Hydrolysis resistant organomodified disiloxane surfactants
A technology of organosilicon and solvents, which is applied in the direction of silicon organic compounds, biocides, animal repellents, etc.
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preparation Embodiment 1
[0100] 1-(2-Trimethylsilylethyl)-1,1,3,3-tetramethyldisiloxane (Structure 1). A 250 mL round bottom flask was charged with tetramethyldisiloxane (51.6 g) and Wilkinson's catalyst ((PPh 3 ) 3 RhCl, 100 ppm), stirred under nitrogen, and warmed to 60 °C. Trimethylvinylsilane (25.6 g) was charged to the addition funnel and added dropwise at a rate such that the reaction temperature was maintained R : M R m R . Fractional distillation of the resulting material under vacuum (about 30 mm Hg) afforded 51.6 g of M'M R Product, 99.1% GC purity. The Si-H content of the product was found to be 96cc H by gasiometric titration. 2 / g.
[0101] Structural Formula 1
[0102]
preparation Embodiment 2
[0104] 1-(3,3-Dimethylbutyl)-1,1,3,3-tetramethyldisiloxane (Structure 2). A 250 mL round bottom flask was charged with tetramethyldisiloxane (46.1 g) and stirred under nitrogen. A solution of Karstedt's catalyst (Pt(0) in divinyltetramethyldisiloxane, 10 ppm) in 3,3-dimethyl-1-butene (19.3 g) was charged to the addition funnel , added dropwise at a rate such that the reaction temperature was kept R Product and M R m R By-products (32:53:9). The resulting material was fractionated under vacuum (about 30 mm Hg) using a 25-cm Vigreux column to give 25.0 g M'M R Product, >98.1% GC purity. The Si-H content of the product was found to be 100cc H by gas titration 2 / g.
[0105] Structural formula 2
[0106]
preparation Embodiment 3
[0108] 1-(2-methylpropyl)-1,1,3,3-tetramethyldisiloxane (Structure 3). Tetramethyldisiloxane (10.0 g), toluene (10.0 g) and Wilkinson's catalyst ((PPh 3 ) 3 RhCl, 40ppm), stirred, and heated to 60°C. The bottle was manifolded and pressurized (25 psig) with isobutylene and maintained at 60-70°C for 8 hours. The pressure was vented and the reaction was sampled for GC analysis; residual tetramethyldisiloxane, M'M R Product and M R m R By-products (2:95:3). The resulting material was stripped at 40°C under vacuum (about 150 mm Hg) to remove olefins and M'M', then filtered through celite to give 21.3 g of M'M R Product / toluene solution, 94% GC purity. The Si-H content of the product was found to be 11cc H by gas titration 2 / g.
[0109] Structural formula 3
[0110]
PUM
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