Method for synthesizing lithium difluoro(oxalato) borate by one-step method
A technology of lithium difluorooxalate borate and lithium oxalate is applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. Lithium is expensive, and exhaust gas treatment is cumbersome, resulting in low production cost, high product yield, and less three wastes.
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Embodiment 1
[0025] Preparation of silicon-aluminum composite oxide solid catalyst:
[0026] Add 100 g of silica gel and 100 g of aluminum hydroxide powder into a 500 ml three-neck flask, then add 500 g of distilled water therein, and heat to reflux for 2 hours under vigorous stirring. Cool to room temperature and filter, put the filter cake into a muffle furnace and bake at 500°C for 6 hours, take it out and place it in a nitrogen atmosphere to cool for later use.
[0027] One-step synthesis of lithium difluorooxalate borate:
[0028] Under nitrogen protection, add lithium oxalate 112g (1.1mol), anhydrous oxalic acid 81g (0.9mol), boron trifluoride dimethyl carbonate complex (boron trifluoride content is 43 %) 316g, followed by adding 1000g of dimethyl carbonate solvent with a moisture content of 80ppm, and adding 2.4g of the silicon-aluminum composite oxide solid catalyst prepared above. Stir and react at 40~50°C under normal pressure, acid gas escapes, and the tail gas is absorbed by ...
Embodiment 2
[0031] Under the protection of nitrogen, add 102g (1mol) of lithium oxalate, 90g (1mol) of anhydrous oxalic acid, and 270g of boron trifluoride etherate (47.2% boron trifluoride content) into a dry stirred reaction flask, and then Add 920 g of 1,4-dioxane solvent with a moisture content of 160 ppm, and add 1 g of the silicon-aluminum composite oxide solid catalyst prepared in Example 1. Stir the reaction at 30~35°C under normal pressure, and absorb the tail gas with potassium hydroxide aqueous solution. After reacting for 5 hours, observe the material in the reaction bottle, the solids are obviously reduced, continue the heat preservation reaction for 3 hours, and stop the reaction.
[0032] The reaction solution was lowered to room temperature, filtered under reduced pressure under a nitrogen atmosphere to remove solid catalyst and unreacted solid impurities, the filtrate was concentrated, evaporated and then crystallized, adding petroleum ether to it, stirred and washed, fil...
Embodiment 3
[0034] Under the protection of nitrogen, add 132.5g (1.3mol) of lithium oxalate, 90g (1mol) of anhydrous oxalic acid, and 240g of boron trifluoride acetonitrile complex (62% boron trifluoride content) into a dry stirred reaction flask , then add 500g of acetonitrile solvent with a moisture content of 248ppm, and add 2g of the silicon-aluminum composite oxide solid catalyst prepared in Example 1. Stir the reaction at 75~80°C under normal pressure, and absorb the tail gas with potassium hydroxide aqueous solution. After reacting for 1 hour, observe the materials in the reaction bottle, the solids are obviously reduced, continue the heat preservation reaction for 1 hour, and stop the reaction.
[0035] The reaction solution was lowered to room temperature, and filtered under reduced pressure under a nitrogen atmosphere to remove solid catalysts and unreacted solid impurities. The filtrate was concentrated and evaporated to crystallize, and toluene was added to it for stirring and...
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