Composition for regenerating an ion exchange resin

Abstract

A method and composition for removing perchlorate from a highly selective ion exchange resin is disclosed. The disclosed approach comprises treating the resin in a solution of super critical or liquid carbon dioxide and one or more quaternary ammonium chloride surfactant compounds.

What is claimed is:  
     
         1 . A process for regenerating a spent ion exchange resin, the process comprising the steps of: 
 a) providing a quantity of a spent ion exchange resin, said resin having a plurality of reaction sites, at least some of said sites containing a perchlorate anion;    b) creating a solution comprising liquid or supercritical carbon dioxide and at least one chloride containing surfactant compound, said compound comprising at least one chloride ion;    c) maintaining the temperature and pressure of said solution at a level so as to maintain said solution in a liquid phase;    d) contacting said resin with said solution thereby causing an exchange of said resin perchlorate ions for said surfactant chloride ions, thereby providing a regenerated resin; and    f) removing said solution and recovering said resin.    
     
     
         2 . The process of  claim 1 , further including the step of washing said recovered resin, comprising washing with liquid or supercritical carbon dioxide.  
     
     
         3 . The process of  claim 1 , wherein the resin is a polymer backbone and a plurality of sites containing chloride anions.  
     
     
         4 . The process of  claim 1 , wherein said resin comprises a plurality of small particles.  
     
     
         5 . The process of  claim 4 , wherein said particles are beads.  
     
     
         6 . The process of  claim 4 , wherein said particles have a 3 dimensional shapes comprising spheres, rods, or prismatic polyhedrons, or some combination of said 3 dimensional shapes.  
     
     
         7 . The process of  claim 1 , wherein the chloride containing surfactant is an ammonium chloride salt.  
     
     
         8 . The process of  claim 7 , wherein the ammonium chloride salt is a quaternary ammonium chloride salt.  
     
     
         9 . The process of  claim 8 , wherein the quaternary ammonium chloride salt contains functional groups.  
     
     
         10 . The process of  claim 9 , wherein the ammonium chloride salt is selected from the list consisting of benzyl dimethyl ammonium chloride, (Aliquat 336, CAS Reg. No. 5137-55-3); didecyl dimethyl ammonium chloride (CAS Reg. No 7173-51-5); n-alkyl(60% C 14 , 25% C 12 , 15% C 16 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68424-85-1); n-alkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) dimethyl ammonium chloride (CAS Reg. No 68391-01-5); n-alkyl(68% C 12 , 32% C 14 ) dimethyl ethylbenzyl ammonium chloride (CAS Reg. No 68956-79-6); n-dialkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) methyl benzyl ammonium chloride (CAS Reg. No 68391-05-9); and combinations thereof.  
     
     
         11 . The process of  claim 1  wherein the surfactant is present in the solution up to a point at which said solution reaches saturation.  
     
     
         12 . The process of  claim 1  wherein the quantity of solution used to treat the resin is less than 40 bed volumes.  
     
     
         13 . The process of  claim 12 , wherein the solution passes over and through the resin bed at about 1 bed volume every 3 minutes.  
     
     
         14 . The process of  claim 1 , wherein the solution comprises a quantity of a simple alcohol, said alcohol having 1-4 carbon atoms per molecule.  
     
     
         15 . The process of  claim 14 , wherein the alcohol is ethanol.  
     
     
         16 . The process of  claim 15 , wherein the ethanol is present in the solution at a concentration from about 10 v / o  to about a saturation limit.  
     
     
         17 . A process for regenerating a spent ion exchange resin, the process comprising the steps of: 
 a) providing a quantity of a spent ion exchange resin, said resin having a plurality of reaction sites, at least some of said sites containing a perchlorate anion;    b) creating a solution comprising water and at least one quaternary ammonium chloride surfactant compound, said compound further comprising at least one chloride ion;    d) contacting and stirring said resin in said solution thereby causing an exchange of said resin perchlorate ions for said surfactant chloride ions;    e) separating said solution from said resin and repeating step d) at least once;    f) removing said solution and washing said resin free of residual surfactant thereby providing a regenerated resin.    
     
     
         18 . The process of  claim 17 , wherein said step of washing comprises washing with liquid or supercritical carbon dioxide.  
     
     
         19 . The process of  claim 17 , wherein the resin is a polymer backbone and a plurality of sites containing chloride anions.  
     
     
         20 . The process of  claim 17 , wherein said resin comprises a plurality of small particles.  
     
     
         21 . The process of  claim 20 , wherein said particles are beads.  
     
     
         22 . The process of  claim 20 , wherein said particles have a 3 dimensional shapes comprising spheres, rods, or prismatic polyhedrons, or some combination of said 3 dimensional shapes.  
     
     
         23 . The process of  claim 17 , wherein the chloride containing surfactant is selected from the list consisting of benzyl dimethyl ammonium chloride, (Aliquat 336, CAS Reg. No. 5137-55-3); didecyl dimethyl ammonium chloride (CAS Reg. No 7173-51-5); n-alkyl(60% C 14 , 25% C 12 , 15% C 16 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68424-85-1); n-alkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68391-01-5); n-alkyl(68% C 12 , 32% C 14 ) dimethyl ethylbenzyl ammonium chloride (CAS Reg. No 68956-79-6); n-dialkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) methyl benzyl ammonium chloride (CAS Reg. No 68391-05-9); and combinations thereof.  
     
     
         24 . The process of  claim 17 , wherein the surfactant is present in the solution in a weight ratio of between about 10 w / o  to about 50 w / o .  
     
     
         25 . The process of  claim 24 , wherein the quantity of solution used to treat the resin is less than 60 bed volumes.  
     
     
         26 . The process of  claim 25 , wherein the solution is allowed to contact the resin for less than 24 hours.  
     
     
         27 . The process of  claim 17 , wherein the solution contains a quantity of a simple alcohol, said alcohol having 1-4 carbon atoms per molecule.  
     
     
         28 . The process of  claim 27 , wherein the alcohol is ethanol.  
     
     
         29 . The process of  claim 28 , wherein the ethanol is present in the solution at a concentration from about 10 v / o  to about a saturation limit.  
     
     
         30 . A composition for regenerating a spent ion exchange resin, comprising: 
 liquid carbon dioxide; and    a chloride containing surfactant.    
     
     
         31 . The composition of  claim 30 , wherein the chloride containing surfactant is an ammonium chloride salt.  
     
     
         32 . The composition of  claim 31 , wherein the ammonium chloride salt is a quaternary ammonium chloride salt.  
     
     
         33 . The composition of  claim 32 , wherein the quaternary ammonium chloride salt contains functional groups.  
     
     
         34 . The composition of  claim 30 , wherein the chloride containing surfactant is at least one surfactant selected from the list consisting of benzyl dimethyl ammonium chloride, (Aliquat 336, CAS Reg. No. 5137-55-3); didecyl dimethyl ammonium chloride (CAS Reg. No 7173-51-5); n-alkyl(60% C 14 , 25% C 12 , 15% C 16 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68424-85-1); n-alkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68391-01-5); n-alkyl(68% C 12 , 32% C 14 ) dimethyl ethylbenzyl ammonium chloride (CAS Reg. No 68956-79-6); n-dialkyl(60% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) methyl ammonium chloride (CAS Reg. No 68391-05-9); and combinations thereof.  
     
     
         35 . A composition for regenerating a spent ion exchange resin, comprising: 
 supercritical carbon dioxide; and    a chloride containing surfactant.    
     
     
         36 . The composition of  claim 35 , wherein the chloride containing surfactant is an ammonium chloride salt.  
     
     
         37 . The composition of  claim 36 , wherein the ammonium chloride salt is a quaternary ammonium chloride salt.  
     
     
         38 . The composition of  claim 37 , wherein the quaternary ammonium chloride salt contains functional groups.  
     
     
         39 . The composition of  claim 35 , wherein the chloride containing surfactant is at least one surfactant selected from the list consisting of benzyl dimethyl ammonium chloride, (Aliquat 336, CAS Reg. No. 5137-55-3); didecyl dimethyl ammonium chloride (CAS Reg. No 7173-51-5); n-alkyl(60% C 14 , 25% C 12 , 15% C 16 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68424-85-1); n-alkyl(6% C 14 , 30% C 16 , 5% C 12 , 5% C 18 ) dimethyl benzyl ammonium chloride (CAS Reg. No 68391-01-5); n-alkyl(68% C 12 , 32% C 14 ) dimethyl ethylbenzyl ammonium chloride (CAS Reg. No 68956-79-6); n-dialkyl(60% C 14 , 30% C 16 , 5% C 12 %, C 18 ) methyl benzyl ammonium chloride (CAS Reg. No 68391-05-9); and combinations thereof.  
     
     
         40 . The composition of  claim 30 , further including ethanol.  
     
     
         41 . The composition of claim  40 , wherein the surfactant is present in the solution up to a point at which said solution reaches saturation.  
     
     
         42 . The composition of  claim 35 , further including ethanol.  
     
     
         43 . The composition of claim  42 , wherein the surfactant is present in the solution up to a point at which said solution reaches a point of saturation.