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Preparation method of transition metal and nitrogen doped multistage pore-passage three-dimensional graphene

A transition metal and transition metal salt technology, applied in graphene, non-metallic elements, chemical instruments and methods, etc., can solve problems such as low catalytic performance, insufficient durability, and easy removal of metals by acids

Active Publication Date: 2017-05-31
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention differs from metal-nitrogen-carbon clusters prepared by pyrolysis of simple nitrogen-containing organic compounds and transition metal complexes or nitrogen-containing polymers, such as urea resin, melamine resin, etc., and transition metal mixtures in that metal-nitrogen-carbon The atomic cluster is not a graphene structure, not co-doped with transition metal ions and nitrogen, and has no large π effect, so the catalytic performance is not high, and its metal is easily removed by acid, so the durability is not good enough, especially due to the metal-nitrogen - Carbon clusters are not porous and their mass transfer effect is not good, so their catalytic activity and durability are not good enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] [Example 1] Preparation of mPBI: Add polyphosphoric acid (PPA) (100 g) into a three-necked flask equipped with electric stirring and nitrogen protection, and stir at 160° C. for 1 h under nitrogen protection to remove excess water and air. DABz (4 g, 18.7 mmol) and isophthalic acid (3.1 g, 18.7 mmol) were mixed evenly, and slowly added into a three-necked flask. The nitrogen flow rate was controlled to prevent DABz from being oxidized, and at the same time, the reaction temperature was increased to 200 °C and the reaction was continued for 5-8 h with insulation and stirring. With the increase of reaction time, the polymerization system gradually became viscous. Stop the reaction when the viscosity is appropriate, slowly transfer the reaction mixture to a large amount of deionized water, spin, wash, dry, pulverize, and wash with deionized water several times to remove polyphosphoric acid and unreacted reactants to obtain mPBI. The molecular weight of mPBI was determined...

Embodiment 2

[0018] [Example 2] Synthesis of mPBI by solid-phase method: DABz (4 g, 18.7 mmol) and isophthalic acid (3.1 g, 18.7 mmol) were mixed in a mortar, thoroughly ground and mixed, transferred to a place with nitrogen protection, stirring in a three-neck flask. Nitrogen was passed for 15 min to exhaust the air in the flask. N 2 Protected and stirred, heated in an oil bath at 225°C for 3h. Take it out after cooling, grind finely, N 2 Under protection, heat in an electric furnace, raise the temperature to 270-275°C, and keep it for 3 hours. After cooling to room temperature, the product was taken out and finely ground to obtain mPBI, and the molecular weight of mPBI was measured with an Ubbelohde viscometer.

Embodiment 3

[0019] [Example 3] The preparation method of ABPBI is similar to that of mPBI, except that 3,4-diaminobenzoic acid (DABA) is used instead of DABz and isophthalic acid. ABPBI can be obtained using only one raw material. Other reaction conditions and operation steps are with embodiment 1 and embodiment 2.

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Abstract

The invention provides a preparation method of a transition metal and nitrogen doped multistage pore-passage three-dimensional graphene. Soluble full-aromatic polybenzimidazole (PBI) serving as carbon and nitrogen sources, transition metal salt and a PBI solution react to obtain a PBI and transition metal ion complex, nano calcium carbonate is added in the mixed liquid to serve as a template agent, even mixing and concentration are performed to coat and regularly arrange the complex on the surface of the template agent, the template agent is removed through pyrolysis, the transition metal and nitrogen doped three-dimensional graphene with a multistage pore-passage structure is obtained, and multistage thorough pore passages can strengthen mass transfer. The viscosity average molecular weight of the PBI is 2-40 thousand. The molar ratio of the PBI to the transition metal is 1:2 to 2:1. The template agent is calcium carbonate, and the particle size of the template agent is 30-100 nm. The mass ratio of the PBI to the template agent is 2:1 to 1:4. Pyrolysis temperature is 800-1100 DEG C. The product can be used for oxidation-reduction reaction catalysts, fuel cells, metal air batteries, oxidation-reduction reaction catalysts, electrolytic water oxygen precipitation catalyst, supercapacitors and other fields.

Description

technical field [0001] Belonging to the field of nanomaterial preparation, it is used in redox reaction catalysts in chemical production, fuel cells in the field of clean energy, cathode catalysts for metal-air batteries, electrolytic water catalysts, lithium-ion battery materials, supercapacitor electrode materials and electrochemical sensors, etc. . Background technique [0002] Although two-dimensional graphene has excellent properties and a variety of potential applications, however, two-dimensional graphene is easy to be layer-by-layer superimposed to form a graphite structure, thus losing its excellent performance. Therefore, the preparation and performance research of three-dimensional graphene has become a research hotspot in the field of nanomaterials. The study found that the electron cloud density on the graphene molecule changes due to the polarity between the C-N bonds in the graphene molecule in nitrogen-doped graphene, so nitrogen-doped graphene has better ca...

Claims

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Application Information

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IPC IPC(8): C01B32/184C08G73/18
CPCC01B2204/04C01B2204/32C01P2006/16C01P2006/17C08G73/18
Inventor 李忠芳王素文张廷尉卢雪伟
Owner SHANDONG UNIV OF TECH
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