Blocked mercaptosilane hydrolyzates as coupling agents for mineral-filled elastomer compositions
A technology of mercaptosilane and condensation products, which is applied in the direction of silicon organic compounds, compounds of group 5/15 elements of the periodic table, compounds of group 4/14 elements of the periodic table, etc. question
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Embodiment 1
[0321] Example 1 Homogeneous preparation of the condensate of 3-acetylthio-1-propyltriethoxysilane
[0322] The crude starting material of 3-acetylthio-1-propyltriethoxysilane was first refined from sodium ethoxide by flashvacuum distillation. The distillate was distilled again. An initial forecut of volatiles was withdrawn and the bulk of the distillate remained as a clear colorless liquid, which was used as starting material for the preparation of the condensate. Under stirring, to a homogeneous mixture of 3-acetylthio-1-propyltriethoxysilane (74.35 g, 0.2525 mol) and absolute ethanol (70 g) was added an appropriate amount of water (2.27 g, 0.126 mol) . The mixture was left to stand at room temperature for 6 weeks. After this time, volatiles were removed by rotary evaporation.
Embodiment 2
[0323] Example 2 Heterogeneous Preparation of the Condensate of 3-Acetylthio-1-Propyltriethoxysilane
[0324] The crude starting material of 3-acetylthio-1-propyltriethoxysilane was first purified from sodium ethoxide by vacuum flash evaporation. The distillate was distilled again. The initial foreflux of volatiles was withdrawn and the overall distillate remained a clear colorless liquid which was used as starting material for the preparation of the condensate. A biphasic mixture of 3-acetylthio-1-propyltriethoxysilane (68.3 g, 0.232 mol) and water (49 g, 2.7 mol) was stirred at ambient temperature for 6 weeks. Thereafter, the liquid layer was separated from the separatory funnel. Volatiles were removed from the organic phase by rotary evaporation.
Embodiment 3
[0325] Example 3 Homogeneous preparation of 8-octanoylthio-1-propyltriethoxysilane condensate
[0326] 8-Octanoylthio-1-propyltriethoxysilane (240 g, 0.66 mol) was added to a homogeneous mixture of absolute ethanol (54 g) and water (5.93 g, 0.329 mol) with stirring middle. The mixture was allowed to stand at ambient temperature for 6 weeks. After this time, volatiles were removed by rotary evaporation. The product was then purified by vacuum flashing to remove the forestrip and retain the non-volatile portion of the sample. The former contains most of the impurities of ethyl octanoate, 3-mercapto-1-propyltriethoxysilane and 3-chloro-1-propyltriethoxysilane. By comparing with the pure samples of each impurity, the GC (gas chromatography) confirmed. GC analysis results (area%): Si-O-Si siloxane "dimer" of 8-octanoylthio-1-propyltriethoxysilane 46.4%; 8-octanoylthio-1- Propyltriethoxysilane is 33.0%; 1-diethoxy-1-sila-2-thiolane is 0.2%; bis-3-triethoxysilyl-1-propyldi Su...
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Abstract
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