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Method for preparing iron phthalocyanine-graphene porous composite material

A porous composite material, graphene technology, applied in the field of electrochemical catalyst preparation, can solve problems such as unsuitable practical application, low solubility, and complicated operation, and achieve the effects of reducing complexity and cost, good porous structure, and simplifying experimental steps.

Inactive Publication Date: 2016-07-06
SHANDONG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, iron phthalocyanine is mainly supported on sheet-shaped graphene, and such graphene is a two-dimensional material, which is easy to cluster, thereby reducing the surface area, and is only suitable for thin film materials, with a small range of applications , in the preparation process of composite materials, iron phthalocyanine can only be loaded on the surface of graphene flakes, there are no more loading points, so there are fewer active sites for catalytic reactions, and its application in catalytic oxygen reduction reaction In addition, the complex cannot fully contact with oxygen, so the catalytic effect is affected; for the preparation of iron phthalocyanine-graphene composites, it is generally used to form a covalent bond through functional group modification or to form a non-covalent bond through ultrasonication and long-term vigorous stirring. The method of π-π interaction enables iron phthalocyanine to be supported on graphene. However, these methods are relatively cumbersome in operation, take a long time, and are not suitable for practical applications. At the same time, the solubility of iron phthalocyanine in organic solvents is small. It is very easy to aggregate, which reduces its catalytic activity, so how to improve the ease of operation and solve the aggregation problem of iron phthalocyanine is also very important

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  • Method for preparing iron phthalocyanine-graphene porous composite material
  • Method for preparing iron phthalocyanine-graphene porous composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 20 mg of graphene oxide into a beaker, add 5 mL of water and ultrasonically disperse for 30 min to obtain a uniform dispersion. Then put the beaker into liquid nitrogen, and after the graphene oxide dispersion is completely frozen to a solid state, put it into a freeze dryer (the freezing temperature has reached -50°C), turn on the vacuum mode, and make the vacuum freeze dryer Operate in this mode for 40 hours, and the graphene oxide porous composite material will be obtained after the water in the sample is completely sublimated. Then, the graphene oxide porous composite was calcined in a nitrogen atmosphere at 700 °C for 1.5 h at a heating rate of 3 °C / min. After the calcination, the sample is taken out to obtain a graphene porous material. Use an electronic analytical balance to weigh 0.3 mg of iron phthalocyanine powder into a small glass bottle, add 3 mL of absolute ethanol, and ultrasonically disperse for 30 minutes to obtain a uniform concentration of 0.1 ...

Embodiment 2

[0027] Weigh 30 mg of graphene oxide into a beaker, add 5 mL of water and ultrasonically disperse for 30 min to obtain a uniform dispersion. Then put the beaker into liquid nitrogen, and after the graphene oxide dispersion is completely frozen to a solid state, put it into a freeze dryer (the freezing temperature has reached -50°C), turn on the vacuum mode, and make the vacuum freeze dryer Operate in this mode for 45 hours, and the graphene oxide porous composite material will be obtained after the water in the sample is completely sublimated. Then, the graphene oxide porous composite was calcined in a nitrogen atmosphere at 750 °C for 2 h at a heating rate of 3 °C / min. After the calcination, the sample is taken out to obtain a graphene porous material. Use an electronic analytical balance to weigh 0.6mg of iron phthalocyanine powder into a small glass bottle, add 3mL of absolute ethanol, and ultrasonically disperse for 30min to obtain a uniform concentration of 0.2mgmL -1 s...

Embodiment 3

[0030]Weigh 35 mg of graphene oxide into a beaker, add 5 mL of water and ultrasonically disperse for 30 min to obtain a uniform dispersion. Then put the beaker into liquid nitrogen, and after the graphene oxide dispersion is completely frozen to a solid state, put it into a freeze dryer (the freezing temperature has reached -50°C), turn on the vacuum mode, and make the vacuum freeze dryer Operate in this mode for 48 hours, and the graphene oxide porous composite material will be obtained after the water in the sample is completely sublimated. Then, the graphene oxide porous composite was calcined at 800 °C for 3 h under the protection of nitrogen atmosphere, and the heating rate was 4 °C / min. After the calcination, the sample is taken out to obtain a graphene porous material. Weigh 1.2 mg of iron phthalocyanine powder into a small glass bottle with an electronic analytical balance, add 3 mL of absolute ethanol, and ultrasonically disperse for 40 minutes to obtain a uniform co...

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Abstract

The invention discloses a method for preparing an iron phthalocyanine-graphene porous composite material. The iron phthalocyanine is dissolved into absolute ethyl alcohol, and fully dissolved by ultrasonic, wherein the concentration range of the iron phthalocyanine is 0.1-0.4mg mL<-1>; the graphene porous composite material is ultrasonically soaked in the prepared solution for 0.5-1.5h; and the soaked graphene porous composite material is taken out and dried to obtain the iron phthalocyanine-graphene porous composite material. According to the method, the graphene porous composite material has a good porous structure and a large surface area, so that iron phthalocyanine can be better contacted with graphene; the iron phthalocyanine is loaded to the surface and the hole wall surface of the graphene porous composite material through a simple impregnating method, so that the experimental procedures are greatly simplified; a more convenient and faster operation, and a stable process are realized; and the preparation complexity and preparation cost of the material are effectively lowered.

Description

technical field [0001] The invention belongs to the technical field of electrochemical catalyst preparation, and in particular relates to a method for preparing iron phthalocyanine-graphene porous composite material. Background technique [0002] Iron phthalocyanine-graphene composites can be used to catalyze the oxygen reduction reaction, which has the advantages of low cost, good stability, and no poisoning effect compared with traditional Pt / C catalysts. Among them, iron phthalocyanine is easy to synthesize and can effectively catalyze the reduction reaction of oxygen; while graphene has good electrical conductivity, which is conducive to the transmission of electrons, which can promote electron transfer in the process of oxygen reduction reaction, and combine iron phthalocyanine and graphene It can greatly improve the catalytic ability of the oxygen reduction reaction, so it has attracted much attention. [0003] In the prior art, it is mainly to load iron phthalocyanin...

Claims

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Application Information

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IPC IPC(8): H01M4/90H01M8/1011
CPCH01M4/90H01M8/1011Y02E60/50
Inventor 钱磊张艳吴海坤孙仲玉
Owner SHANDONG UNIV
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