Porous graphene loaded ferrocobalt sulfide catalyst as well as preparation method and application thereof

A porous graphene and sulfide technology, which is applied in the field of clean energy nanomaterials and catalysis, can solve the problems of easy damage to the porous network structure, complex template etching process, weak contact between heterogeneous interfaces, etc., to make up for low specific surface area. And the effect of insufficient exposure of active sites, accelerated catalytic reaction rate, and uniform particle size

Pending Publication Date: 2021-12-07
JIANGSU UNIV
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Problems solved by technology

However, the simple combination of the two tends to lead to the aggregation of a large number of nanoparticles and the insufficient exposure of the active sites, which reduces the catalytic activity of the composite material; in addition, the weak anchoring between the nanoparticles and graphene makes it easy for the nanoparticles to be leached. reduce the stability of the composite
[0004] At present, the preparation methods of porous graphene reported in the literature mainly include template method and self-assembly method. Although the template method can effectively control the particle size and distribution of pores, the template design and etching process are complicated and costly; the self-assembly method usually It uses graphene oxide and some organic modifiers to produce polymerization or crosslinking reactions to obtain liquid gels, and then freeze-dry the liquid gels to obtain porous graphene aerogels, but porous graphene used as catalytic materials, It is often necessary to carry out high-temperature heat treatment to remove excessive oxygen-containing functional groups, improve the conductivity and graphitization degree of the material, and the mechanical stability of the porous graphene prepared by this method is poor, and the porous network structure is easily destroyed, because the graphite The ene sheets are linked together by some weaker bonds such as van der Waals force and π–π conjugation (Adv. Mater., 2015, 27, 5171–5175)
At present, the preparation method of cobalt-based sulfide is mainly solvothermal method, which usually requires the use of some toxic organic solvents such as N,N-dimethylformamide, etc. (Small, 2020, 16, 2001665). bring many hidden dangers
It can be seen that in the current preparation process, both the preparation of porous graphene and the preparation of cobalt-based sulfides have many shortcomings. The problems such as poor contact between heterogeneous interfaces have limited the development and application of such cobalt-based sulfide / porous graphene non-PGM composite catalytic materials

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  • Porous graphene loaded ferrocobalt sulfide catalyst as well as preparation method and application thereof
  • Porous graphene loaded ferrocobalt sulfide catalyst as well as preparation method and application thereof
  • Porous graphene loaded ferrocobalt sulfide catalyst as well as preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0040] The mixture hydrogel was prepared by hydrothermal method.

[0041] Concrete preparation steps are as follows:

[0042] 1) Put 10mg / mL graphene oxide water-soluble dispersion and 0.56mg / mL melamine formaldehyde dispersion into the reaction kettle liner according to the ratio of graphene oxide and melamine mass ratio of 1:1.5 and stir rapidly for 2.0 h time.

[0043] 2) 1.0 mL of cobalt metal compound (CoCl 2 ·6H 2 O) precursor aqueous solution and 0.5 mL molar concentration of 0.1 mol / L iron metal compound (FeCl 3 ·6H 2 O) Add the aqueous precursor solution to the mixed dispersion in 1), that is, the molar ratio of the two metal compounds is 1:0.5, stir for 2.0 hours, mix evenly, and take out the magneton.

[0044] 3) Seal the reaction kettle, put it into a constant temperature oven, and keep it warm at 180° C. for 12 hours to obtain the mixture hydrogel.

[0045] The morphology of the obtained hybrid hydrogels was characterized by scanning electron microscopy (SEM...

Embodiment 2

[0048] The step of embodiment 2 is similar to that in embodiment 1, other reaction conditions are constant, just the hydrogel obtained in embodiment 1 is mixed with dibenzyl disulfide uniformly, after vacuum drying, carry out heat treatment under argon protection atmosphere, The obtained samples were labeled as Co 8 Fe 8 S 8 @NSG-BA(BA denotes before acid leaching).

[0049] Concrete preparation steps are as follows:

[0050] 1) Redisperse all the mixture hydrogels (10 mL in volume) obtained in Example 1 in a beaker filled with 40 mL of deionized water, add 0.5 g of dibenzyl disulfide, and stir rapidly for 2.0 h; then The beaker was placed in a constant temperature oven at 80°C to dry, and the mixture xerogel was obtained after the water was completely evaporated.

[0051] 2) Grind the xerogel of the mixture obtained in the above 1) and put it into a magnetic boat, transfer it to a tube furnace and heat-treat it at 850°C for 5.0h under an argon atmosphere to obtain a porou...

Embodiment 3

[0055] The steps of embodiment 3 are similar to those in embodiment 2, and other reaction conditions are constant, but the porous graphene-supported cobalt iron sulfide powder material obtained in embodiment 2 is subjected to acid treatment, and the obtained sample is marked as Co 8 Fe 8 S 8 @NSG - A (Adenotes acid leaching).

[0056] Concrete preparation steps are as follows:

[0057] 1) the porous graphene-supported cobalt iron sulfide powder material obtained in embodiment 2 is dispersed in 0.5mol / L H 2 SO 4 In the aqueous solution, 50mL of acid solution was used as the standard according to 1.0g of catalyst, and the sample was stirred and acid-washed for 9.0h at a temperature of 85°C in a condensing reflux device.

[0058] 2) The mixture obtained in the above step 1) is centrifuged and washed with water, and dried to obtain an acid-treated porous graphene-supported cobalt iron sulfide powder sample.

[0059] image 3 It is the SEM and TEM photo of the acid-treated po...

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Abstract

The invention relates to a porous graphene loaded ferrocobalt sulfide catalyst as well as a preparation method and application thereof, and belongs to the technical field of clean energy nano materials and catalysis. Graphene oxide, melamine, formaldehyde, a cobalt source and an iron source are subjected to a hydrothermal reaction to prepare graphene hydrogel, and the graphene hydrogel and a sulfur source are fully mixed and then subjected to high-temperature heat treatment in a protective atmosphere to prepare the porous graphene loaded ferrocobalt sulfide powder material. The powder is subjected to acid pickling and secondary heat treatment to prepare the porous graphene loaded ferrocobalt sulfide nano-particles, the nano-particles are of a special core-shell structure, and the particle size is 21-24 nm. The material shows excellent catalytic activity and stability when being used as an oxygen reduction and oxygen evolution catalyst of an alkaline reaction system, and can be applied to electrode materials of fuel cells and zinc-air batteries.

Description

technical field [0001] The invention relates to a porous graphene-supported cobalt-iron sulfide catalyst, a preparation method and an application, and belongs to the technical field of clean energy nanomaterials and catalysis. Background technique [0002] At present, platinum-group metals (PGM) are considered to be the best performing oxygen reduction reaction (Oxygen reduction reaction, ORR) and oxygen evolution reaction due to their ideal electronic structure and high density of under-coordinated surface atoms. Oxygen evolution reaction (OER) electrocatalytic materials, but limited reserves and high cost limit its wide application in fuel cells and zinc-air batteries (Adv. Mater., 2021, 33(6): 2000381). Therefore, the development of low-cost non-PGM catalysts is the key technology to promote the commercialization of fuel cells and zinc-air batteries, and has become a research hotspot. Carbon-supported cobalt-based sulfides such as CoS 2 、Co 3 S 4 and Co 9 S 8 Combin...

Claims

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Application Information

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IPC IPC(8): H01M4/90H01M4/88C01B32/184C01B32/194C01G51/00B82Y30/00
CPCH01M4/90H01M4/9083H01M4/88C01B32/184C01B32/194C01G51/30C01G51/006B82Y30/00Y02E60/50
Inventor 李毅杨娟武子瑞成超刘振中王永瑛
Owner JIANGSU UNIV
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