A kind of preparation method of high ceramic yield polycarborane
A technology of polycarborane and ceramics, which is applied in the field of preparation of high ceramic yield polycarborane, and can solve the problems of lack of boron carbide hollow microsphere preparation process, retention, lack of high ceramic yield boron carbide precursor, etc.
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Embodiment 1
[0022] This embodiment includes the following steps:
[0023] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:1; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero and repeat it three times to remove the air and moisture in it, and then pre-cool the reactor to -20°C;
[0024] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 4mol / L;
[0025] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a heating rate of 1.5°C / min. 2 Under the protection of the atmosphere, the reaction was continuously stirred, the stirring rate was 150r / min, and the reaction was carried out for 24h;
[0026] (4) in N 2 Under the protection of the atmospher...
Embodiment 2
[0029] This embodiment includes the following steps:
[0030] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:0.5; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero, repeat three times to remove the air and moisture, and then pre-cool the reactor to -15°C;
[0031] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 3mol / L;
[0032] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a rate of 1°C / min. 2 Under the protection of the atmosphere, continue to stir the reaction, the stirring rate is 60r / min, and the reaction is 20h;
[0033] (4) in N 2 Under the protection of the atmosphere, the temperature of the system was raised to ...
Embodiment 3
[0036] This embodiment includes the following steps:
[0037] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:2; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero and repeat it three times to remove the air and moisture in it, and then pre-cool the reactor to -25°C;
[0038] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 5mol / L;
[0039] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a heating rate of 2°C / min. 2 Under the protection of the atmosphere, the reaction was continuously stirred, the stirring rate was 240r / min, and the reaction was 28h;
[0040] (4) in N 2 Under the protection of the atmosphere, the temperature...
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