A kind of method of synthesizing difluorooxalate lithium borate by one-step method
A technology of difluorooxalate lithium borate and lithium oxalate, which is applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. Lithium is expensive, tail gas treatment is cumbersome, etc., and the production cost is low, the product yield is high, and the three wastes are less.
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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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