Hydrogen Sulfide → 3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy-

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Reaction Steps

A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in molten form is then metered in through a fine nozzle. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content.

Provenance & Evidence