IP Library Granted Patent US 9,856,543
Granted Patent B2
US 9,856,543 · App. 13/814,088 · Granted Jan 2, 2018

Purification process

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Quick Facts
Patent No.
US 9,856,543
App. No.
13/814,088
Granted
Jan 2, 2018
Kind
B2
Abstract

A process for purifying Mo-99 from an acidic solution obtained by dissolving an irradiated solid target comprising uranium in an acidic medium, or from an acidic solution comprising uranium and which has previously been irradiated in a nuclear reactor, or from an acidic solution comprising uranium and which has been used as reactor fuel in a homogeneous reactor, the process comprising contacting the acidic solution with an adsorbent comprising a zirconium oxide, zirconium hydroxide, zirconium alkoxide, zirconium halide and/or zirconium oxide halide, and eluting the Mo-99 from the adsorbent using a solution of a strong base, the eluate then being subjected to a subsequent purification process involving an alkaline-based Mo-99 chromatographic recovery step on an anion exchange material. Also provided is apparatus for carrying out the process.

Claims (19)

1. A process for purifying Mo-99 from (i) an acidic solution by dissolving an irradiated solid target comprising uranium in an acidic medium; (ii) an acidic solution comprising uranium and which has previously been irradiated in a nuclear reactor, or (iii) an acidic solution comprising uranium and which has been used as reactor fuel in a homogeneous reactor, the process comprising

(a) adsorbing the Mo-99 in the acidic solution onto an adsorbent comprising a zirconium compound selected from the group consisting of zirconium oxide, zirconium hydroxide, zirconium alkoxide, zirconium halide and zirconium oxide halide and eluting the Mo-99 from the adsorbent using a solution of base;

(b) adsorbing the eluted Mo-99 in the solution of base onto an anion exchange material and eluting the Mo-99 from the anion exchange material using a solution of acid;

(c) adsorbing the eluted Mo-99 in the solution of acid onto a MnO 2 material and dissolving the MnO 2 material bearing the adsorbed Mo-99 with a solution of sulfuric acid containing thiocyanide ions and a reducing agent to form a solution comprising [Mo(SCN) 6 ] 3− ; and

(d) contacting the solution comprising [Mo(SCN) 6 ] 3− with an ion exchange material comprising iminodiacetate groups to adsorb the Mo-99 onto the ion exchange material and eluting the Mo-99 from the ion exchange material using a solution of base.

2. The process of claim 1 , wherein the adsorbent also comprises a titanium oxide and/or silicon oxide.

3. The process of claim 2 , wherein the zirconium compound is present at a concentration of from 5 to 70 mol % of the adsorbent.

4. The process of claim 1 , wherein the adsorbent is in the form of pellets.

5. The process of claim 1 , wherein the acidic solution is contacted with the adsorbent in a column packed with the adsorbent and provided with an inlet and an outlet.

6. The process of claim 5 , wherein, following passage of the acidic solution through the column packed with the adsorbent, the column is flushed with an acid solution and/or rinsed with water.

7. The process of claim 1 , wherein the solution of base used in step (a) is 1 M sodium hydroxide.

8. The process of claim 1 , wherein the solution of acid used in step (b) is 3-4 M nitric acid.

9. The process of claim 1 , wherein the solution of sulfuric acid containing thiocyanide ions used in step (c) comprises 9 M sulfuric acid.

10. The process of claim 1 , wherein the solution of base used in step (d) is 1 M sodium hydroxide.

11. The process of claim 10 , wherein the solution of base further comprises hydrogen peroxide.

12. The process of claim 1 , wherein the Mo-99 eluted from the ion exchange material in step (d) is adsorbed to an anion exchange material and the Mo-99 is eluted from the anion exchange material using a solution of nitric acid.

13. The process of claim 12 , wherein the eluted Mo-99 in the solution of nitric acid is heated until dryness, thereby forming a dried product.

14. The process of claim 13 , wherein the dried product is sublimated at 800° C. to form a sublimated solid.

15. The process of claim 14 , wherein the sublimated solid is solubilized in an alkaline solution.

Assignments (5)
RELEASE OF PATENT SECURITY INTERESTS RECORDED AT REEL 032480, FRAME 0001 Recorded Nov 16, 2023
From: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
To: THERAKOS, INC.; MALLINCKRODT INTERNATIONAL FINANCE S.A.; MALLINCKRODT CB LLC; MALLINCKRODT FINANCE GMBH; MALLINCKRODT US HOLDINGS LLC (F/K/A MALLINCKRODT US HOLDINGS INC.); MALLINCKRODT CARRIBEAN, INC.; MALLINCKRODT US POOL LLC; MNK 2011 LLC (F/K/A MALLINCKRODT INC.); LUDLOW LLC (F/K/A LUDLOW CORPORATION); CNS THERAPEUTICS, INC.; MALLINCKRODT ENTERPRISES HOLDINGS LLC (F/K/A MALLINCKRODT ENTERPRISES HOLDINGS, INC.); MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; LAFAYETTE PHARMACEUTICALS LLC; LIEBEL-FLARSHEIM COMPANY LLC; MALLINCKRODT BRAND PHARMACEUTICALS LLC (F/K/A MALLINCKRODT BRAND PHARMACEUTICALS, INC.); MALLINCKRODT VETERINARY, INC.; MALLINCKRODT US HOLDINGS LLC; IMC EXPLORATION COMPANY; MEH, INC.; MALLINCKRODT HOSPITAL PRODUCTS IP UNLIMITED COMPANY (F/K/A MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED); MALLINCKRODT ARD IP UNLIMITED COMPANY (F/K/A MALLINCKRODT ARD IP LIMITED); OCERA THERAPEUTICS LLC (F/K/A OCERA THERAPEUTICS, INC.); SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC (F/K/A VTESSE INC.); MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY (F/K/A MALLINCKRODT PHARMA IP TRADING D.A.C.); INFACARE PHARMACEUTICAL CORPORATION; ST SHARED SERVICES LLC; IKARIA THERAPEUTICS LLC; INO THERAPEUTICS LLC
Reel/Frame 065609/0322 →
RELEASE OF SECURITY INTEREST Recorded Jan 31, 2017
From: DEUTSCHE BANK AG NEW YORK BRANCH
To: MALLINCKRODT NUCLEAR MEDICINE LLC
Reel/Frame 041131/0213 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 13, 2016
From: MALLINCKRODT LLC
To: MALLINCKRODT NUCLEAR MEDICINE LLC
Reel/Frame 039149/0234 →
SECURITY INTEREST Recorded Mar 19, 2014
From: MALLINCKRODT INTERNATIONAL FINANCE S.A.; MALLINCKRODT CB LLC; MALLINCKRODT FINANCE GMBH; MALLINCKRODT US HOLDINGS INC.; MALLINCKRODT CARIBBEAN, INC.; MALLINCKRODT US POOL LLC; MALLINCKRODT INC.; LUDLOW CORPORATION; CNS THERAPEUTICS, INC.; ENTERPRISES HOLDINGS, INC.; MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; LAFAYETTE PHARMACEUTICALS LLC; LIEBEL-FLARSHEIM COMPANY LLC; MALLINCKRODT BRAND PHARMACEUTICALS, INC; MALLINCKRODT VETERINARY, INC.; MALLINCKRODT US HOLDINGS LLC; IMC EXPLORATION COMPANY; MEH, INC; MALLINCKRODT ENTERPRISES HOLDINGS, INC.
To: DEUTSCHE BANK AG NEW YORK BRANCH
Reel/Frame 032480/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 25, 2013
From: BARBOSA, LUIS A.M.M.
To: MALLINCKRODT LLC
Reel/Frame 029868/0423 →