Verfahren zur Herstellung von Hydrazoniumsalzen

• Main Authors: RAHLFS,ERICH,DR, THRAUM,WERNER,DR, HENRICH,GUENTER,DR
• Format: Patent
• Language: German
• Published: 30.11.1963
• Subjects: CHEMISTRY; COMPOUNDS THEREOF; INORGANIC CHEMISTRY; METALLURGY; NON-METALLIC ELEMENTS; PERFORMING OPERATIONS; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL; SEPARATION; TRANSPORTING

<PICT:0839819/III/1> Hydrazonium salts are prepared by acid decomposition of aqueous solutions containing the reaction products of hydrazine hydrate and acetone, wherein distillation of the acetone liberated gradually by the action of the acid is effected in stages, each of which is preceded by a delay period interposed to allow for the liberation of an amount of acetone to be distilled off in the next succeeding distillation stage. Aqueous hydrazine/acetone solution and an acid, e.g. sulphuric acid pass in stoichiometric proportions from storage vessels 1 and 2 respectively into mixing vessel 3 at the rate for the total mixture of 1 litre/hour. Hydrazonium salt solution freed from acetone in proportion of 5-10X the volume of the mixture is charged into vessel 3 from one of the final delay vessels 6 by pump 4. The resulting aqueous mixture is charged continuously to the upper fractionating column 5 operated under such conditions that some acetone, possibly containing a little hydrazine, distils off and is collected in a receiver. The aqueous solution, partially free from acetone, collects in an upper delay vessel 6 until sufficient quantity is present to pass through a second fractionating column 5 where further quantities of acetone formed during the delay period are removed by distillation. The process may be repeated several times as indicated in the Figure, an aqueous solution of hydrazonium salt free from acetone collecting finally in sump 7.