Process for preparing bis(silylorganyl)-polysulfanes

• Main Authors: MUENZENBERG, JOERG, PANSTER, PETER, PRINZ, MATTHIAS
• Format: Patent
• Language: English; French; German
• Published: 01.09.1999
• Edition: 6
• Subjects: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM; CHEMISTRY; COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSESC01D OR C01F; COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM,RUBIDIUM, CAESIUM, OR FRANCIUM; COMPOUNDS THEREOF; INORGANIC CHEMISTRY; METALLURGY; NON-METALLIC ELEMENTS; ORGANIC CHEMISTRY

A method for the preparation of bis(silyl-organyl)-poly-sulphane of formula (I) comprises reacting halo(alkyl)alkoxysilane of formula (II) with a polysulphide of formula (III): (R R R SiR )2Sx (I) R R R SiR X (II) M2Sx (III) R -R = 1-8C alkyl, 1-8C alkoxy or aryl (preferably phenyl, toluyl or benzyl); R = 1-8 (1-4)C alkylidene or (CH2)n-C6H4-(CH2)n-; n = 1-4; x = greater than 1 (2-8) for (I), or 2-8 for polysulphide; X = halogen, eg. Cl, Br or I; and M = alkali metal cation or an alkaline earth metal or zinc cation equivalent, with the provision that at R -R<3)<s) is an alkoxy group. In the first step dry polysulphide is prepared by reacting a sulphide of formula (IV) containing water of crystallisation with sulphur at 60-300 degrees C under vacuum, in the absence of an organic solvent: M2Sx-z (IV) z = 1-7; and (x - z) ≥ 1. Also claimed are: (i) dry polysulphide prepared by the above method; and (ii) mixtures of dry polysulphides of formula (V) in which the average poly-sulphane chain length in the polysulphides is greater than 1 and less than or equal to 8: M2Sy (V) y = 1-8.