Method for producing coated bleach activator granules

Abstract

The present invention relates to methods for coating bleach activator-containing granules by treatment with an acidic aqueous consolidating solution, comprising polymeric polycarboxylate and/or alkali metal phosphonate as coating and consolidation active ingredient, with simultaneous drying in a fluidized-bed apparatus.

What is claimed:  
     
         1 . A method for producing a bleach-activator-coated particulate preparation, comprising a compound according to formula (I):  
       
         
           
           
               
               
           
         
       
       wherein: 
 R 1  is —H, —CH 3 , optionally substituted (C 2 -C 24 )-alkyl radical, optionally substituted (C 2 -C 24 )-alkenyl radical, optionally substituted alkyl radical containing a (C 1 -C 24 )-alkyl group, or optionally substituted alkenylaryl radical containing a (C 1 -C 24 )-alkyl group;  
 R 2  and R 3  are independently —CH 2 —CN, —CH 3 , —CH 2 —CH 3 , —CH 2 —CH 2 —CH 3 , —CH(CH 3 )—CH 3 , —CH 2 —OH, —CH 2 —CH 2 —OH, —CH(OH)—CH 3 , —CH 2 —CH 2 —CH 2 —OH, —CH 2 —CH(OH)—CH 3 , —CH(OH)—CH 2 —CH 3 , or —(CH 2 CH 2 —O) n H;  
 R 4  and R 5  are independently —H, —CH 3 , optionally substituted (C 2 -C 24 )-alkyl radical, optionally substituted (C 2 -C 24 )-alkenyl radical, optionally substituted alkyl radical containing a (C 1 -C 24 )-alkyl group, optionally substituted alkenylaryl radical containing a (C 1 -C 24 )-alkyl group, CH 2 —CN, —CH 2 —CH 3 , —CH 2 —CH 2 —CH 3 , —CH(CH 3 )—CH 3 , —CH 2 —OH, —CH 2 —CH 2 —OH, —CH(OH)—CH 3 , —CH 2 —CH 2 —CH 2 —OH, —CH 2 —CH(OH)—CH 3 , —CH(OH)—CH 2 —CH 3 , or —(CH 2 CH 2 —O) n H;  
 n is an integer of 1, 2, 3, 4, 5 or 6;  
 X (−)  is a charge-balancing anion; 
 wherein said particulate is produced by the steps of:  
 a) spraying said compound of formula (I) onto a carrier material to produce a carrier-coated-compound, and b) drying said carrier-coated-compound in a fluidized-bed apparatus with an acidic aqueous solution comprising a coating and consolidation active ingredient; or  
 c) mixing said compound of formula (I) with an organic or inorganic carrier material in an aqueous solution, and d) optionally removing the aqueous solvent under reduced pressure and elevated temperature.  
 
 
     
     
         2 . The method of  claim 1 , wherein R 1 , R 2 , and R 3  are the same.  
     
     
         3 . The method of  claim 1 , wherein R 1 , R 2 , and R 3  are —CH 3 .  
     
     
         4 . The method of  claim 1 , wherein 1 or 2 of said R 1 , R 2 , and R 3  radicals are —CH 3  and at least one of said R 1 , R 2 , and R 3  radicals contains 2 or more carbon atoms.  
     
     
         5 . The method of  claim 1 , wherein X (−)  is halide, nitrate, hydroxide, phosphate, hydrogenphosphate, dihydrogenphosphate, pyrophosphate, metaphosphate, hexafluorophosphate, carbonate, hydrogencarbonate, sulfate, hydrogensulfate, (C 1 -C 20 )-alkyl sulfate, (C 1 -C 20 )-alkylsulfonate, optionally (C 1 -C 18 )-alkyl-substituted arylsulfonate, chlorate, perchlorate, an anion of (C 1 -C 24 )-carboxylic acid, or combinations thereof.  
     
     
         6 . The method of  claim 1 , wherein X (−)  is chloride, sulfate, hydrogensulfate, methosulfate, ethosulfate, (C 12 -C 18 )-alkyl sulfate, (C 12 -C 16 )-alkyl sulfate, or (C 13 -C 15 )-alkyl sulfate, lauryl sulfate, dodecylbenzenesulfonate, toluenesulfonate, cumenesulfonate, xylenesulfonate or combinations thereof.  
     
     
         7 . The method of  claim 1 , wherein said particulate has a diameter in the range of from about 0.4 mm to about 3 mm.  
     
     
         8 . The method of  claim 1 , wherein said carrier material is alkali metal cumenesulfonate, surfactant, organic acid, organic polymer, alkali metal carbonate, alkali metal sulfate, alkali metal hydrogensulfate, alkali metal hydrogencarbonate, alkali metal phosphate, alkali metal dihydrogenphosphate, dialkali metal hydrogenphosphate, alkali metal silicate, silicas, silica gel, silica clay, or combinations thereof.  
     
     
         9 . The method of  claim 1 , wherein the internal surface area of said carrier material is in the range of from about 10 m 2 /g to about 500 m 2 /g.  
     
     
         10 . The method of  claim 1 , wherein said carrier material particle size in the range of from about 100 μm to about 1.5 mm.  
     
     
         11 . The method of  claim 1 , further comprising the steps of: 
 e) preparation of an aqueous solution comprising cationic nitrile and optionally alkali metal cumenesulfonate;    f) optional adjustment of the solution to an acidic pH;    g) atomization and drying of the solution in a fluidized-bed apparatus;    h) optional powdering of the resulting primary granules in the fluidized bed;    i) spraying the resulting optionally powdered granules with an aqueous consolidation and coating solution, and simultaneous drying in the same or optionally in a downstream second fluidized-bed apparatus;    j) discharging the granules from the fluidized-bed apparatus and optionally separating the granules into acceptable granules and coarse/fine granules;    k) optionally returning fine granules and/or ground coarse granules to the fluidized bed in step g); and    l) optionally returning fine granules and/or ground coarse granules to the powdering step of step h).    
     
     
         12 . The method of  claim 11 , wherein said cationic nitrile is present in a range of from about 10% by weight to about 90% by weight.  
     
     
         13 . The method of  claim 11 , wherein said cationic nitrile is present in a range of from about 15% by weight to about 50% by weight.  
     
     
         14 . The method of  claim 11 , wherein said alkali metal cumenesulfonate is sodium cumenesulfonate.  
     
     
         15 . The method of  claim 11 , wherein the pH is adjusted to an acidic value by the addition of sulfuric acid, citric acid or combinations thereof.  
     
     
         16 . The method of  claim 11 , wherein the pH is in the range of from about 4 to about 4.4.  
     
     
         17 . The method of  claim 11 , wherein said primary granules are powdered with silica, zeolite, alkali metal cumenesulfonate, or combinations thereof.  
     
     
         18 . The method of  claim 11 , wherein said primary granules are powdered with Na cumenesulfonate.  
     
     
         19 . The method of  claim 11 , wherein said aqueous consolidation and coating solution comprises polymeric polycarboxylate, phosphonic acid, alkali metal phosphonate, or combinations thereof.  
     
     
         20 . The method of  claim 11 , wherein said polymeric polycarboxylate is polymerization products of acrylic acid, methacrylic acid, maleic acid, or copolymers of at least two of the polymerization products, in at least partially neutralized form.  
     
     
         21 . The method of  claim 11 , wherein said granules are coated with an amount of said aqueous consolidation and coating solution in the range of from about 1% by weight of granules to about 25% by weight of granules.  
     
     
         22 . The method of  claim 11 , wherein said granules are coated with an amount of said aqueous consolidation and coating solution in the range of from about 2% by weight of granules to about 15% by weight of granules.  
     
     
         23 . The method of  claim 11 , wherein said granules are separated by sieving.  
     
     
         24 . The method of  claim 11 , wherein the bulk density of the coated particulate preparation is in the range of from about 300 g/l to about 1000 g/l.  
     
     
         25 . The method of  claim 11 , wherein the bulk density of the coated particulate preparation is in the range of from about 400 g/l to about 800 g/l.  
     
     
         26 . The method of  claim 11 , wherein the proportion of compound according to formula (I) in the coated particulate preparation is in the range of from about 10% by weight to about 90% by weight.  
     
     
         27 . The method of  claim 11 , wherein the proportion of compound according to formula (I) in the coated particulate preparation is in the range of from about 15% by weight to about 50% by weight.  
     
     
         28 . A particulate detergent or cleaner prepared by the method of  claim 1 .  
     
     
         29 . A particulate detergent or cleaner prepared by the method of  claim 11 .  
     
     
         30 . The particulate detergent or cleaner of  claim 28 , wherein said coated particulate is present in a range of from about 0.1% by weight to about 10% by weight.  
     
     
         31 . The detergent or cleaner of  claim 28 , wherein said coated particulate is present in a range of from about 0.2% by weight to about 7% by weight.  
     
     
         32 . The detergent or cleaner of  claim 29 , wherein said coated particulate is present in a range of from about 0.1% by weight to about 10% by weight.  
     
     
         33 . The detergent or cleaner of  claim 29 , wherein said coated particulate is present in a range of from about 0.1% by weight to about 10% by weight.