Preparation method for synthesis of nitrogen heterocycle modified silicone resin by dehydrogenation coupling reaction
A technology of dehydrocoupling and nitrogen heterocycle, which is applied in organic chemistry, organic silicon compounds, chemical instruments and methods, etc., can solve problems such as excessive salt waste, dangerous reaction conditions, and low polymer yield, and achieve improved durability High temperature performance, effect of improving mechanical properties
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Embodiment 1
[0031] Step 1: All experimental operations were carried out using the Schlenk technique under a dry argon atmosphere or in a glove box under a nitrogen atmosphere. 16.428 g of triethoxysilane and 10.716 g of benzylamine were dissolved in a two-neck reaction flask, and 32 mg of Ru was added. 3 (CO) 12 Fully dissolved in a nitrogen-protected two-necked reaction flask, vigorously stirred in an oil bath at 120 °C for 24 h, and after the reaction was completed, nitrogen-heterocycle-modified organosilane was obtained, which was stored at low temperature.
[0032] Step 2: Weigh 21.06 g of ultrapure water and 0.211 g of tetramethylammonium hydroxide and dissolve each other in a three-necked reaction flask. Weigh out 2.904 g of dimethyldiethoxysilane, 1.900 g of diphenyldimethoxysilane, 9.776 g of methyltrimethoxysilane, 6.213 g of phenyltrimethoxysilane, and 5.79 g of nitrogen heterocycle-modified organic Silane was added dropwise to the three-necked reaction flask in turn, stirred ...
Embodiment 2
[0035] Step 1: All experimental operations were carried out using the Schlenk technique under a dry argon atmosphere or in a glove box under a nitrogen atmosphere. 16.428 g of triethoxysilane, 15.02 g of 2-aminobenzothiazole, and 20 g of DMSO were dissolved in a two-neck reaction flask, and 32 mg of Ru was added. 3 (CO) 12 Fully dissolved in a nitrogen-protected two-necked reaction flask, vigorously stirred in an oil bath at 120 °C for 24 h, and after the reaction was completed, nitrogen-heterocycle-modified organosilane was obtained, which was stored at low temperature.
[0036] Step 2: Weigh 21.06 g of ultrapure water and 0.211 g of tetramethylammonium hydroxide and dissolve each other in a three-necked reaction flask. Weigh out 2.904 g of dimethyldiethoxysilane, 1.900 g of diphenyldimethoxysilane, 9.776 g of methyltrimethoxysilane, 6.213 g of phenyltrimethoxysilane, and 12.92 g of nitrogen heterocycle-modified organic Silane was added dropwise to the three-necked reaction...
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