Borazine aryne resin and preparation method thereof
A technology of aryne resin and borazine, which is applied in the field of functional polymer materials, can solve the problems that the dielectric properties and high temperature resistance cannot meet the needs of hypersonic aircraft, VLSI and chips, and achieve excellent durability. Effects of thermal performance, low dielectric constant, and low dielectric loss
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Embodiment 1 3
[0036] The synthesis of embodiment 1 trichloroborazine (TCB)
[0037] 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 oxygen removal by vacuuming and passing nitrogen, add NH 4 Cl powder 32g (0.30mol) and toluene 300ml, and vigorously stirred to form a suspension, heated to 110 ° C, slowly into the four-necked flask BCl 3 Gas, heat preservation reaction at this temperature for 10h, and cool to room temperature. Then use shleck technology to filter under nitrogen protection, transfer the filtrate to a rotary evaporator, and distill off the solvent under reduced pressure to obtain colorless needle-shaped crystals of trichloroborazine (TCB). The infrared spectrum is as follows: figure 1 shown.
Embodiment 2 3
[0038] Example 2 Synthesis of Triallyl Trichloroborazine (TV-TCB)
[0039] 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 oxygen removal by vacuuming and nitrogen, add BCl 3 (0.09mol) of toluene solution, cooled to -10°C with salt ice, and slowly added dropwise a mixture of 18.22g (0.18mol) of triethylamine and toluene (20mL), and then added olefin Propylamine 5.14g (0.09mol) and toluene (10mL), then the system was slowly raised to 110°C for 6h, then cooled to room temperature. The shleck technique was used for suction filtration under the protection of nitrogen, the filtrate was transferred to a rotary evaporator, and the solvent was distilled off under reduced pressure to obtain a colorless and transparent liquid triallyl trichloroborazine (TV-TCB). The infrared spectrum was as follows: figure 1 shown.
Embodiment 3
[0040] Example 3 Synthesis of borazine aryne resin (PBZA-1)
[0041] (1) In a 500ml four-necked flask equipped with nitrogen conduit, stirrer, thermometer and condenser tube, add NH 4 Cl powder 32g (0.30mol) and toluene 300ml, and vigorously stirred to form a suspension, heated to 110 ° C, slowly into the four-necked flask BCl 3 Gas, heat preservation reaction at this temperature for 10h, and cool to room temperature. Then, the shleck technique was used for suction filtration under the protection of nitrogen, the filtrate was transferred to a rotary evaporator, and the solvent was distilled off under reduced pressure to obtain colorless needle-shaped crystals of trichloroborazine (TCB).
[0042] (2) Under nitrogen protection, add magnesium powder 3.20g (0.13mol) / tetrahydrofuran (80ml) into a 500ml four-neck flask, cool with a cold water bath, add bromoethane (EtBr) dropwise through a constant pressure funnel The mixed solution of 13.08g (0.12mol) and tetrahydrofuran (30ml) w...
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