5, 10-dialkyl-5, 10-dihydrophenazine polymer as well as preparation method and application thereof
A technology of dihydrophenazine and dihydrophenazine, which is applied in the field of 5,10-dialkyl-5,10-dihydrophenazine polymers, can solve the problem of reducing the theoretical specific capacity of materials and poor battery cycle performance. It can achieve the effect of high cycle stability and high capacity ratio
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[0060] Example 1 Synthesis of (2-vinyl-5,10-dimethyl-5,10-dihydrodoxazine)
[0061] Step 1: Synthesis of 2-bromo-5,10-dimethyl-5,10-dihydromidazine (Compound 2)
[0062]
[0063] 1 (0.89 g, 3.45 mmol) was added 1 (0.89 g, 3.45 mmol) to the preset stirrer, and the refluxing device was placed, and the nitrogen was discharged three times, and then 15 ml of ethanol was added to the syringe, and stirred and dissolved. Dissolis sodium sulfite (7 g, 34.5 mmol) was dissolved in 130 ml of distilled water, and the system was added through a syringe, and the temperature was raised to about 40 ° C for 4 hours to obtain a blue-green solid suspension. Solid filtration, washed, freeze, and dried to give 0.695 g of 2-bromo-5,10-dihydromidazine intermediate. 2-bromo-5,10-dihydromidazine (0.695 g, 2.67 mmol) was added to the 100 ml of three-neck bottle preset, and the nitrogen gas was discharged three times, and then 20 ml of super dry tetrahydrofuran was added with a syringe, and dry ice was pro...
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[0075] Example 2 Synthesis of poly (2-ethynyl-5, 10-dimethyl-5,10-dihydropazide)
[0076]Step 1: Synthesis of 2-ethynyl-5,10-dimethyl-5,10-dihydromidazine (Compound 4)
[0077]
[0078] Compound 2 (28.9 mg, 1 mmol), copper iodide (3.8 mg, 20 μmol), bis (21 mg, 30 μmol) of biodine (21 mg, 30 μmol), and displaced nitrogen three times, The syringe was added to 0.12 mL of tri-butylphosphine (10 W / V%, 60 μmol), 0.7 ml of trimethylcycera (490 mg, 5 mmol), 5 mL dioxane and 3 ml diisopropylamine, heated to 60 ° C for 48 hours . The resulting mixture was separated by silica gel column (eluent: n-hexane) to obtain an intermediate product dissolved in 10 ml of tetrahydrofuran, and 1.2 ml of tetra-nanohydrofluoride (1 mol / lin THF, 1.2 mmol) was added, and the mixture was stirred at room temperature 2 hours. The resulting solution was concentrated and separated by silica gel column (eluent: n-hexane) to give compound 4 about 80 mg.
[0079] Rim f 0.68 (N-HEXANE / Ethyl acetate: 10 / 1); 1 ...
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[0085] Example 3 Electrochemical properties of the positive electrode material of the lithium secondary battery by polymer P1 and P2
[0086] Preparation of a positive electrode composite pole: Preparation of a positive electrode composite plate of P1 or P2 as an active material, 45 mg of the active material P1 or P2 and 40 mg electrically conductors (CCA black and / or super p) are mixed together by manual grinding. Polyvinylidene fluoride (PVDF) was dissolved in N-methylpyrrolidone (NMP), and the abrasive was dispersed in NMP and stirred at room temperature for 24 hours. The fluid aluminum foil was prepared on the glass sheet, and the slurry roller was pressed into a film with a roller press, dried under vacuum at 70 ° C for 12 hours. The slice was pressed into a zipper having a radius of 6 mm.
[0087] Upset of the button battery: The composite film prepared by the above is a positive electrode, the lithium sheet is an negative electrode, the CelGard 2400 microporous film is a ...
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