Diacetylene-containing poly-siloxane and method for preparing same
A butadiynyl polysilazane and phenyl technology, which is applied in the field of conjugated polymers and its preparation, can solve the problems of difficult processing, poor solubility, high rigidity, etc., achieve excellent performance, increase ceramic yield, and produce high rate effect
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Embodiment 1
[0018] Example 1, preparation of butadiynyl-containing polysilazane (R, R' in formula I are methyl, m, n are 1.4, 4.0)
[0019] In a 250ml three-necked flask, add 50ml tetrahydrofuran, and 20ml n-BuLi (2.5mol / L), under N 2 Under the protection of air, slowly drop the mixed solution of 50ml tetrahydrofuran and 2.0ml hexachlorobutadiene into the three-necked flask at -78°C. After the dropwise addition, keep the temperature at low temperature and continue to stir for 2 hours, then gradually raise the temperature to 20° C. and continue to stir for 10 hours to obtain an off-white turbid butadiynyl dilithium salt solution.
[0020] Add 100ml tetrahydrofuran and 0.125mol Me 2 SiCl 2 , use a low temperature bath to keep the system at -5°C, N 2 Slowly drop the turbid solution of butadiynyl dilithium salt under protection. After the dropwise addition, continue to stir at -5°C for 2 hours, raise the system to 20°C and continue to stir for 10 hours. Leave to stand and separate layers. ...
Embodiment 2
[0034] Example 2, preparation of butadiynyl-containing polysilazane (R, R' in formula I are phenyl, methyl respectively, m, n are 2.3, 2.7)
[0035] In a 250ml three-necked flask, add 50ml of toluene, and 20ml of n-BuLi (2.5mol / L), in N 2 Under air protection, a mixed solution of 50 ml of toluene and 2.0 ml of hexachlorobutadiene was slowly dropped into the three-necked flask at -40°C. After the dropwise addition, keep the temperature at low temperature and continue to stir for 2 hours, then gradually raise the temperature to 20° C. and continue to stir for 10 hours to obtain an off-white turbid butadiynyl dilithium salt solution.
[0036] Add 100ml toluene and 0.125mol MePhSiCl to a 500ml three-necked flask 2 ,, keep the system at -70°C with a low temperature bath, N 2 Slowly drop the turbid diacetylenyl dilithium salt solution under protection. After the dropwise addition, stir and react at -70°C for 10 hours, raise the system to 0°C and continue to stir for 36 hours. Leav...
Embodiment 3
[0050] Example 3, preparation of butadiynyl-containing polysilazane (R, R' in formula I are phenyl, m, n are 4.9, 1.6)
[0051] In a 250ml three-necked flask, add 50ml of ether and 20ml of n-BuLi (2.5mol / L), under N 2 Under the protection of air, slowly drop the mixed solution of 50ml tetrahydrofuran and 2.0ml hexachlorobutadiene into the three-necked flask at -78°C. After the dropwise addition, keep the temperature at low temperature and continue to stir for 2 hours, then gradually raise the temperature to -10°C and continue to stir for 20 hours to obtain an off-white turbid butadiynyl dilithium salt solution.
[0052] Add 100ml tetrahydrofuran and 0.125mol Ph 2 SiCl 2 , use a low temperature bath to keep the system at -5°C, N 2 Slowly drop the turbid solution of dilithium dilithium salt under protection. After the dropwise addition, stir and react at -5°C for 2 hours, raise the system to 100°C and continue to stir for 3 hours. Leave to stand and separate layers. The upper...
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