Siloxane bridged ladderlike polysiloxane and preparation method thereof
The technology of siloxane bridge and polysiloxane is applied in the field of siloxane bridge ladder polysiloxane and its preparation, which can solve the difficulty of organic polymer performance, the reduced flexibility of the ladder double chain and the high brittleness of the polymer. problem, to achieve the effect of good optical performance, high strength and high flexibility
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Embodiment 1
[0040] Preparation of siloxane bridging ladder polysiloxane by phenyltrichlorosilane and diphenyldihydroxysilane.
[0041] (1) Under the protection of dry nitrogen, put 50.8 grams (0.24 moles) of phenyltrichlorosilane, 150 grams of toluene, and 150 grams of tetrahydrofuran into a multi-necked flask equipped with a condenser tube and a dropping funnel, and stir evenly; Add 26.0 grams (0.12 moles) of diphenyldihydroxysilane to the multi-neck flask in batches at -10°C, and add 26 grams (0.26 moles) of triethylamine dropwise at the same time; after the addition, gradually raise the temperature to 60 ℃ reaction for 1 hour; after stopping the reaction, filter the solution, collect the clear liquid, and obtain an intermediate solution; concentrate the obtained intermediate solution by distillation to obtain an intermediate solution with a concentration of about 30wt%;
[0042] (2) At a temperature of 0°C, add 2.88 grams (0.16 moles) of water and 40.5 grams (0.4 moles) of triethylamin...
Embodiment 2
[0045] Via phenyltrichlorosilane, vinyltrichlorosilane and HO(MePhSiO) 5 H Preparation of siloxane bridging ladder polysiloxane.
[0046] (1) Under the protection of dry nitrogen, 31.7 grams (0.15 moles) of phenyltrichlorosilane, 24.2 grams (0.15 moles) of vinyltrichlorosilane were placed in a multi-necked flask equipped with a condenser tube and a dropping funnel and 500 grams of toluene, stir evenly; at -10 ° C, 83.9 grams of HO (MePhSiO) 5 H (0.12 mol) was added to the multi-neck flask in batches, and 60.7 g (0.6 mol) of triethylamine was added dropwise at the same time; after the dropwise addition, the temperature was gradually raised to 60°C for 3 hours; after the reaction was stopped, the solution was filtered, Collect the supernatant to obtain an intermediate solution;
[0047] (2) At a temperature of 25°C, add 9 grams (0.5 moles) of water and 60.7 grams (0.6 moles) of triethylamine (molecular weight: 101.19) dropwise to the intermediate solution obtained in step (1)....
Embodiment 3
[0050] Via methyltrichlorosilane, 3-acryloyloxytrichlorosilane and HO(MePhSiO) 3 H Preparation of siloxane bridging ladder polysiloxane.
[0051] (1) Under the protection of dry nitrogen, 17.9 grams (0.06 moles) of methyltrichlorosilane and 29.7 grams (0.18 moles) of 3-acryloyloxy 300 grams of trichlorosilane and cyclohexanone, stirred evenly; 51.2 grams of HO(MePhSiO) 3 H (0.12 mol) was added to the multi-neck flask in batches, and 60.7 g (0.6 mol) of triethylamine was added dropwise; after the dropwise addition, the temperature was gradually raised to 60°C for 5 hours; after the reaction was stopped, the solution was filtered, Collect the clear liquid to obtain an intermediate solution; the obtained intermediate solution is concentrated by distillation and then added toluene to obtain an intermediate solution with a concentration of about 30wt%;
[0052] (2) At a temperature of 25°C, add 21.6 grams (1.2 moles) of water and 0.18 grams (0.002 moles) of triethylamine dropwise...
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