Authors: BorkinaG.G., VoroninaS.G., DoroshenkoM.A., ProkhorenkoV.S., KhudiakovaE.V., A.L. Perkel’

Title of the article: The gas-chromatographic determination of N-hydroxyphthalimide the catalyst of the processes of liquid-phase oxidation

Year: 2018, Issue: 3, Pages: 62-69

Branch of knowledge: Chemical technology

Index UDK: 543.544.3

DOI: 10.26730/1999-4125-2018-3-62-69

Abstract: N-hydroxyphthalimide (N-GFI) is widely used as the catalyst of the oxidation processes of organic compounds by molecular oxygen to hydroperoxide compounds and other valuable oxychemicals. The low solubility of N-GFI in non-polar organic substrates even at high temperatures and a possibility of the destructive disintegration complicate working with it and require analytical monitoring. The possibility of the N-GFI con-tent determination is studied by the gas-chromatographic method. N-GFI itself is not defined directly because of high polarity of a molecule. The possibilities of determination of N-GFI in the form of O-alkylic and O-acylic derivatives are considered. O-alkylic derivatives were supposed to be received on Vilyamson's reaction or processing by diazoalkanes (diazomethane). The first approach was inapplicable during the work in semi-micro-scale. When processing N-GFI by diazomethane, the formed N-methoxyphthalimide reacts with an excess of diazomethane. It leads to decreased yield of N-MOFI. Quantitative results were received at application of phthalimide as the internal standard (technique No. 1). O-acylic derivatives were received in acetylation of N-GFI by acetic anhydride in the pyridine medium (technique No. 2). The influence of temperature on the solubility of N-hydroxyphthalimide in p-xylene, n-decane, cyclohexanone and a mixture of cyclohexanone with chlorobenzene was studied by means of technique No. 1.

Key words: N-hydroxyphthalimide N-methoxyphthalimide N-acetoxyphthalimide gas chromatographic determination gas liquid chromatography

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