Synthesis of porous aromatic skeletal compound and application thereof in oxygen evolution reaction
A porous aromatic skeleton, oxygen evolution reaction technology, applied in organic compound/hydride/coordination complex catalysts, chemical/physical processes, organic chemistry, etc. Expensive, complex and harsh reaction conditions, etc., to achieve the effects of low cost, reduced reaction cost, and mild reaction conditions
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[0036] The present invention provides a kind of synthetic method of porous aromatic skeleton compound, comprises the following steps:
[0037] S1: Synthetic steps of polymer TPHTP
[0038] Porphyrin compound and 1,3,5-triformylphloroglucinol were added into a dry two-necked flask. After degassing with argon, DMF was added, and the mixture was heated to 150°C and kept under an inert atmosphere for 72 hours. After cooling to room temperature, the crude product was collected by filtration with a membrane filter, and then washed three times with dichloromethane, acetone and ethanol. The intermediate product was further purified by Soxhlet extraction with tetrahydrofuran and methanol for 24 hours, and then the product was vacuum-dried at 393K to obtain a black powder. Wherein, porphyrin compounds include 5,10-bis(4-aminophenyl)-10,20-diphenylporphyrin and / or tetraaminotetraphenylporphyrin, porphyrin compounds and 1,3,5-trimethyl The molar ratio of acylphloroglucinol is (2.5-6.5):...
Embodiment 1
[0044] This implementation provides a kind of synthetic method of porous aromatic skeleton compound, comprises the following steps:
[0045] S1: Synthesis of polymer TPHTP:
[0046] Add 5,10-bis(4-aminophenyl)-10,20-diphenylporphyrin (0.2 mmol) and 1,3,5-triformylphloroglucinol (0.3 mmol) into a dry 25 mL two-neck in the flask. After degassing with argon, DMF (10 mL) was added and the mixture was warmed to 150 °C and kept under inert atmosphere for 72 h. After cooling to room temperature, the crude product was collected by filtration with a membrane filter, and then washed three times with acetone and ethanol respectively. The intermediate was further purified by Soxhlet extraction with tetrahydrofuran and methanol for 24 hours, respectively. The product was vacuum-dried at 393K, black powder, the yield was 94%, the scanning electron microscope picture is shown in figure 1 .
[0047] S2: Synthesis of polymer TPHTPTP:
[0048] The intermediate product (100 mg) and cobalt ...
Embodiment 2
[0051] This implementation provides a kind of synthetic method of porous aromatic skeleton compound, comprises the following steps:
[0052] S1: Synthesis of polymer TPHTP:
[0053] Add 5,10-bis(4-aminophenyl)-10,20-diphenylporphyrin (0.45 mmol) and 1,3,5-triformylphloroglucinol (0.4 mmol) into a dry 25 mL two-neck in the flask. After degassing with argon, DMF (15 mL) was added and the mixture was warmed to 150 °C and kept under inert atmosphere for 72 h. After cooling to room temperature, the crude product was collected by filtration with a membrane filter, and then washed three times with acetone and ethanol respectively. The intermediate was further purified by Soxhlet extraction with tetrahydrofuran and methanol for 24 hours, respectively. The product was vacuum-dried at 393K and became a black powder with a yield of 96%.
[0054] S2: Synthesis of polymer TPHTPTP:
[0055] The intermediate product (100 mg) and cobalt acetate (350 mg) were added to a dry 100 mL round b...
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