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Halogen-substituted binuclear phthalocyanine ferrite reduction catacolyst and preparing method thereof

A nuclear iron phthalocyanine and catalyst technology, applied in the field of electrocatalysis, can solve problems such as poor stability, and achieve the effects of good stability, high catalytic activity, and efficient oxygen reduction

Inactive Publication Date: 2009-07-08
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to solve the problem of poor stability of mononuclear phthalocyanine complexes as oxygen reduction catalysts, and to provide a novel non-precious metal fuel cell cathode oxygen reduction catalyst-halogen-substituted dinuclear iron phthalocyanine complex and its preparation method

Method used

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  • Halogen-substituted binuclear phthalocyanine ferrite reduction catacolyst and preparing method thereof
  • Halogen-substituted binuclear phthalocyanine ferrite reduction catacolyst and preparing method thereof
  • Halogen-substituted binuclear phthalocyanine ferrite reduction catacolyst and preparing method thereof

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Experimental program
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Effect test

Embodiment 1

[0019] (1) 6.51g3.6-dichlorophthalic anhydride, 1.10g pyromellitic anhydride, 1.98gFeCl 2 4H 2 O, 9.47g of urea and 0.25g of ammonium molybdate were mixed evenly and finely ground. After the mixture was heated at 190°C for 1 hour, the reaction was continued at 250°C for 2 hours. The product was successively washed with ammonia solution, dilute hydrochloric acid and water, and then dried. The crude product was extracted and washed with ethanol and tetrahydrofuran until it was colorless, and further purified by silica gel chromatography (N,N-dimethylformamide as the eluent) to obtain the dark blue target product dodecachloro-substituted dinuclear phthalocyanine iron (II ). UV-Vis (DMSO as a solution): λ max 662nm. 1 HNMR (DSMO-d 8 ): δ11.3~11.8 (2H, aroma). Elemental Analysis: Calculated for C, 50.07; H, 13.58; N, 15.10; Fe, 7.53. Found C, 50.01; H, 13.55; N, 15.12; Fe, 7.60. Mass Spectrum (LDI-TOF-MS) Found (Calcd): M / e=1483.6 (1483.1) [M + ]

Embodiment 2

[0021] 6.60g tetrafluorophthalic anhydride, 1.10g pyromellitic anhydride, 1.98g FeCl 2 4H 2 O, 9.47g of urea and 0.25g of ammonium molybdate were mixed evenly and finely ground. After the mixture was heated at 110°C for 1.5h, the reaction was continued at 220°C for 3h. The product was washed with ammonia solution, dilute hydrochloric acid and water in turn, and then dried. The crude product was extracted and washed with ethanol and tetrahydrofuran until it was colorless, and further purified by silica gel chromatography (N,N-dimethylformamide as the eluent) to obtain the dark blue target product Tetrafluoro-substituted dinuclear iron phthalocyanine ( II). UV-Vis (DMSO as a solution): λ max 651nm. 1 HNMR (DSMO-d 8 ): δ 10.5 to 10.8 (2H, aroma). Elemental analysis: calculated value C: 49.06, H: 13.31, N: 14.30, Fe: 7.37; found value C: 49.02, H: 13.40, N: 14.26, Fe: 7.42. Mass Spectrum (LDI-TOF-MS) Found (Calcd): M / e=1514.2 (1513.6) [M + ]

[0022] The target product obt...

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Abstract

A halogen-substituted dinuclear phthalocyanine iron-oxygen reduction catalyst and a preparation method thereof belong to the field of battery material science and technology. Aiming at the problem of poor stability of mononuclear phthalocyanine complexes as oxygen reduction catalysts, the method of the present invention comprises the following steps: uniformly mixing halogenated phthalic anhydride, pyromellitic anhydride, FeCl2 4H2O, urea and ammonium molybdate mixture Grinding, the molar ratio of reactants is halogenated phthalic anhydride: pyromellitic anhydride: FeCl2 4H2O: urea is 6:1~1.5:2~3:20~40; react at 100℃~190℃ for 1 After ~3h, continue to react at 200~270℃ for 2~4h, the product is washed with ammonia solution, dilute hydrochloric acid and water in sequence, and then dried to obtain the crude product; it is extracted and washed with ethanol and tetrahydrofuran respectively until it is colorless, and further purified by column chromatography Halogen substituted dinuclear iron phthalocyanine. It not only has high catalytic activity and good stability, but also can realize the 4e process of efficient oxygen reduction.

Description

field of invention [0001] The invention relates to a non-noble metal oxygen reduction catalyst, which belongs to the technical fields of battery material science and electrocatalysis. Background technique [0002] A fuel cell is an environmentally friendly power generation device. The cathode oxygen reduction catalyst plays a very critical role in the performance of fuel cells. At present, the cathode catalysts of fuel cells usually use precious metal platinum and its alloys. Due to the high price and insufficient resources of this type of catalysts, the commercial development of fuel cells is limited. In the research of non-platinum catalysts, macrocyclic conjugated complexes such as phthalocyanine and porphyrin have attracted much attention. The existing literature reports that the catalysts for oxygen reduction are mainly mononuclear phthalocyanine complexes. Although their catalytic activity is high, However, the stability of the catalyst in acidic medium is poor. The...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/28
Inventor 左霞胡晓明夏定国
Owner BEIJING UNIV OF TECH
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