Before the experiment, reactive pure-grade toluene was dried and distilled at atmospheric pressure. 4-Methoxytoluene, 2-, 3-, and 4-phenoxytoluenes and 4-phenyltoluene were synthesized by procedures described in the literature [4, 5]. According to gas-liquid chromatography data, purity >95%. Experiments were carded out in a reactor with a 1200 x 20 mm contact tube of 1Khl8N9T stainless steel. Reaction products were collected in acetone-sprayed and water-cooled scrubbers. The design of the laboratory unit was described in more detail in [6]. Oxide catalysts (a sintered vanadium-titanium catalyst, a vanadium-antimony catalyst, an alumina-supported and cosupported vanadium-titanium-antimony-chromium catalyst) were prepared by known procedures [7-9]. The main products of oxidative ammonolysis of toluene, 4-methoxytoluene, 2-, 3and 4phenoxytoluenes and 4-phenyltoluene were benzonitrile and respectively 4-methoxy-, 2-, 3and 4-phenoxyand 4-phenylbenzonitriles, and also carbon oxides and hydrogen cyanide. All the aromatic nitriles were isolated from the catalysts in pure form. Their physicochemical properties were in agreement with published characteristics. Quantitative analysis of unreacted initial substances and the nitriles corresponding to them was carried out by means of gasliquid chromatography on a Khrom-3 instrument. The 1000 x 3 mm separating column of molybdenum glass was filled with a phase prepared from DS-550 silicone elastomer applied to N-AW-DMCS Chromaton (0.20-0.35 mm) in a quantity of 5% of the mass of stationary phase. Carbon oxides were determined by gas chromatography on an LKhM-8MD instrument.
In the oxidative ammonolysis of o-xylene on oxide catalysts, phthalimide can be obtained from phthalodinitrile through an intermediate phthalocyanine step. The catalyst ability to form phthalocyanine can be used to estimate its selectivity to phthalimide.
AbstractIn Gemischen von Acetaldehyd (I) mit Olefinen (Molverhältnis wie 5: I) entstehen bei der Oxidation mit Luft‐O, in Gegenwart von Co‐acetat die Radikale (II).
AbstractDurch Luftoxidation von Durylenglykol (I) an geschmolzenem Di‐V‐pentoxid bei 400‐420°C läßt sich Pyromellitsäureanhydrid (II) (Ausbeute 52%) darstellen.