Redox catalyst oxidant, catalyst and polymerization therewith

Claim 1

A method of preparing a composite suitable as an oxidizing component in a redox aqueous emulsion polymerization initiator which consists essentially of the steps of (A) obtaining the oxidation product of reacting p-diisopropylbenzene with oxygen at a temperature in the range of about 105° C. to about 120° C. to a sufficient conversion that said product has about 40 to about 70 percent hydroperoxide content according to ASTM No. E-298-68 and is comprised of a mixture of p-disopropylbenzene mono- and dihydroperoxide, unreacted p-diisopropylbenzene, and oxygenated byproducts containing aqueous emulsion diene polymerization inhibitors, (B) removing by a separation procedure, selected from at least one of crystallization and fractionation, followed by subsequent filtration, a major portion of said p-diisopropylbenzene dihydroperoxide, and treating a portion of the filtrate by fractionation to a pot temperature in the range of about 70° C. to about 110° C. to remove p-diisopropylbenzene and a portion of said p-diisopropylbenzene monohydroperoxide distillate to effect a concentration of the remainder as a distilland having an equivalent monohydroperoxide content by ASTM No. E-298-68 in the range of about 70 percent to about 90 percent comprised, by weight of about 45 to about 65 percent p-diisopropylbenzene monohydroperoxide, about 5 to about 15 percent p-diisopropylbenzene dihydroperoxide and about 10 to about 30 percent oxygenated byproducts, (C) forming a solid/liquid two-phase product by mixing with 100 parts by weight of said remainder distilland, at a temperature in the range of about 15° C. to about 50° C., about 50 to about 400 parts by weight of at least one liquid, non-polar saturated hydrocarbon selected from at least one of n-hexane, isohexane, n-heptane, isoheptane, n-octane, isoctane, n-decane, cyclopentane, cyclohexane, cycloheptane and cyclooctane (D) recovering said liquid phase by filtration, (E) treating 100 parts by weight of said liquid phase by mixing therewith, at a temperature in the range of about 15° C. to about 50° C., about 50 to about 400 parts by weight aqueous sodium or potassium hydroxide solution containing about 0.5 to about 15 weight percent sodium or potassium hydroxide and allowing the mixture to equillibrate to form an organic/aqueous two-phase product, (F) recovering said organic phase by draining or decantation, (G) treating 100 parts of the recovered organic phase one to three times with about 50 to about 400 parts by weight dilute aqueous sodium hydroxide solution containing about 1 to about 4 weight percent sodium hydroxide to form an organic/aqueous two-phase product by the method of Step (E) and (H) recovering the final organic phase.

Claim 2

A method of preparing a composite suitable as an oxidizing component in a redox aqueous emulsion polymerization initiator which consists essentially of the steps of (A) obtaining the oxidation product of reacting p-diisopropylbenzene with oxygen at a temperature in the range of about 105° C. to about 120° C. to a sufficient conversion that said product has about 40 to about 70 percent hydroperoxide content according to ASTM No. E-298-68 and is comprised of a mixture of p-disopropylbenzene mono- and dihydroperoxide, unreacted p-diisopropylbenzene, and oxygenated byproducts containing aqueous emulsion diene polymerization inhibitors, (B) removing by a separation procedure, selected from at least one of crystallization and fractionation, followed by subsequent filtration, a major portion of said p-diisopropylbenzene dihydroperoxide, and treating a portion of the filtrate by fractionation to a pot temperature in the range of about 70° C. to about 110° C. to remove p-diisopropylbenzene and a portion of said p-diisopropylbenzene monohydroperoxide distillate to effect a concentration of the remainder as a distilland having an equivalent monohydroperoxide content by ASTM No. E-298-68 in the range of about 70 percent to about 90 percent comprised, by weight of about 45 to about 65 percent p-diisopropylbenzene monohydroperoxide, about 5 to about 15 percent p-diisopropylbenzene dihydroperoxide and about 10 to about 30 percent oxygenated byproducts, (C) forming a solid/liquid two-phase product by mixing with 100 parts by weight of said remainder distilland, at a temperature in the range of about 15° C. to about 50° C., about 50 to about 400 parts by weight of at least one liquid, non-polar saturated hydrocarbon selected from at least one of n-hexane, isohexane, n-heptane, isoheptane, n-octane, isoctane, n-decane, cyclopentane, cyclohexane, cycloheptane and cyclooctane (D) recovering said liquid phase by filtration, (E) treating 100 parts by weight of said liquid phase by mixing therewith, at a temperature in the range of about 15° C. to about 50° C., about 50 to about 400 parts by weight aqueous sodium or potassium hydroxide solution containing about 0.5 to about 15 weight percent sodium or potassium hydroxide and allowing the mixture to equillibrate to form an organic/aqueous two-phase product, (F) recovering said organic phase by draining or decantation, (G) treating 100 parts of the recovered organic phase one to three times with about 50 to about 400 parts by weight dilute aqueous sodium hydroxide solution containing about 1 to about 4 weight percent sodium hydroxide to form an organic/aqueous two-phase product by the method of Step (E) and (H) recovering the final organic phase.