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US4861490A Expired / Lapsed US ⏱️ 0.0 years remaining

Removal of cationic impurities from inorganic solutions

Assignee: PHOSPHATE ENGINEERING AND CONSTRUCTION COMPANY PO BOX 5167 LAKELAND FLORIDA 33807
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Filing: 1987-08-21
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Granted: 1989-08-29
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Expires: 2007-08-21
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Abstract

Abstract A process for the removal of cationic impurities from inorganic solutions and especially wet process phosphoric acid solutions wherein the solutions are passed through an ammonium ion or hydrogen ion charged cation exchange resin to remove various metal cations and thereafter the ion exchange resin is regenerated using an excess volume of ammonium sulfate solution which is subsequently treated to precipitate and filter out the cationic impurities so that the ammonium sulfate solution may be recycled for further ion exchange regeneration.

Inventors

  • 👤 Susan B. Morris

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 02:37
CPC Classifications
C; C01; C01B; C01B25/00; C01B25/16; C01B25/18; C01B25/234; C01B25/237; C01B25/238; B; B01; B01J; B01J39/00; B01J39/04; B01J49/00; B01J49/05; B01J49/06

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 102 words
A method for removing cationic impurities from inorganic feed solutions comprising the steps of passing the feed solution through an ion exchanger having an ion exchange resin charged with a cation selected from the group consisting of ammonium ions and hydrogen ions in order to remove the cationic impurities from the feed solution, regenerating the ion exchange resin within the ion exchanger by passing a saturated ammonium sulfate regenerant solution therethrough and recovering a dilute regenerant solution, resaturating the dilute regenerant solution passing from the ion exchanger to thereby precipitate impurities therefrom as sulfate salts and recovering a resaturated ammonium sulfate solution.
Claim 2
Independent Claim 102 words
A method for removing cationic impurities from inorganic feed solutions comprising the steps of passing the feed solution through an ion exchanger having an ion exchange resin charged with a cation selected from the group consisting of ammonium ions and hydrogen ions in order to remove the cationic impurities from the feed solution, regenerating the ion exchange resin within the ion exchanger by passing a saturated ammonium sulfate regenerant solution therethrough and recovering a dilute regenerant solution, resaturating the dilute regenerant solution passing from the ion exchanger to thereby precipitate impurities therefrom as sulfate salts and recovering a resaturated ammonium sulfate solution.
Claim 3
Dependent Claim 25 words
The method of claim 1 in which at least 4-10 bed volumes of saturated ammonium sulfate solution are used to regenerate the ion exchange resin.
Claim 4
Dependent Claim 87 words
The method of claim 1 including the additional steps of filtering the dilute regenerant solution passing from the ion exchanger to remove solids therefrom prior to resaturating, said resaturating of the dilute regenerant solution including adding NH 3 to the dilute regenerant solution to form metallic hydroxides, filtering the metallic hydroxides from the dilute regenerant solution and subsequently adding substantially pure sulfuric acid to the dilute regenerant solution to obtain said resaturated ammonium sulfate solution, and thereafter recycling the resaturated ammonium sulfate solution to the ion exchanger.
Claim 5
Dependent Claim 25 words
The method of claim 3 in which at least 4-10 bed volumes of saturated ammonium sulfate solution are used to regenerate the ion exchange resin.
Claim 6
Dependent Claim 43 words
The method of claim 4 including the additional step of passing a dilute solution of sulfuric acid through the ion exchanger to replace ammonium ions with hydrogen ions and obtaining an effluent of dilute ammonium sulfate solution, and thereafter recovering the ammonia therefrom.
Claim 7
Dependent Claim 27 words
The method of claim 5 in which said inorganic solution is a wet process phosphoric acid solution which is maintained at a temperature of approximately 140° F.
Claim 8
Dependent Claim 51 words
The method of claim 1 in which the resaturating of the dilute regenerant solution passing from the ion exchanger is achieved by adding NH 3 and (NH 4 )2SO 4 , thereafter filtering and recovering said resaturated ammonium sulfate solution, and recycling said resaturated ammonium sulfate solution to the ion exchanger.
Claim 9
Dependent Claim 25 words
The method of claim 7 in which at least 4-10 bed volumes of saturated ammonium sulfate solution are used to regenerate the ion exchange resin.
Claim 10
Dependent Claim 43 words
The method of claim 8 including the additional step of passing a dilute solution of sulfuric acid through the ion exchanger to replace ammonium ions with hydrogen ions and obtaining an effluent of dilute ammonium sulfate solution, and thereafter recovering the ammonia therefrom.
Claim 11
Dependent Claim 17 words
The method of claim 1 in which said inorganic solution is a wet process phosphoric acid solution.
Claim 12
Independent Claim 191 words
A method for removing cationic impurities from a wet process phosphoric acid solution comprising the steps of: (a) passing the wet process phosphoric acid solution through an ion exchanger having an ion exchange resin charged with cations selected from the group of ammonium ions and hydrogen ions, in order to remove the cationic impurities from the solution; (b) regenerating the ion exchange resin by passing first and second portions of a saturated ammonium sulfate regenerant solution therethrough in which a total of 4-10 bed volumes of saturated ammonium sulfate solution are used to regenerate the ion exchange resin; (c) filtering the first portion of regenerant solution passing from the ion exchanger to remove solids therefrom; (d) adding NH 3 to the first portion of regenerant solution to form metallic hydroxides; (e) filtering the metallic hydroxides from the first portion of regenerant solution; (f) thereafter combining the second portion of regenerant solution passing from the ion exchanger with the first portion regenerant solution and adding substantially pure sulfuric acid thereto to obtain a resaturated ammonium sulfate regenerant solution; and (g) subsequently recycling the resaturated ammonium sulfate regenerant solution to the ion exchanger.
Claim 13
Independent Claim 191 words
A method for removing cationic impurities from a wet process phosphoric acid solution comprising the steps of: (a) passing the wet process phosphoric acid solution through an ion exchanger having an ion exchange resin charged with cations selected from the group of ammonium ions and hydrogen ions, in order to remove the cationic impurities from the solution; (b) regenerating the ion exchange resin by passing first and second portions of a saturated ammonium sulfate regenerant solution therethrough in which a total of 4-10 bed volumes of saturated ammonium sulfate solution are used to regenerate the ion exchange resin; (c) filtering the first portion of regenerant solution passing from the ion exchanger to remove solids therefrom; (d) adding NH 3 to the first portion of regenerant solution to form metallic hydroxides; (e) filtering the metallic hydroxides from the first portion of regenerant solution; (f) thereafter combining the second portion of regenerant solution passing from the ion exchanger with the first portion regenerant solution and adding substantially pure sulfuric acid thereto to obtain a resaturated ammonium sulfate regenerant solution; and (g) subsequently recycling the resaturated ammonium sulfate regenerant solution to the ion exchanger.
Claim 14
Dependent Claim 22 words
The method of claim 11 including the additional step of initially filtering the wet process phosphoric acid solution to remove solids therefrom.
Claim 15
Dependent Claim 33 words
The method of claim 12 including the additional step of heating the wet process phosphoric acid solution to a temperature of approximately 140° F. prior to passing the solution through the ion exchanger.
Claim 16
Dependent Claim 42 words
The method of claim 11 including the additional step of passing a dilute solution of sulfuric acid through the ion exchanger to replace ammonium ions with hydrogen ions, obtaining an effluent of dilute ammonium sulfate solution, and thereafter recovering the ammonia therefrom.
Claim 17
Independent Claim 126 words
A method for removing cationic impurities from a wet process phosphoric acid solution comprising the steps of (a) passing the solution through an ion exchanger having an ion exchange resin charged with cations selected from the group of ammonium ions and hydrogen ions, in order to remove the cationic impurities from the solution; (b) regenerating the exchange resin by passing a saturated ammonium sulfate regenerant solution therethrough in which 4-10 bed volumes of saturated ammonium sulfate regenerant solution are used to regenerate the ion exchange resin; (c) resaturating the regenerant solution passing from the ion exchanger by adding NH 3 and (NH 4 )2SO 4 to obtain a resaturated ammonium regenerant solution, and filtering; (d) subsequently recycling the resaturated ammonium regenerant solution to the ion exchanger.
Claim 18
Independent Claim 126 words
A method for removing cationic impurities from a wet process phosphoric acid solution comprising the steps of (a) passing the solution through an ion exchanger having an ion exchange resin charged with cations selected from the group of ammonium ions and hydrogen ions, in order to remove the cationic impurities from the solution; (b) regenerating the exchange resin by passing a saturated ammonium sulfate regenerant solution therethrough in which 4-10 bed volumes of saturated ammonium sulfate regenerant solution are used to regenerate the ion exchange resin; (c) resaturating the regenerant solution passing from the ion exchanger by adding NH 3 and (NH 4 )2SO 4 to obtain a resaturated ammonium regenerant solution, and filtering; (d) subsequently recycling the resaturated ammonium regenerant solution to the ion exchanger.
Claim 19
Dependent Claim 42 words
The method of claim 15 including the additional step of passing a dilute solution of sulfuric acid through the ion exchanger to replace ammonium ions with hydrogen ions obtaining an effluent of dilute ammonium sulfate solution, and thereafter recovering the ammonia therefrom.

References Cited (Backward Citations)

US2628165A Cited
US4511675A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-08-28 1993-02-27 1993-08-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-08-28 1997-02-27 1997-08-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-08-28 2001-02-27 2001-08-29 $7700.00 Window Closed / Lapsed

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