A kind of boron trifluoride 2-methylimidazole complex and preparation method thereof
A technology of boron trifluoride and methyl imidazole is applied in the field of boron trifluoride 2-methyl imidazole complex and its preparation, and can solve the problem that there is no efficient preparation of boron trifluoride 2-methyl imidazole complex and other problems, to achieve the effect of being conducive to separation, improving purity and improving fluidity
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[0018] The present invention provides a method of preparing a trifluoride 2-methylimidazole complex, comprising the steps of:
[0019] The boron trifluoride was positively formed into a closed container containing 2-methylimidazole dichloromethane solution, and the complex reaction was carried out to obtain a reaction liquid; the temperature of the complex reaction ≤ 30 ° C;
[0020] The reaction liquid was separated from 0 to 5 ° C, and the solid was dried to give a boron trifluoride 2-methylimidazole complex.
[0021] The present invention first introduces trifluoride into a closed container containing 2-methylimidazole dichloromethane solution to obtain a reaction liquid.
[0022] The present invention is not particularly limited to the preparation method of the 2-methylimidazole dichloromethane solution, and 2-methylimidazole can be dissolved in dichloromethane; in the embodiment of the present invention, 2-A Base imidazole is dissolved in dichloromethane below 30 ° C, the tem...
Embodiment 1
[0039] The cooling water of -5 ° C continuously passed into the jacket of the jacket reaction can, 50 kg of dichloromethane was added to the jacket reaction tank, stirred at a speed of 100 rpm, and the temperature of dichloromethane fell to 20 ~ 30 ° C; 50 kg of 2-methylimidazole was added to the jacket reaction tank, continued to be stirred to dissolve; the resulting solution was lowered to 20 to 30 ° C, then the trifluoride gas was slowly transferred into 41.5 kg, access The speed is accurate in the pressure gauge of the jacket reaction tank (i.e., the main pressure) is accurate; after the addition is completed, the reaction liquid is maintained in a closed jacket reaction tank, and the resulting reaction liquid is lowered. The obtained solid was dried under vacuum conditions at 50 to 60 ° C for 2 h at a vacuum condition of 50 to 60 ° C to obtain a trifluoride 2-methylimidazole complex.
Embodiment 2
[0041] The cooling water of -5 ° C continuously into the jacket of the jacket reaction can, 50 kg of dichloromethane is added to the jacket reaction tank, stirred at a rotational speed of 100 rpm, and the temperature of dichloromethane is reduced to 10 ~ 15 ° C; 50 kg of 2-methylimidazole is added to the jacket reaction tank, continue to stir to dissolve; the resulting solution is lowered to 10 to 15 ° C, then the trifluoride gas is 41.5 kg, which is accessed. The speed is accurate in the pressure gauge of the jacket reaction tank (i.e., the main pressure) is accurate; after the addition is completed, the reaction liquid is maintained in a closed jacket reaction tank, and the resulting reaction liquid is lowered. The obtained solid was dried under vacuum conditions at 50 to 60 ° C for 2 h at a vacuum condition of 50 to 60 ° C to obtain a trifluoride 2-methylimidazole complex.
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