Cobalt ion liquid redox couple and preparation and application thereof
A technology of ionic liquids and cobalt ions, which is applied in the field of dye-sensitized solar cells, can solve the problems of poor thermal stability, difficult packaging of batteries, and easy volatilization, and achieves broad application prospects, easy leakage, and industrialization.
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Embodiment 1
[0031] Embodiment one: see figure 1 As shown, the preparation of compound 7a specifically includes the following steps:
[0032] (1) Put 4,4'-dimethyl-2,2'-bipyridine (5g, 27.1mmol) into a 250mL three-necked flask, add concentrated sulfuric acid (150mL) into it, and slowly heat to 60°C with magnetic stirring, At this time, potassium dichromate (32g, 110.8mmol) was slowly added in, and the reaction temperature was kept at 70-80°C during the reaction. After the reaction, a dark green solution was obtained after cooling, and then the dark green solution was poured into 600mL of ice water solution, and filtered to obtain Wash the yellow solid twice with water, reflux the obtained yellow solid in 50% concentrated nitric acid (150mL) for 4h, cool, pour the reaction solution into ice water (800mL) and filter to obtain a white solid, wash twice with water , and weighed dry to obtain compound 2 (6.4g), yield 97%. The melting point is greater than 300°C.
[0033] Compound 2 was analy...
Embodiment 2
[0044] Embodiment two: see figure 1 And Example 1, the preparation of compound 7b specifically includes the following steps:
[0045] (1) Weighing Compound 5 (1.0g, 2.90mmol) and 1-ethylimidazole (0.59g, 6.17mmol) were dissolved in methanol, refluxed for 3 days, and the detection reaction was completely rotary evaporated to remove methanol, washed with ether to obtain Product 1.3g; Gained product is analyzed, and data is as follows: 1 H NMR (CDCl 3 , 400Hz): δ(ppm): hydrogen on the aliphatic chain 1.27 (6H, t); 4.15 (4H, q); 5.94 (4H, s); hydrogen on the imidazole ring 10.18 (2H, d); 7.75-7.76 (4H, d); hydrogens on the pyridine ring 7.41 (2H, dd); 8.91 (2H, s); 8.78 (2H, d). The above results prove that the obtained compound is compound 6b.
[0046] (2) Weigh compound 6b (1.0g, 2.67mmol) and dissolve it completely in methanol, CoCl 3 .6H 2 O (0.16g, 0.066mmol) was dissolved in 5mL of water, slowly added to the methanol solution of compound 6b, stirred for 1 hour, and the...
Embodiment 3
[0047] Embodiment three: see figure 1 And Example 1, the preparation of compound 7c specifically includes the following steps:
[0048] (1) Weighing Compound 5 (1.0g, 2.90mmol) and 1-butylimidazole (0.76g, 6.17mmol) were dissolved in methanol, refluxed for 3 days, and the detection reaction was completely rotary evaporated to remove methanol, washed with ether to obtain Product 1.5g; Gained product is analyzed, and data is as follows: 1 H NMR (CDCl 3 , 400Hz): δ (ppm): hydrogen on the aliphatic chain 0.79 (4H, t); 1.29 (4H, m); 1.68 (4H, m); 4.01 (4H, t); 5.48 (4H, s); imidazole Hydrogens on the ring 9.89 (2H,d); 7.67-7.64 (4H,d) Hydrogens on the pyridine ring 8.76 (2H,d); 8.25 (2H,d). 7.25 (2H, dd). The above results prove that the obtained compound is compound 6c.
[0049] (2) Weigh compound 6c (1.0g, 1.7mmol) and completely dissolve it in methanol, CoCl 3 .6H 2 O (0.16g, 0.066mmol) was dissolved in 5mL of water, slowly added to the methanol solution of compound 6c, s...
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