GB1110184A - Electrolytic process for preparing cyclohexylhydroxylamine - Google Patents

Abstract

Cyclohexylhydroxylamine is produced by electrolytic reduction at a chosen voltage of nitro-cyclohexane suspended in an electrolyte of pH 2 to 11 and precipitating out the cyclohexylhydroxy-lamine so formed. Typically the process is effected in a cell divided into two compartments by a regenerated cellulose or porous porcelain diaphragm with a cathode of zinc, lead, tin or preferably mercury; an anolyte of an aqueous solution of sodium and ammonium bicarbonates; a catholyte of sodium and ammonium bicarbonates, a non-ionic surfactant such as an alkylphenol-ethylene oxide condensate, and nitrocyclohexane dispersed by stirring; and with an applied cathode voltage which is at -1.4 to -1.7 volts with respect to a mercury-mercurous sulphate saturated potassium sulphate reference electrode. A carbon anode may be employed. Whilst acid pH may be used, the catholyte is preferably of pH 7 to 9.5 since these conditions cause precipitation and crystallization of the reduced product. The operating temperature is 20 to 60 DEG C., at the higher temperatures the product subliming and being thus removed from the bath. The process may be made continuous by adding further nitrocyclohexane.