipitant solution to precipitate first impurities, the first impurities comprising at least one of magnesium hydroxide, aluminum hydroxide, or iron hydroxide, the precipitant solution comprising tetraalkylammonium hydroxide and having a pH in the range of 7.5 to 8.5;

separating the first impurities from the barium nitrate aqueous solution;

following separating the first impurities, increasing the pH of the barium nitrate aqueous solution after separating the first impurities;

reducing the oxymetal ions in the barium nitrate aqueous solution to precipitate second impurities, the second impurities including ions that have an oxidation-state-number of 6 or 7 prior to reducing;

separating the second impurities from the barium nitrate aqueous solution; and

following separating the second impurities, combining the barium nitrate aqueous solution with a separation solution using a liquid-liquid extraction column to remove third impurities from the barium nitrate aqueous solution, the third impurities comprising strontium ions.

21. The method of claim 20, wherein increasing the pH of the barium nitrate aqueous solution includes increasing the pH to approximately 10.

22. The method of claim 20, wherein the separation solution includes decanoic acid.

23. A method of purifying a barium nitrate aqueous solution, the method comprising:

providing the barium nitrate aqueous solution;

combining the barium nitrate aqueous solution with a precipitant solution to precipitate first impurities, the first impurities comprising at least one of magnesium hyroxide, aluminum hydroxide, or iron hydroxide, the precipitant solution comprising tetraalkylammonium hydroxide and having a pH in the range of 7.5 to 8.5, strontium ions substantially remaining in solution;

separating the first impurities from the barium nitrate aqueous solution;

increasing the pH of the barium nitrate aqueous solution to approximately 10 using tetraalkylammonium hydroxide after separating the first impurities;

reducing the oxymetal ions in the barium nitrate aqueous solution to precipitate second impurities, the second impurities including ions that have an oxidation-state-number of 6 or 7 prior to reducing;

separating the second impurities from the barium nitrate aqueous solution; and

following separating the second impurities, combining the barium nitrate aqueous solution with a separation solution using a liquid-liquid extraction column to remove third impurities from the barium nitrate aqueous solution, the third impurities comprising strontium ions, the separation solution including decanoic acid.