A kind of fluorine-containing silicon aryl alkynyl resin and preparation method thereof
A technology of aryl alkynyl and fluorine-containing alkyl, which is applied in the field of preparation of fluorine-containing silicon aryl alkynyl resin
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Embodiment 1
[0040] Embodiment 1 Fluorine-containing silicon aryl alkynyl resin PSAF-1
[0041] In a 500ml four-necked flask equipped with a nitrogen conduit, a stirrer, a thermometer and a condenser tube, after several dehumidification and deoxygenation after vacuuming and nitrogen displacement, under the protection of nitrogen, 3.02g (0.126mol) of magnesium powder / tetrahydrofuran (50ml) was added to a four-neck flask, cooled with an ice-water bath, and then 18.13g (0.12mol) / tetrahydrofuran solution of bromopentane was added dropwise. A solution of 7.56 g (0.06 mol) of diethynylbenzene / tetrahydrofuran was added dropwise, and after the dropwise addition, the reaction was kept at 70°C for 2 hours. The reaction system was cooled to below room temperature, and a 9.50 g (0.045 mol) / tetrahydrofuran solution of trifluoropropylmethyldichlorosilane was added thereto, and the reaction was maintained at 60° C. for 3 hours. Terminate the reaction with an acid, wash with water and take the organic ph...
Embodiment 2
[0047] Example 2 Fluorine-containing silicon aryl alkynyl resin PSAF-2
[0048] In a 500ml four-necked flask equipped with a nitrogen conduit, a stirrer, a thermometer and a condenser tube, after several cycles of dehumidification and deoxygenation through vacuuming and nitrogen displacement, under nitrogen protection, magnesium powder 3.02g (0.126mol) / Methyltetrahydrofuran (60ml) was added to a four-neck flask, cooled with an ice-water bath, and bromoethane 13.08g (0.12mol) / methyltetrahydrofuran (30ml) was added dropwise therein, and then kept at 50°C for 2 hours, and then cooled Afterwards, 7.56 g (0.06 mol) of diethynylbenzene / methyltetrahydrofuran (30 ml) was added dropwise to the reaction system, and the reaction was carried out at reflux temperature (about 80° C.) for 2 hours after the dropwise addition. The system was cooled to below room temperature, and 6.33 g (0.03 mol) of trifluoropropylmethyldichlorosilane / methyltetrahydrofuran (30 ml) was added thereto, followed ...
Embodiment 3
[0049] Example 3 Fluorine-containing silicon aryl alkynyl resin PSAF-3
[0050] In a 500ml four-necked flask equipped with a nitrogen conduit, a stirrer, a thermometer and a condenser tube, after several cycles of dehumidification and deoxygenation after vacuuming and nitrogen displacement, under nitrogen protection, magnesium powder 3.02g (0.12mol) / Methyltetrahydrofuran (60ml) was added into a four-necked flask, cooled with a cold water bath, and bromopentane 18.13g (0.12mol) / methyltetrahydrofuran (30ml) was added thereto, then reacted at 60°C for 2 hours, and then cooled to Diethynylbenzene 7.56g (0.06mol) / methyl tetrahydrofuran (30ml) was added dropwise into the system, and reacted at 70°C for 2 hours. The system was cooled to below room temperature, and 11.63 g (0.02 mol) of perfluorooctylethyltrichlorosilane / methyltetrahydrofuran (30 ml) was added thereto, and the mixture was kept at 70° C. for 2 hours. Terminate the reaction with an acid, wash with water and take the o...
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