Pyrazole carboxylic acid coni complex with visible light catalytic performance and preparation method and application thereof
A technology of visible light and coordination polymers, applied in the field of material science, can solve the problems of ineffective use of visible light, and achieve the effect of good stability and performance
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Embodiment 1
[0038] The coordination polymer 1[NiL(H 2 O) 3 ] preparation
[0039] Weigh NiCl 2 ·6H 2 O (0.1 mmol, 24.0 mg), H 2 L (0.1 mmol, 17.0 mg) was dissolved in N-methylpyrrolidone (NMP) (2 mL), H 2 In the mixed solution of 0 (1 mL), ultrasonically dissolve and stir evenly to obtain a green clear and transparent liquid. The green liquid is placed in a hydrothermal reaction kettle, placed in an oven at 140 ° C for 72 hours, cooled to room temperature, filtered and washed to obtain the product , observed under the microscope as green transparent square crystals with a yield of 41.3%.
[0040] IR(KBr, cm-1): 3447(s), 1558(s), 1402(m), 1301(m), 1030(w), 285(m), 650(w). Elemental Analysis: C 6 H 10 N 2 O 7 Ni, experimental (theoretical) %: C, 25.86 (25.66); H, 3.66 (3.59); N, 10.12 (9.97). The PXRD results were measured as figure 2 shown.
Embodiment 2
[0042] The coordination polymer 2[Co 0.4 Ni 0.6 L(H 2 O) 3 ] preparation
[0043] Weigh CoCl 2·6H 2 O (0.05mmol, 12.0mg), NiCl 2 ·6H 2 O (0.05mmol, 12.0mg), H 2 L (0.1 mmol, 17.0 mg) was dissolved in N,N-dimethylformamide (3 mL) and H 2 O (3mL) mixed solution, ultrasonically dissolved and stirred evenly to obtain a light pink-purple transparent liquid. The liquid was placed in a hydrothermal reactor, placed in an oven at 100°C for 72h and cooled to room temperature. The obtained crystals were observed under a microscope. It was observed as a light pink purple rectangle, and was filtered, washed and dried with a yield of 70.2%.
[0044] IR(KBr,cm -1 ): 3414(s), 1617(m), 1556(m), 1399(m), 1300(m), 1028(w), 787(w), 617(w). The PXRD results were measured as figure 2 shown.
Embodiment 3
[0046] The coordination polymer 3[CoL(H 2 O) 3 ] preparation
[0047] Weigh Co(NO 3 ) 2 ·6H 2 O (0.1 mmol, 29.1 mg), H 2 L (0.1 mmol, 17.0 mg) was dissolved in ethanol (4 mL) and H 2 O (1mL) mixed solution, and add 50μL NaOH (1mol / L) to adjust the pH to 5, stir and mix evenly to obtain a pink liquid, put it into a hydrothermal kettle, and place it in an oven at 120°C for 72h after reaction After cooling to room temperature, the product was observed under a microscope as pink transparent bulk crystals, which were filtered, washed and dried with a yield of 65.0%.
[0048] IR(KBr,cm-1): 3411(s), 1615(s), 1557(s), 1399(m), 1301(m), 1025(w), 786(w), 610(w), 497 (w). Elemental Analysis: C 6 H 10 N 2 O 7 Co, experimental (theoretical) %: C, 25.86 (25.64); H, 3.69 (3.58); N, 10.12 (9.97). The PXRD results were measured as figure 2 shown.
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