Lithium secondary battery
A lithium secondary battery and electrolyte technology, applied in secondary batteries, lithium batteries, battery electrodes, etc., can solve serious battery, cycle characteristics degradation, expansion high temperature stability and other problems
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Embodiment 1
[0224] [Example 1] Amyl difluorophosphite (CH 3 (CH 2 ) 4 OPF 2 (hereinafter referred to as "PDFP") preparation
[0225]
[0226] Step 1: Amyl dichlorophosphite (CH 3 (CH 2 ) 4 OPCl 2 ) preparation
[0227]
[0228] Tetrahydrofuran (200 mL) was added to the 500 mL flask. Phosphorus trichloride (PCl 3 ) (56mL, 0.57mol), stirred for 10 minutes, and lowered the temperature to a low temperature near 0°C using ice water. 1-Pentanol (50 g, 0.57 mol) was slowly added dropwise thereto for 30 minutes, and the solution was stirred for 3 hours while raising the temperature to room temperature. The reaction mixture was reduced to vacuum to remove volatiles. Analysis using NMR equipment to confirm residual material and final product. The final product after reduced pressure, pentyl dichlorophosphate (75 g, 0.40 mol) was obtained in 70% yield with almost 100% purity.
[0229] 1 H NMR (500MHz, C 6 D. 6 )δ0.94 (m, 3H), 1.00-1.40 (m, 6H), 3.80 (m, 2H) ppm.
[0230] Step ...
Embodiment 2
[0234] [Example 2] Preparation of (1,3-bis(allyloxy)prop-2-yl)difluorophosphite
[0235]
[0236] Step 1: (1,3-bis(allyloxy)propan-2-yl)dichlorophosphite (C 9 h 15 C l2 o 3 P) preparation
[0237]
[0238] Under a nitrogen atmosphere, 150ml of acetonitrile was added to a 500ml flask, and 37.78g (275.5mmol) of phosphorus trichloride (PCl 3 ), and the temperature was lowered to -15 °C using saline and dry ice. A mixed solution of 43.56 g (252.9 mmol) of 1,3-bis(allyloxy)propan-2-ol and 20 ml of acetonitrile was slowly added dropwise thereto for 1 hour, and the solution was stirred while raising the temperature to room temperature 3 hours. The reaction mixture was depressurized to vacuum to remove the solvent to obtain 58.85 g (215.5 mmol) of (1,3-bis(allyloxy)propan-2-yl)dichlorophosphite (C 9 h 15 C l2 o 3 P) with a yield of 85.2%.
[0239] 1 H NMR (500MHz, C 6 D. 6 )δ5.70 (m, 2H), 5.13 (d, 2H), 4.99 (d, 2H), 4.77 (m, 1H), 3.68 (m, 4H), 3.45 (m, 4H) ppm.
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Embodiment 3- Embodiment 6
[0245] The solution was used to prepare the electrolyte by further adding the components described in Table 1 below, as the base electrolyte (1.0M LiPF 6 , EC / EMC=25:75) solution, LiPF 6 It was dissolved in a mixed solvent of ethylene carbonate (EC) and ethyl methyl carbonate (EMC) at a volume ratio of 25:75 so that the solution became a 1.0M solution.
[0246] First lithium metal oxide contained in positive electrode active material having a structure (NCM-811) including secondary particles formed by aggregating primary particles and having no concentration gradient or having a core-shell structure (CSG-811) LiNi 0.8 co 0.1 mn 0.1 o 2 , prepared in the form of the first lithium metal oxide precursor according to the following steps.
[0247] Preparation for the preparation of LiNi 0.8 co 0.1 mn 0.1 o 2 An aqueous metal solution (which has a structure including secondary particles formed by aggregating primary particles and having no concentration gradient or has a co...
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