Graphene/phthalocyanine supercapacitor electrode material, and preparation method thereof
A technology for supercapacitors and electrode materials, which is applied in the manufacture of hybrid capacitor electrodes and hybrid/electric double-layer capacitors to achieve the effects of simple operation, good cycle stability and mild reaction conditions.
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Embodiment 1
[0038] (1) Preparation of functionalized reduced graphene (rGO-pPD): 300 mg of graphene oxide (GO) was weighed, dispersed in 300 ml of deionized water, 900 mg of p-phenylenediamine (pPD) was added, and after ultrasonication for 1 h, Add 240 μl of 25wt% concentrated ammonia water under reflux, and react at 70°C for 6 h. After the reaction is completed, wash and dry to obtain functionalized reduced graphene (rGO-pPD).
[0039](2) Preparation of tetranitronickel phthalocyanine (NiTNPc): urea (8.5 g), 4-nitrophthalic acid (6.0 g), nickel sulfate (1.8 g), and ammonium chloride (0.6 g) were sequentially Add to the flask, add the catalyst ammonium molybdate (0.08g) and 10 ml of nitrobenzene solvent under reflux, heat to 120°C at 3°C / min, react for 20 min; heat the system to 170°C at 5°C / min After reacting for 3 hours, filter and wash; soak the filter cake in 250mL of 0.5mol / L dilute hydrochloric acid, boil for 10min, filter, then add 250mL of 1mol / L NaOH solution and heat to 60°C unt...
Embodiment 2
[0043] (1) Preparation of functionalized reduced graphene (rGO-pPD): 300 mg of graphene oxide (GO) was weighed, dispersed in 300 ml of deionized water, 100 mg of p-phenylenediamine (pPD) was added, and after ultrasonication for 1 h, Add 400 μl of 25 wt% concentrated ammonia water under reflux, and react at 100°C for 24 h. After the reaction is completed, wash and dry to obtain functionalized reduced graphene (rGO-pPD).
[0044] (2) Preparation of tetranitronickel phthalocyanine (NiTNPc): urea (10.0 g), 4-nitrophthalic acid (7.0 g), nickel chloride hexahydrate (2.2 g), ammonium chloride (0.8 g) Add to the flask in turn, add the catalyst ammonium molybdate (0.15g) and 10 ml of nitrobenzene solvent under reflux, heat at 3°C / min to 170°C, react for 60 min; heat the system at 5°C / min to 200°C, react for 8 hours, filter and wash; soak the filter cake in 250mL 2mol / L dilute hydrochloric acid and boil for 60min, filter, then add 250mL1mol / L NaOH solution and heat to 95°C until no ammo...
Embodiment 3
[0048] (1) Preparation of functionalized reduced graphene (rGO-pPD): 300 mg of graphene oxide (GO) was weighed, dispersed in 300 ml of deionized water, 500 mg of p-phenylenediamine (pPD) was added, and after ultrasonication for 1 h, Under reflux, 320 μl of concentrated ammonia water with a concentration of 25 wt% was added, and reacted at 85°C for 15 h. After the reaction was completed, it was washed and dried to obtain functionalized reduced graphene (rGO-pPD).
[0049] (2) Preparation of tetranitronickel phthalocyanine (NiTNPc): urea (9.25 g), 4-nitrophthalic acid (6.5 g), nickel chloride hexahydrate (2.0 g), ammonium chloride (0.7 g) Add to the flask in turn, add the catalyst ammonium molybdate (0.115g) and 10 ml of nitrobenzene solvent under reflux, heat at 3°C / min to 145°C, react for 40 min; heat the system at 5°C / min to 185°C, react for 5.5 hours, filter and wash; soak the filter cake in 250mL1.25mol / L dilute hydrochloric acid, boil for 35min, filter, then add 250mL1mol / ...
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