Synthesis method and application of aluminum bis(oxalato) borate
A bisoxalate aluminum borate and bisoxalate borate technology, applied in the field of electrochemical materials, can solve problems such as high cost, limited service life, and large safety hazards, and achieve short reaction time, simple and easy-to-operate reaction conditions, and high yield Effect
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Embodiment 1
[0023] S1, weigh 20.83 g oxalic acid, 4.74 g boric acid, 1.99 g aluminum hydroxide;
[0024] S2. Heat and dry the weighed oxalic acid at 100°C for 3 h in vacuum, and heat and dry boric acid and aluminum hydroxide at 65°C for 3 h without vacuum;
[0025] S3. Put the dried oxalic acid, boric acid, and aluminum hydroxide in a round-bottomed flask, shake well (about 1 hour), press into tablets at 10 Mpa, transfer to a beaker, place in a vacuum drying oven, and react at 120 °C After 30 min, vacuumize to 0.07 Mpa, and react at a temperature of 150 °C for 12 h to obtain a white solid;
[0026] S4. The obtained white solid was transferred to 500 mL of acetonitrile, stirred for 15 min and then filtered, and the obtained filtrate was evaporated at 65°C to obtain about 12.7 g of aluminum bisoxalate borate with a primary conversion rate of about 84.7% and a purity of about 98.5%.
[0027] The infrared spectrogram of the double oxalate aluminum borate prepared by the present embodiment i...
Embodiment 2
[0029] S1, weigh 19.33 g oxalic acid, 4.74 g boric acid, 1.99 g aluminum hydroxide;
[0030] S2. The weighed oxalic acid was heated and dried under vacuum at 110°C for 3 h, and the boric acid and aluminum hydroxide were heated at 65°C for 3 h without vacuum;
[0031] S3. Put the dried oxalic acid, boric acid, and aluminum hydroxide in a round bottom flask, shake well (about 1 hour), press 10 Mpa into tablets, transfer to a beaker, place in a vacuum drying oven, and react at 120 °C After 45 min, vacuumize to 0.07 Mpa, and react at a temperature of 150 °C for 12 h to obtain a white solid;
[0032] S4. Transfer the obtained white solid into 500 mL of dimethyl carbonate, stir for 15 min and then filter, evaporate the solvent from the obtained filtrate at 65°C to obtain about 11.5 g of aluminum bisoxalate borate, with a primary conversion rate of about 76.7% , the purity is about 99%.
[0033] figure 2 The XRD spectrum of the aluminum bisoxalate borate prepared in this example ...
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