Amino alkoxy-modified silsesquioxane adhesives for adhering steel alloy to rubber
A silsesquioxane, aminoalkoxy technology, used in non-polymer organic compound adhesives, adhesives, applications, etc.
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Embodiment 1
[0067] Embodiment 1: Preparation of 3-aminopropyl AMS hydrochloride .
[0068] To a 1 liter flask was added 300 mL of absolute ethanol, 24.42 g of 3-aminopropyltriethoxysilane (110 mmol), 21.6 mL of 12N hydrochloric acid (259 mmol of acid and 900 mmol of water) and 16.6 mL of water (920 mmol). Once mixed, the solution immediately became cloudy, and after standing at room temperature for 3 days, a viscous semi-crystalline mass was obtained. The solvent was decanted, purged with nitrogen to remove residual solvent, and dried under vacuum to give 16.28 g of white crystalline hydrochloride. The theoretical yield (TY) is 16.13 g. The solid was readily dissolved in about 120 mL of distilled water to give 149.69 g of a clear solution containing about 10.8% total solids and having a density of 1.035 g / mL. The AMS concentration of the solution in the silicone was calculated to be 0.761N. The pH is about 1.0. Standard sodium hydroxide titration results showed that the concentratio...
Embodiment 2
[0069] Example 2: Preparation of co- AMS .
[0070] Implementation according to the steps of Example 1, the difference is that the alkoxysilane component is 23.35g 3-aminopropyltriethoxysilane (105.2mmol) and 16.27g 3-mercaptopropyltriethoxysilane (84.6mmol) ). A cloudy solution formed initially which remained unchanged after 18 hours. The solution was heated to 50°C to 60°C with a nitrogen purge to remove most of the solvent to give a white waxy solid that did not change upon drying in vacuo. About 100 mL of water was added, resulting in a slightly cloudy solution, and a small amount (0.56 g) of solid was removed. 130.72 g of solution did not change further on standing. The solution had a density of 1.061 g / mL and a calculated co-AMS concentration of 1.44N. This represents a total solids content of 19.4%. Titration results showed that 0.800N free hydrochloric acid existed in the solution.
Embodiment 3
[0071] Example 3: Preparation of co-AMS salt comprising 3-octanoylthio-1-propyl and 3-aminopropyl in a ratio of 31:69 co-AMS .
[0072] Implementation according to the steps of Example 1, except that the alkoxysilane component is 28.6g 3-aminopropyltriethoxysilane (129.2mmol) and 21.44g 3-octanoylthio-1-propyltriethyl Oxysilane (NXT TM ) (58.8 mmol). A cloudy solution formed initially and remained unchanged after 18 hours. The solution was heated to 50°C to 60°C with a nitrogen purge to remove most of the solvent to give a white waxy solid which after vacuum drying yielded 33.68 g of a white crystalline powder. About 200 mL of water needed to be added to obtain a stirrable mixture. A slightly cloudy fluid solution was obtained after stirring overnight. The 285.9 g solution did not change further on standing, had a density of 1.029 g / mL and a calculated co-AMS concentration of 0.47N. This represents a total solids content of 8.19% based on the theoretical yield of the ...
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