Synthetic method of tetra(dimethylamino)hafnium
A synthesis method, dimethylamine-based technology, applied in the field of synthesis of metal-organic complexes, can solve the problems of small lithium chloride salt particles, difficulty in separating lithium chloride salt, and difficulty in filtration, so as to simplify operations, reduce costs, Handle simple effects
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[0027] Example 1: Synthesis of tetrakis(dimethylamino)hafnium
[0028] (1) Under an argon atmosphere, add 108 grams of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked flask, stir mechanically, and place the reaction flask between -40°C and -80°C. Drop 800 mL of 2.5 mol / L n-butyl lithium solution into the reaction flask. After the addition, the reaction was stirred for 10 hours.
[0029] (2) Add 160 grams of hafnium tetrachloride to the above reaction system in batches, keeping the temperature of the reaction system not higher than 60°C. After the addition of hafnium tetrachloride, the reaction system is allowed to react for 24-30 hours under the protection of inert gas under mechanical stirring.
[0030] (3) After the reaction is over, the reaction device is directly changed to a distillation device, the solvent in the reaction is removed under one atmospheric pressure, and after the solvent n-hexane is completely removed, vacuum distillation is carried out to col...
Example Embodiment
[0031] Example 2:
[0032] The synthesis method of tetrakis (dimethylamino) hafnium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked flask, stir well, and place the reaction flask at -40°C ,According to the molar ratio of dimethylamine: n-butyllithium of 1.1:1, add the n-butyllithium solution dropwise to the reaction flask, stir and react for 10 hours after the addition is complete; press hafnium tetrachloride: n-butyllithium For a molar ratio of 1:4.1, add hafnium tetrachloride to the above reaction system, keep the temperature of the reaction system at 20°C, after the addition of hafnium tetrachloride, let the reaction system stir and react under the protection of inert gas 24 hours; after the completion of the reaction, remove the solvent of the reaction under one atmosphere pressure, and after the solvent n-hexane is completely removed, distill under reduced pressure to collect the 80-85℃ / 2-5 mmHg fract...
Example Embodiment
[0033] Example 3:
[0034] The synthesis method of tetrakis (dimethylamino) hafnium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked flask, stir well, and place the reaction flask at -80 ℃, according to the molar ratio of dimethylamine: n-butyl lithium of 1.2:1, add the n-butyl lithium solution dropwise to the reaction flask, stir and react for 10 hours after the addition is complete; press hafnium tetrachloride: n-butyl The molar ratio of lithium is 1:4.2, add hafnium tetrachloride to the above reaction system, keep the temperature of the reaction system at 60℃, after adding hafnium tetrachloride, let the reaction system stir under the protection of inert gas Reaction for 30 hours; after the reaction, the solvent of the reaction is removed under one atmosphere pressure, and after the solvent n-hexane is completely removed, distillation is carried out under reduced pressure, and the fraction of 80-85℃ / 2-5 ...
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