Nitrobenzene → Nitrobenzene

A mixture of nitrobenzene and nitrogen, preheated to 396° C., was continuously conducted through a glass pipe with an inside diameter of 1 cm and a length of about 50 cm, which contained 16 cc of a freshly prepared Pb/Mn catalyst (catalyst preparation 1) in the form of 1 mm spherules. The throughput was 27 g/hour (0.22 mol) of nitrobenzene and 45 Nlit/hour of nitrogen. After leaving the reaction pipe, which, by means of electrical heating, was kept practically isothermally at 396° C., the reaction mixture was indirectly cooled with water to 25° C. and the constituents of low volatility were separated. The small quantities of compounds with low volatility still present in the exhaust gas were subsequently absorbed by a washer filled with dioxane. A nitrobenzene conversion of 17% was obtained under these conditions, whereby nitrosobenzene had been formed with a selectivity of 89%. The remainder of the solution was composed of azobenzene, azoxybenzene and aniline. The reactor was operated continuously for a total of 10 hours, during which it was not possible to determine any decline in the activity of the catalyst. A gas-chromatographic investigation of the exhaust gas showed only carbon dioxide and water in addition to nitrogen, as well as traces of nitrosobenzene and nitrobenzene. The following Table I shows the yields and selectivities in dependence upon the duration of operation.

1. custompreheated to 396° C.
2. customAfter leaving the reaction pipe, which
3. customwas kept practically isothermally at 396° C.
4. customthe constituents of low volatility were separated
5. customThe small quantities of compounds with low volatility still present in the exhaust gas were subsequently absorbed by a washer
6. additionfilled with dioxane

ORD record

ord-771e11ede5144cb286381d8149025a41

Source dataset

uspto-grants-1982_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04317947