Polymerizable composition containing reactive fluorinated silicone compound
A technology of polymeric composition and reactive silicone, applied in the direction of instruments, optics, optical components, etc., can solve the problems of inability to guarantee heat resistance, high refractive index, low Abbe number, etc.
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Embodiment 1
[0257] [Example 1] Production of reactive fluorine-containing organosilicon compound (F-SC)
[0258] Into a 200 mL eggplant-shaped flask equipped with a condenser, 43.3 g (0.200 mol) of diphenylsilanediol [manufactured by Tokyo Chemical Industry Co., Ltd.], trimethoxy(4-vinylphenyl)silane [Shin-Etsu Chemical Co., Ltd. Co., Ltd.] 44.0 g (0.196 mol), trimethoxy(3,3,3-trifluoropropyl) silane [Shin-Etsu Chemical Co., Ltd.] 0.873 g (0.004 mol), and toluene 35 g, nitrogen gas The bulb replaced the air in the flask with nitrogen. The reaction mixture was heated to 50°C, and 38 mg (0.2 mmol) of barium hydroxide monohydrate [manufactured by Aldrich] was added thereto. In this way, it stirred at 50 degreeC for 1 hour, and further stirred at 85 degreeC for 5 hours, and dealcoholized and condensed. The reaction mixture was cooled to room temperature (about 25° C.), and insoluble matter was removed using a membrane filter with a pore size of 0.2 μm. Using a rotary evaporator, toluene an...
manufacture example 1
[0260] [Production Example 1] Production of Reactive Silicone Compound (SC)
[0261] Into a 1 L eggplant-shaped flask equipped with a condenser, 177 g (0.80 mol) of diphenylsilanediol [manufactured by Tokyo Chemical Industry Co., Ltd.], trimethoxy(4-vinylphenyl) silane [Shin-Etsu Chemical Co., Ltd. Co., Ltd.] 179 g (0.80 mol) and toluene 141 g, and the air in the flask was replaced with nitrogen gas using a nitrogen balloon. This reaction mixture was heated to 50° C., 0.303 g (1.6 mmol) of barium hydroxide monohydrate [made by Aldrich] was added, and stirring was further carried out at 50° C. for 2 days to perform dealcoholation condensation. The reaction mixture was cooled to room temperature (about 25° C.), and insoluble matter was removed using a membrane filter with a pore size of 0.2 μm. Using a rotary evaporator, toluene and by-product methanol were distilled off from the reaction mixture under reduced pressure at 50° C. to obtain 305 g of a colorless and transparent oi...
Embodiment 2
[0263] [Example 2] Preparation of polymerizable composition
[0264] 60 parts by mass of F-SC produced in Example 1 as a reactive organosilicon compound, 30 parts by mass of FDA as a (meth)acrylate compound, 5 parts by mass of BPEA and 5 parts by mass of TMP3A, and as a polymerization initiator 3 parts by mass of POO were mixed, stirred and defoamed at 2,000 rpm for about 30 minutes until it became uniform, and polymerizable composition 1 was prepared.
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