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A kind of preparation method of nitrogen-doped graphene supported metal single-atom catalyst

A nitrogen-doped graphene, metal-loaded technology is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., to achieve the effect of simple and practical preparation methods

Active Publication Date: 2020-05-05
TSINGHUA UNIV
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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a general method for the simple and high-efficiency mass preparation of nitrogen-doped graphene-supported metal single-atom catalysts in view of the current state of the art that cannot simply and macro-preparate graphene-supported metal single-atom catalysts At the same time, the prepared catalyst has the advantages of high metal loading, wide coverage of metal types, and high atomic dispersion.

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  • A kind of preparation method of nitrogen-doped graphene supported metal single-atom catalyst
  • A kind of preparation method of nitrogen-doped graphene supported metal single-atom catalyst
  • A kind of preparation method of nitrogen-doped graphene supported metal single-atom catalyst

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preparation example Construction

[0019] The preparation method of a nitrogen-doped graphene-supported metal single-atom catalyst provided by the present invention uses disodium salt of ethylenediaminetetraacetic acid as a complexing agent to form a stable complex with metal ions in a liquid phase by ion exchange reaction After being evaporated to dryness, it is fully mixed with an alkali metal salt, and a nitrogen-doped graphene-supported metal single-atom catalyst is obtained by synchronous pyrolysis conversion. The preparation method mainly includes the following steps:

[0020] 1) Add the nitrogen-containing organic compound ethylenediaminetetraacetic acid disodium salt and the metal salt into deionized water, the mass ratio of the two is between 1000:1 and 100:1, mix well, and the molar concentration of the metal salt obtained is 0.001~0.5mol / L aqueous solution; then carry out ion exchange reaction at 40~120°C for 0.5~6h to obtain a stable complex, evaporate to dryness and obtain solid powder of the comple...

Embodiment 1

[0028] Preparation of graphene-supported Pd single-atom catalysts:

[0029] Step 1, add 4 g of ethylenediaminetetraacetic acid disodium salt and 12 mg of sodium tetrachloropalladate into deionized water, stir magnetically, react at 80°C for 2 hours, and then evaporate to dryness;

[0030] Step 2, fully mix 4 g of the product obtained in step 1 with 30 g of sodium carbonate, put it into a tube furnace, heat treat at 800° C. for 3 hours under an inert atmosphere, and cool it down to room temperature naturally to obtain a black mixture;

[0031]In step 3, the black mixture obtained in step 2 is sequentially washed and dried with 1M hydrochloric acid solution, pure water and absolute ethanol to obtain a nitrogen-doped graphene-supported metal Pd single-atom catalyst. Such as figure 1 Shown is the image of the graphene-supported Pd single-atom catalyst under the high-angle annular dark-field scanning transmission electron microscope, the bright metal Pd single atoms are uniformly...

Embodiment 2

[0033] Preparation of graphene-supported Pt single-atom catalysts:

[0034] Step 1, add 6 g of ethylenediaminetetraacetic acid disodium salt and 5.6 mg of potassium hexachloroplatinate into deionized water, stir magnetically, react at 80°C for 6 hours, and then evaporate to dryness;

[0035] Step 2, fully mix 6 g of the product obtained in step 1 with 30 g of sodium sulfate, put it into a tube furnace, heat-treat at 850° C. for 2 hours under an inert atmosphere, and cool it down to room temperature naturally to obtain a black mixture;

[0036] In step 3, the black mixture obtained in step 2 is sequentially washed and dried with 0.5 M sulfuric acid solution, pure water and absolute ethanol to obtain a nitrogen-doped graphene-supported metal Pt single-atom catalyst. Such as figure 2 Shown is the image of the graphene-supported Pt single-atom catalyst under a transmission electron microscope. The overall morphology is an ultrathin two-dimensional nanostructure, which has typica...

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Abstract

Disclosed is a preparation method of nitrogen-doped graphene-loaded metal single atom catalysts. As a compounding agent, ethylenediamine tetraacetic acid disodium salt is subjected to an ion exchange reaction with metal ions in liquid phases to form a stable compound, the compound is fully and evenly mixed with alkali metal salt after drying by distillation, and the nitrogen-doped graphene-loaded metal single atom catalysts are obtained through simultaneous pyrolysis conversion. The prepared catalysts have the appearance characteristics of two-dimensional microstructures which are super-thin and large in area, the thickness is 0.5-2 nm, the number of graphene layers is 1-8, the metal load is within 0.01-10 wt%, and the catalysts can be applied to the field of catalysis synthesis of energy, catalysis, medicine and biology. The method can be widely applied to the synthesis of various metal single atom catalysts, obtained metal single atoms can all be firmly riveted on the surface of graphene, the load amount is high, and the thermal stability is good. The method has the advantages of being simple and safe in operation process, low in cost, controllable to prepare, large in synthesis amount, suitable for industrialized production and large-scale application and the like.

Description

technical field [0001] The invention belongs to the technical field of single-atom catalyst preparation, and specifically relates to a Nitrogen-containing organic complexes Simultaneous pyrolytic transformation for the preparation of nitrogen-doped graphene-supported metal single-atom catalysts. Background technique [0002] Reducing the dimension and size of materials to synthesize nano-clusters or single-atom dispersed catalysts can significantly improve the catalytic activity of materials and obtain ideal catalytic efficiency. With the continuous development of nanomaterial synthesis technology, human beings have made great progress in multi-scale material materials, but they still face major challenges in realizing the structural synthesis, regulation and application of single-atom dispersed catalytic materials. Due to the instability of single atoms themselves and their easy aggregation during synthesis and application, so far, simple and efficient mass synthesis of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24
CPCB01J27/24
Inventor 李亚栋朱有启李治彭卿王定胜陈晨
Owner TSINGHUA UNIV
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