Abstract:
The invention relates to a method for producing a crystalline hydroxylamine-O-sulfonic acid wherein a) hydroxylamine or a hydroxylammonium salt is reacted with oleum/sulfuric acid or with chlorosulfuric acid/sulfuric acid at a temperature in the region of between 90 to 130 °C, b) the reaction mixture is subsequently mixed for between 2 to 24 hours at a temperature in the region of between 90 to 130°C, c) the reaction mixture is cooled for between 1 to 12 hours at a temperature in the region of between 10 to 40 °C and d) the crystallised hydroxylamine-O-sulfonic acid is subsequently separated and washed.
Abstract:
Procedimiento para la obtención de ácido hidroxilamin-O-sulfónico, caracterizado porque a. se disuelve sulfato hidroxilamónico en ácido sulfúrico, y se añade con dosificación oleum en un intervalo de tiempo de 0,2 a 4 horas, a una temperatura en el intervalo de 105 a 115ºC, b. una vez concluida la adición de oleum, la mezcla de reacción se agita de modo subsiguiente durante un intervalo de tiempo de 6 a 10 horas a una temperatura en el intervalo de 105 a 115ºC, c. a continuación se enfría la mezcla de reacción en el intervalo de 6 a 9 horas a una temperatura en el intervalo de 20 a 30ºC, y d. los cristales de ácido hidroxilamin-O-sulfónico formados se separan por filtración y se lavan con benzoato de metilo, y a continuación con acetato de etilo.
Abstract:
A process for preparing crystalline hydroxylamine-O-sulfonic acid by a. reacting hydroxylamine or a hydroxylammonium salt with oleum/sulfuric acid or with chlorosulfonic acid/sulfuric acid at a temperature in the range from 90 to 130° C., b. continuing to stir the reaction mixture at a temperature in the range from 90 to 130° C. for a period of from 2 to 24 hours, c. cooling the reaction mixture to a temperature in the range from 10 to 40° C. within a period of from 1 to 12 hours and d. subsequently removing and washing the hydroxylamine-O-sulfonic acid which has crystallized out.