METHOD OF MAKING GRANULAR ZIRCONIUM HYDROUS OXIDE ION EXCHANGERS, SUCH AS ZIRCONIUM PHOSPHATE AND HYDROUS ZIRCONIUM OXIDE, PARTICULARLY FOR COLUMN USE

• US 3,850,835 A
• Filed: 11/08/1971
• Issued: 11/26/1974
• Est. Priority Date: 11/08/1971
• Status: Expired due to Term

• Current Assignee: Clifford M. Moran, Laurence B. Marantz
• Original Assignee: Clifford M. Moran, Laurence B. Marantz
• Inventors: Moran, Clifford M., Marantz, Laurence B.
• Primary Examiner(s): Lechert, Jr., Stephen J.
• Assistant Examiner(s): Gluck, Irwin
• Application Number:
  US05/196,805
• Time in Patent Office: 1,114 Days
• Field of Search: 252/182,179,313R 423/70,80,84,85,181 210/24,263
• US Class Current: 423/81
• CPC Class Codes: B01J 39/02 Processes using inorganic exchangers
• CPC Class Codes: B01J 39/10 Oxides or hydroxides
• CPC Class Codes: B01J 39/12 Compounds containing phosphorus
• CPC Class Codes: C01G 25/02 Oxides
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer

Abstract

A method of producing zirconium hydrous oxide ion exchangers by adding zirconium compound in granular form to a reagent which fixes the shape of the initial zirconium compound particles by converting the zirconium compound to insoluble zirconium hydrous oxide ion exchangers.

Claims

1. A PROCESS FOR PRODUCING A GRANULAR ZIRCONIUM HYDROUS OXIDE ION EXCHANGER OF A PREDETERMINED PARTICLE SIZE DISTRIBUTION COMPRISING THE STEPS OF:

SELECTING AAN AQUEOUS SOLUTION OF A REAGENT WHEREIN THE REAGENT IS SELECTED FROM THE GROUP CONSISTING OF WATER SOLUBLE PHOSPHATES AND THE BASES WHICH PROVIDE A HYDROXYL ION IN AQUEOUS SOLUTION;

REACTING THE REAGENT WITH A GRANULAR ZIRCONIUM COMPOUND TO FROM A GRANULAR ZIRCONIUM HYDROUS OXIDE ION EXCHANGER PRODUCT, IN THE REAGENT SOLUTION, OF A PARTICLE SIZE DISTRIBUTION DETERMINED BY THAT OF THE GRANULAR ZIRCONIUM COMPOUND, SAID REACTION BEING ACCOMPLISHED BY ADDING TO THE REAGENT SOLUTION, IN GRANULAR FROM, A GRANULAR ZIRCONIUM COMPOUND WHICH IS MORE SOLUBLE IN THE AQUEOUS REAGENT THAN SAID GRANULAR ION EXCHANGER PRODUCT FORMED THEREIN AND ALLOWING THE ZIRCONIUM COMPOUND TO REACT WITH THE REAGENT FOR AT LEAST A SUFFICIENT TIME TO SUBSTANTIALLY CONVERT THE ZIRCONIUM COMPOUND TO SAID GRANULAR ION EXCHANGER PRODUCT IN THE REAGENT SOLUTION;

AND RECOVERING SAID ION EXCHANGER PRODUCT.

2. The process of claim 1 wherein during the reacting step the temperature of the aqueous reagent solution is from about room temperature to about 100*C and the granular zirconium compound is added with stirring which continues from about 5 to about 30 minutes.

3. The process of claim 1 wherein the granular zirconium compound has a particle size distribution band which corresponds generally to an ion exchanger particle size distribution band usable in an ion exchanger column.

4. The process of claim 3 wherein the particle size distribution band of the granular zirconium compound is from about 12 to about 325 mesh.

5. The process of claim 1 wherein the granular zirconium compound is selected from the group consisting of zirconium oxychloride, zirconium nitrate, zirconium sulfate, zirconium acetate, and basic zirconium sulfate.

6. The process of claim 1 wherein the reagent is a water soluble phosphate and the insoluble zirconium hydrous oxide ion exchanger product is a zirconium phosphate.

7. The process of claim 6 wherein the concentration of the phosphate in the aqueous reagent solution remains above about 0.5 molar during the reaction step of the process.

8. The process of claim 6 wherein the water soluble phosphate is selected from the group consisting of phosphoric acid, sodium phosphate, and a mixed sodium hydrogen phosphate solution.

9. The process of claim 5 wherein the reagent is a water soluble phosphate and the insoluble zirconium hydrous oxide ion exchanger is an insoluble zirconium phosphate.

10. The process of claim 1 wherein the reagent is a base which provides a hydroxyl ion in aqueous solution and the insoluble zirconium hydrous oxide ion exchanger product is an insoluble hydrous zirconium oxide.

11. The process of claim 10 wherein the base is selected from the group consisting of sodium hydroxide and ammonium hydroxide.

12. The process of claim 5 wherein the reagent is a base which provides a hydroxyl ion in aqueous solution and the product is an insoluble hydrous zirconium oxide.

13. The process of claim 1 wherein the recovery step includes the step of drying the product.