Nonaqueous electrolytic solution containing monofluorophosphate salt and nonaqueous electrolytic solution battery using same
A technology of non-aqueous electrolyte and monofluorophosphate, which is applied in the direction of non-aqueous electrolyte batteries, non-aqueous electrolyte batteries, organic electrolyte batteries, etc., can solve the problem of low solubility and achieve the effect of inhibiting decomposition
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manufacture example 1
[0084] [Production Example 1] Production of lithium methyl monofluorophosphate
[0085] 7.6 g (0.18 mol) of lithium chloride, 25.0 g (0.16 mol) of phosphorus oxychloride, and 62.5 g of dimethyl carbonate were weighed into a 250 mL container made of PFA. Next, 2.9 g (0.16 mol) of pure water was dripped over 30 minutes, stirring at 10 degreeC under nitrogen sealing. After stirring for 30 minutes, 5.2 g (0.16 mol) of anhydrous methanol (water content 0.1%) was slowly added dropwise over 30 minutes while stirring. Furthermore, after stirring for 30 minutes, 34.3 g (0.24 mol in conversion of hydrogen fluoride) of 14% hydrogen fluoride dimethyl carbonate solution was added, and it stirred at 10 degreeC for 30 minutes. Thereafter, stirring was carried out at 120° C. for 1 hour while sealing with nitrogen. After heating at 120°C for 2 hours, the remaining solvent and reaction by-products were distilled off. Then, it was cooled to room temperature to obtain crude lithium methyl mono...
manufacture example 2
[0086] [Production Example 2] Production of lithium ethyl monofluorophosphate
[0087] 7.6 g (0.18 mol) of lithium chloride, 25.0 g (0.16 mol) of phosphorus oxychloride, and 62.5 g of diethyl carbonate were weighed into a 250 mL container made of PFA. Next, 2.9 g (0.16 mol) of pure water was dripped over 30 minutes, stirring at 10 degreeC under nitrogen sealing. After stirring for 30 minutes, 7.4 g (0.16 mol) of absolute ethanol (water content 0.5%) was slowly added dropwise while stirring for 30 minutes. Furthermore, after stirring for 30 minutes, 34.3 g (0.24 mol in conversion of hydrogen fluoride) of 14% hydrogen fluoride dimethyl carbonate solution was added, and it stirred at 10 degreeC for 30 minutes. Thereafter, stirring was carried out at 120° C. for 1 hour while sealing with nitrogen. After heating at 120°C for 2 hours, the remaining solvent and reaction by-products were distilled off. Then, it was cooled to room temperature to obtain crude ethyl monofluorophosphat...
manufacture example 3
[0088] [Production Example 3] Production of lithium hexyl monofluorophosphate
[0089] 7.6 g (0.18 mol) of lithium chloride, 25.0 g (0.16 mol) of phosphorus oxychloride, and 62.5 g of dimethyl carbonate were weighed into a 250 mL container made of PFA. Next, 2.9 g (0.16 mol) of pure water was dripped over 30 minutes, stirring at 10 degreeC under nitrogen sealing. After stirring for 30 minutes, 16.3 g (0.16 mol) of anhydrous n-hexanol was slowly added dropwise while stirring for 30 minutes. Furthermore, after stirring for 30 minutes, 34.3 g (0.24 mol in conversion of hydrogen fluoride) of 14% hydrogen fluoride dimethyl carbonate solution was added, and it stirred at 10 degreeC for 30 minutes. Then, it heated at 120 degreeC for 2 hours, and the remaining solvent and reaction by-products were distilled off. Then, it was cooled to room temperature to obtain crude lithium hexyl monofluorophosphate. As a result of purification treatment of the obtained crude product, a peak of li...
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