Preparation method and application of a photosensitive silicone resin containing polyurethane bridged polysilsesquioxane
A polysilsesquioxane and polyurethane bridging technology, which is applied in semiconductor devices, electrical components, circuits, etc., can solve unsatisfactory problems, such as the large difference in the solubility parameters of polysiloxane and polyurethane, and achieve Good flexibility and air tightness, good bonding effect
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Embodiment 1
[0037] (1) Add 3-isocyanatopropyltrimethoxysilane (41.056 g, 0.2mol) for about 0.5h, after the dropwise addition, react at 30°C for 4h to prepare 132.056g of acetone solution of coupling agent with polyurethane segment.
[0038] (2) Add dropwise a mixed solution of 108 g of dioxane, 10.8 g of distilled water and 0.66 g of potassium carbonate to the coupling agent with polyurethane segments obtained in (1) at 20°C, and after 2 hours of dripping, Seal it, and stir the hydrolysis-condensation reaction at 20°C for 24 h, then filter to remove potassium carbonate, and evaporate to dryness under reduced pressure to obtain 52.256 g of hydroxyl-terminated polysilsesquioxane containing polyurethane bridge.
[0039] (3) In a 2L dry and clean three-necked flask, add 52.256g of hydroxyl-terminated polysilsesquioxane containing polyurethane bridge and 27.93g of methacryloxypropyltrimethoxysilane obtained in (2), 93.05g Dimethyldimethoxysilane, 136.2 g methyltrimethoxysilane and 300 g tolue...
Embodiment 2
[0043] (1) To a clean three-neck flask containing PTMG-2000 (200 g, 0.1 mol) and 125 g tetrahydrofuran dehydrated under reduced pressure at 105°C for 2 hours, add 3-isocyanatopropyltriethoxy dropwise at 60°C Silane (49.4 g, 0.2 mol) was used for about 0.5 h. After the dropwise addition was completed, it was reacted at 60°C for 2 h, and then tetrahydrofuran was distilled off under reduced pressure to prepare 374.4 g of a tetrahydrofuran solution of a coupling agent with a polyurethane segment.
[0044] (2) Add a mixed solution of 1080g of dioxane, 10.8g of distilled water and 5.457g of sodium carbonate dropwise to the coupling agent with polyurethane segment obtained in (1) at 0°C, and seal it after 2 hours. , and stirred the hydrolysis-condensation reaction at 0° C. for 72 hours, then filtered to remove sodium carbonate, and evaporated to dryness under reduced pressure to obtain 235.6 g of hydroxyl-terminated polysilsesquioxane containing polyurethane bridges.
[0045] (3) In ...
Embodiment 3
[0049] (1) Add PTMG-1000 (50 g, 0.05 mol), PTMG-1800 (90 g, 0.05 mol), 355 g of dichloromethane and 200 g of petroleum ether to a clean three-necked flask that has been dehydrated under reduced pressure at 105 °C for 2 hours. , add 3-isocyanatopropyltrimethoxysilane (20.528 g, 0.1mol) and 3-isocyanatopropyltriethoxysilane (24.7 g, 0.1mol) dropwise at 40°C for about 0.5h, and the addition is complete After reacting at 40°C for 6 hours, 740.2 g of a solution of a coupling agent with polyurethane segments was obtained.
[0050] (2) Add a mixed solution of 100g of dioxane, 432g of distilled water and 5.457g of potassium hydroxide dropwise to the coupling agent with polyurethane segment obtained in (1) at 20°C, and after 1.5 hours of dripping, Seal it, and stir the hydrolysis-condensation reaction at 20°C for 48 hours, then filter to remove potassium hydroxide, and evaporate to dryness under reduced pressure to obtain 171.4 g of hydroxyl-terminated polysilsesquioxane containing pol...
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