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P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof

A technology of dicyanophenyl and dicyanobenzene, which is applied in the field of synthesis of a p-phenylene disulfide polymerized iron phthalocyanine and its preparation, can solve the problems of high production cost, poor activity and stability of noble metal nanocatalysts, etc. Achieve the effect of excellent catalytic activity and stability, simple synthesis method and wide application prospect

Inactive Publication Date: 2016-02-10
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is that noble metal nano catalysts (mainly platinum) have high production cost, poor activity and stability

Method used

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  • P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof
  • P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof
  • P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0037] Disperse 0.5g of graphite and 0.5g of sodium nitrate in 42.32g of concentrated sulfuric acid, slowly add 3g of potassium permanganate under mechanical stirring at 0°C; stir in a water bath at 35°C for 1 hour; add 40g of water, After stirring for 30 minutes, add 100g of water and 4.44g of 30% hydrogen peroxide (H 2 o 2 ) after suction filtration, washing with water and centrifugation until the centrifuged water is neutral, and vacuum drying at 45° C. for 12 hours to obtain graphene oxide.

Embodiment 2

[0039] in N 2 Under gas protection, 1 mmol of hydroquinone, 2 mmol of 4-nitrophthalonitrile, 2 mmol of anhydrous potassium carbonate and 259.2 mmol of N,N-dimethylformamide (DMF) were reacted at 55°C for 6 hours with magnetic stirring. Pour into deionized water after being cooled to room temperature, filter, obtain the powdered terephthalate (3,4-dicyanophenyl) sulfide monomer; ) sulfide monomer was washed 3 times with ethanol, and dried under vacuum at 50°C; 2 4H 2 O), 3.345mmol DBU and 184.9mmol n-pentanol reacted at 160°C with magnetic stirring for 6 hours, cooled naturally to room temperature after the reaction, added three times of water and filtered to obtain p-phthalenic di(3,4-dicyanophenyl)sulfur The crude product of ether polymerized iron phthalocyanine; the crude product of terephthalocyanine (3,4-dicyanophenyl) sulfide polymerized iron phthalocyanine is washed with DMF, water and ethanol to neutrality respectively, and after drying, terephthalo(3 , 4-dicyanophen...

Embodiment 3

[0041] Disperse the graphene oxide of 10mg embodiment 1 in 14.2125gDMF2, add the PTFePPc of 30mg embodiment 2, in 160 ℃ hydrothermal reaction 12 hours, obtain the graphene oxide composite material of PTFePPc / reduction; The PTFePPc / reduction Graphene oxide composites were heat-treated at 700 °C for 2 hours to obtain N / S double-doped graphene-supported Fe with a mass ratio of 3:1. 9 S 10 Nanocrystalline [PTFePPc / rGO, 3:1, 700 °C].

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Abstract

The invention discloses a p-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine (PTFePPc) and a preparation method and an application thereof, and belongs to the technical field of cathode catalysts of proton exchange membrane fuel cells. A polymerization unit of PTFePPc is formed by connecting 3,4-dicyano phenyl iron phthalocyanine and dithiohydroquinone through a covalent bond; and the preparation method of the PTFePPc comprises the following steps: preparing p-phenyl di(3,4-dicyano phenyl) thioether from 4-nitrophthalonitrile and the dithiohydroquinone; making the p-phenyl di(3,4-dicyano phenyl) thioether react with iron dichloride tetrahydrate, so as to prepare the PTFePPc; and heating the PTFePPc and a graphene oxide solvent and then carrying out a high-temperature heat treatment, so as to obtain N / S doubly doped graphene-loaded Fe<9>S<10> nanocrystals. The N / S doubly doped graphene-loaded Fe<9>S<10> nanocrystal disclosed by the invention has excellent catalytic performance on oxygen reduction.

Description

technical field [0001] The invention relates to the technical field of the application of proton exchange membrane fuel cell cathode catalysts, in particular to the synthesis of a terephthalobis(3,4-dicyanophenyl) sulfide polymerized iron phthalocyanine and its preparation method and application. Background technique [0002] With the continuous growth of global energy demand and the excessive utilization of non-renewable energy, people have strongly realized that the development of a sustainable society in the future must be based on the development and utilization of sustainable energy. Fuel cell is a new energy source with high efficiency, high reliability, environment-friendly, clean and renewable. As a highly efficient energy conversion device that converts chemical energy into electrical energy, fuel cells play an important role in the field of sustainable energy utilization, so they have attracted much attention. [0003] Proton exchange membrane fuel cell (PEMFC) is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/88H01M4/9008Y02E60/50
Inventor 何兴权苏艳徐丛丛
Owner CHANGCHUN UNIV OF SCI & TECH
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