Abstract: This invention provides a highly pure and highly concentrated free hydroxylamine aqueous solution substantially not containing any salt or organic substance. This invention is a process for obtaining a free hydroxylamine aqueous solution, comprising the steps of letting an aqueous solution or slurry containing hydroxylammonium sulfate and an alkali react with each other, to obtain an aqueous solution or slurry containing free hydroxylamine and dissolved or partially precipitated sulfates; mixing the obtained reaction solution and a lower alcohol, to precipitate solid sulfates; separating a solution containing the lower alcohol and some of water by distillation from the aqueous solution remaining after separating and removing the solid sulfates; and obtaining a free hydroxylamine aqueous solution from the remaining solution by distillation.

Abstract: This invention provides a process for producing a free hydroxylamine aqueous solution, by letting an alkali react with separated sulfates, for conversion into ammonia and sulfates not containing any nitrogen atom, recovering the valuable ammonia and recycling it in the reaction system for effective use. This invention is a process for producing a free hydroxylamine aqueous solution, in which a free hydroxylamine aqueous solution is obtained by letting an aqueous solution or slurry containing hydroxylammonium sulfate and a gas mainly containing ammonia react with each other, mixing a solution mainly containing a lower alcohol with the produced aqueous solution or slurry, and separating the precipitated sulfates containing ammonium sulfate, comprising the steps of mixing an alkali with the separated sulfates, to produce ammonia gas, and recycling the ammonia in the reaction system.