US2004210083A1PendingUtilityA1

Process for production of essentially chloride-free calcium sulfonate

37
Priority: Apr 17, 2003Filed: Apr 17, 2003Published: Oct 21, 2004
Est. expiryApr 17, 2023(expired)· nominal 20-yr term from priority
Inventors:Abraham Robert De KrakerSteven HolmesKrishna Rangraj Kaushik
C07C 303/32C10M 135/10C10N 2030/04C10M 2219/046C10M 2219/044C10N 2070/00C10M 159/24
37
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Claims

Abstract

The invention relates to a process for the preparation of a low-base number calcium sulfonate that is essentially chloride free. The process involves preparing a sulfonic acid solution by adding a solvent to sulfonic acid, removing dissolved or entrained SO 2 or SO 3 , mixing the solution with a specific amount of water and calcium hydroxide, heating the mixture, separating out excess calcium hydroxide and calcium salts from the mixture, and recovering solvent and oil to capture the calcium sulfonate product.

Claims

exact text as granted — not AI-modified
We claim:  
     
         1 . A process for the production of low base number calcium sulfonate comprising: 
 a. preparing a sulfonic acid solution by adding about 1 to about 20 volumes of a miscible solvent to sulfonic acid and removing dissolved or entrained SO 2  or SO 3  if present;    b. mixing the sulfonic acid solution with about 1 to about 5 moles of water per mol of sulfonic acid and about 1 to about 10 moles of calcium hydroxide per mole of sulfonic acid to create a reaction mixture;    c. heating the reaction mixture with stirring to between about 40° C. and about 200° C.;    d. separating excess calcium hydroxide and calcium salts of mineral acid from the reaction mixture; and,    e. recovering solvent and oil to make a final essentially chloride free calcium sulfonate product.    
     
     
         2 . The process of  claim 1  in which the final calcium sulfonate product has a viscosity of between about 10 cSt/100° C. and about 100 cSt/100° C.  
     
     
         3 . The process of  claim 1  in which the solvent is heptane.  
     
     
         4 . The process of  claim 1  in which the dissolved or entrained SO 2  or SO 3  is removed via stripping with nitrogen.  
     
     
         5 . The process of  claim 4  in which the sulfonic acid is centrifuged prior to stripping.  
     
     
         6 . The process of  claim 1  in which the amount of water is from about 1 to about 3 mol/mol of sulfonic acid.  
     
     
         7 . The process of  claim 1  in which the amount of calcium hydroxide is about 1 to about 5 mol/mol of sulfonic acid.  
     
     
         8 . The process of  claim 1  in which the reaction temperature is from about 80° C. to about 140° C.  
     
     
         9 . The process of  claim 1  in which the reaction mixture is mixed for a period of time up to 60 minutes.  
     
     
         10 . The process of  claim 1  in which the reaction mixture is mixed for a period of time up to 30 minutes.  
     
     
         11 . The process of  claim 1  in which excess calcium hydroxide is separated from the reaction mixture by centrifugation.  
     
     
         12 . The process of  claim 11  in which the centrifugation is performed for less than about 20 minutes.  
     
     
         13 . The process of  claim 1  in which the product after solvent removal is further concentrated by a method selected from the group consisting of distillation and vacuum flashing.  
     
     
         14 . The process of  claim 1  in which the process is performed continuously.  
     
     
         15 . The process of  claim 1  in which the solvent is heptane, the sulfonic acid is centrifuged prior to removing the dissolved or entrained SO 2  or SO 3  via stripping with nitrogen, the amount of water is from about 1 to about 3 mol/mol of sulfonic acid, the amount of calcium hydroxide is about 1 to about 5 mol/mol of sulfonic acid, the reaction temperature is from about 80° C. to about 140° C., the reaction mixture is mixed for a period of time up to 30 minutes, excess calcium hydroxide is removed by centrifugation, and the product after solvent removal is further concentrated by a method selected from the group consisting of distillation and vacuum flashing.  
     
     
         16 . The process of  claim 15  in which the process is performed continuously.  
     
     
         17 . The process of  claim 15  in which the centrifugation to remove excess calcium hydroxide is performed for less than about 20 minutes.  
     
     
         18 . The process of  claim 15  in which the final calcium sulfonate product has a viscosity of between about 10 cSt/100° C. and about 100 cSt/100° C.  
     
     
         19 . The process of  claim 18  in which the process is performed continuously.  
     
     
         20 . The process of  claim 19  in which the product is further concentrated by distillatio

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