Preparation method and device of trimethyl borate-10
A technology of trimethyl borate and esterification reaction, applied in the field of trimethyl boron-10 acid, can solve the problems of large loss of trimethyl borate, difficulty in single treatment, complicated process, etc. Beautiful, good separation effect
Inactive Publication Date: 2014-01-22
TIANJIN UNIV +1
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The invention relates to a preparation method and device of trimethyl borate-10. The preparation method comprises the steps of adding reactants into a reaction kettle, taking methanol as a solvent, and stirring for reacting for 30-45h; setting the reaction temperature to be 50-70 DEG C, and performing esterification reaction to generate trimethyl borate-10; performing azeotropic distillation on an esterification reaction product, and setting the temperature to be 70-90 DEG C; collecting a fraction at the temperature of 50-60 DEG C, then continuously heating, and recovering methanol; adding the fraction collected in azeotropic distillation into an extraction and distillation tower kettle; heating the tower kettle, controlling the heating voltage to be 120-150V and controlling the total reflux time to be 20-30min according to the total reflux speed to meet a heat load of a system, adding an extraction agent N, N-dimethylformamide or dimethyl sulfoxide or a mixed extraction agent into a high-level tank at the tower top of a distillation tower, and collecting trimethyl borate at the temperature of 67-68.5 DEG C at the tower top. The operation of the method is stable, and the purity of trimethyl borate-10 obtained by the method can be above 99%.
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