Patent ID: 9079926
Filing Date: 2015-07-14
Classification: C07F

Abstract:
1. A process for working up a salt-containing residue from a preparation of an amino-functional organosilane of the formula (Ia): wherein R groups are the same or different and R is hydrogen or a linear or branched alkyl group having 1 to 4 carbon atoms; R′ groups are the same or different and R′ is hydrogen or a linear or branched alkyl group having 1 to 8 carbon atoms or an aryl group; R″ groups are the same or different and R″ is a linear or branched alkyl group having 1 to 8 carbon atoms or an aryl group; Z is a bivalent alkyl group selected from the group consisting of —CH n is 0, 1, 2, or 3; and z is 0, 1, or 2, wherein the salt-containing residue comprises at least one component selected from the group consisting of an ammonium halide and an organic amine hydrohalide, the process comprising: (1) reacting at least one halogen-functional organosilane of the formula (II) wherein X is Cl, Br, or I; Z is a bivalent alkyl group from the group of —CH R′ groups are the same or different and R′ is a hydrogen or a linear or branched alkyl group having 1 to 8 carbon atoms or an aryl group; R″ groups are the same or different and R″ is a linear or branched alkyl group having 1 to 8 carbon atoms, or an aryl group; and n is 0, 1, 2, or 3, wherein R groups are the same or different and R is hydrogen or a linear or branched alkyl group having 1 to 4 carbon atoms; and z is 0, 1 or 2, thereby obtaining a crude preparation of an amino-functional organosilane of the formula (Ia), and (2) subsequently separating the salt-containing residue by processing the crude preparation of the amino-functional organosilane and working up the obtained salt-containing residue by a process comprising: (A) adding an nonpolar organic solvent and an aqueous alkali to the salt-containing residue to give a mixture; (B) allowing the mixture to react and yield an aqueous phase and an organic phase; (C) then separating the aqueous phase from the organic phase, comprising the nonpolar organic solvent; and (D) removing the nonpolar organic solvent from the organic phase, thereby obtaining a remaining organic phase comprising bis- and tris-amino-functional organosilanes, wherein the nonpolar organic solvent is added to the salt-containing residue after a distillation of the crude product, while stirring, wherein the aqueous alkali is added and said aqueous alkali is a strong aqueous alkali, wherein the aqueous alkali is a sodium hydroxide solution or potassium hydroxide solution, wherein the mixture is allowed to react with mixing up to 30 minutes so that to form the aqueous phase and the organic phase, and wherein the nonpolar organic solvent is added and is toluene.