OBTAINING METHOD FOR HIGH PURITY CRYSTAL OF HYDROXYLAMINE SULFATE FROM REACTION SOLUTION BY SULFITE PROCESS

摘要

PURPOSE:To obtain pure hydroxylamine sulfate from a hydrolyzed soln. by a sulfite process in a high yield by adding a mixt. of alkali and alcohol to a mixed soln. of hydroxylamine sulfate, ammonium sulfate and sulfuric acid and further adding sulfuric acid. CONSTITUTION:A soln. prepared by allowing sulfur dioxide gas to be absorbed in an aq. soln. of ammonium nitrite and acidic ammonium sulfite is heated and hydrolyzed to form a mixed soln. of hydroxylamine sulfate, ammonium sulfate and sulfuric acid. To this hydrolyzed soln. is added a mixt. of alkali and methanol and/or ethanol, whereby hydroxylamine ions are dissolved in the aq. alcohol soln. as free hydroxylamine, and most of the ammonium sulfate is separated as crystals from the soln. By adding sulfuric acid to the soln. hydroxylamine sulfate crystals are obtd.