The invention provides a three-dimensional multi-level structure type high-dispersion nickel-based electro-catalytic material and a preparation method thereof. The method takes foam nickel as a conducting matrix and a nickel source needed by reaction is provided; urea is used as a precipitating agent, ammonium fluoride is used as an etching agent and an NiAl-LDH//NF precursor grows on the surfaceof a foam nickel framework structure in situ; negative ions including H2PO4 and B(OH)4 are introduced into hydrotalcite layers through an ion exchanging method; a hydrotalcite intermediate containing the negative ions is reduced at high temperature to obtain the three-dimensional multi-level structure type high-dispersion nickel-based electro-catalytic material; a chemical formula is NiY-Al2O3/NF, wherein Y is one of P or B. The material is used for electro-catalytic oxygen evolution reaction under an alkaline condition; when the current density reaches 10mA.cm , the overpotential ofthe oxygen evolution reaction is 270 to 190mV. When the material is used for carrying out selective electro-catalytic oxidization reaction on 5-hydroxymethylfurfural under the alkaline condition, theconversion rate and the selectively reach 92 to 100 percent and 95 to 100 percent respectively, and the invention proves that the material is suitable for being used as the electro-catalytic material.

Three-dimensional multi-level structure type high-dispersion nickel-based electro-catalytic material and preparation method thereof

The invention discloses a self-supporting nickel phosphide catalyst and a preparation method and application thereof. The self-supporting nickel phosphide catalyst is a nickel phosphide catalyst obtained by in-situ growing of a nickel oxalate or nickel hydroxide crystal layer on a framework matrix through a hydrothermal method and performing phosphating while secondary forming is not needed, and the nickel phosphide catalyst is composed of the framework matrix and a nickel-phosphorus compound, wherein the nickel-phosphorus compound is at least one of Ni3P, Ni12P5, Ni2P and Ni5P4, total mass ratio of the nickel-phosphorus compound is 0.1-50%, and the balance is the framework matrix. Experiments show that the self-supporting nickel phosphide catalyst is high in stability and thermal conductivity, easy to form and fill, high in flux and low in pressure drop, especially has the advantages of high low-temperature activity, high dimethyl oxalate conversion rate and high methyl glycolate selectivity and can be used as a reaction catalyst for hydrogenating dimethyl oxalate to prepare methyl glycolate.

Self-supporting nickel phosphide catalyst and preparation method and application thereof

The invention discloses a catalyst for a reaction of water electrolysis for producing hydrogen, i.e. 3D mesoporous FePx and a preparation method thereof. Through physical vapor deposition, ferrocene is supported in pores in a carrier, SBA-15; then the SBA-15 template is removed through high-temperature calcination to obtain 3D mesoporous FeOx; furthermore, a low temperature reaction is carried outwith NaH2PO2 to obtain the product. The FePx catalyst is weak-crystalline FeP and has the 3D mesoporous structure and large specific surface area. The preparation method is simple, is environment-friendly and is low in cost, and has high catalytic activity when being used as a water electrolysis HER catalyst.

Preparation of FePx having 3D mesoporous structure, and application thereof in water electrolysis for producing hydrogen

The invention relates to the technical field of electrode materials, in particular to a graphene outer layer@nickel phosphide interlayer@nickel inner layer frame composite material and a preparation method and application thereof. The preparation method of the graphene outer layer@nickel phosphide interlayer@nickel inner layer frame composite material comprises the following steps: providing foamed nickel@graphene; placing the foamed nickel@graphene in an acidic solution for etching to obtain etched foamed nickel@graphene; and carrying out phosphating treatment on the etched foamed nickel@graphene to obtain the graphene outer layer@nickel phosphide interlayer@nickel inner layer frame composite material. By adopting the preparation method provided by the invention, nickel phosphide can be wrapped in an interlayer of graphene and foamed nickel, active site exposure, mass transfer and electron transfer are improved, and the stability and the energy conversion efficiency of the composite material are further improved.

Graphene outer layer@nickel phosphide interlayer@nickel inner layer frame composite material as well as preparation method and application thereof

The invention relates to a preparation method of a self-supporting nickel phosphide foam electrode for water decomposition, and belongs to the field of electrochemistry. The preparation method comprises the following steps: firstly, soaking foamed nickel into an iron chloride containing solution to carry out a skeleton roughening treatment, and then carrying out low-temperature gas-phase phosphating reaction on the obtained foamed nickel in a tubular furnace to obtain the final nickel phosphide electro-catalytic oxygen evolution material. The microstructure of the foam electrode is a nano sheet array with a large specific surface area. Effective contact between an electrolyte and an active site is facilitated, diffusion of the electrolyte is promoted, and the catalytic performance is enhanced. The prepared catalyst is loaded on a carrier in-situ, the binding force is strong, thus the catalyst is not easy to fall off, and the contact resistance is small. The prepared oxygen evolution electrode has an excellent electro-catalytic oxygen evolution performance and a low overvoltage. The method is simple and convenient to operate and easy for industrial production, and the raw materialsare cheap.

Preparation method of self-supporting nickel phosphide foam electrode for water decomposition

The invention relates to the technical field of electrolytic hydrogen production, in particular to a preparation method of an integrated nickel-based porous nickel phosphide hydrogen evolution electrode. The preparation method of the integrated nickel-based porous nickel phosphide hydrogen evolution electrode comprises the specific steps that firstly, deionized water is prepared, specifically, a mixed solution with the mass ratio of organic alcohols being 1:(0-100) is prepared; secondly, weak acid is added into the mixed solution obtained in the first step, so that a weak acid solution with the weak acid concentration being 0.01-2 mol/L is prepared; thirdly, a foamed nickel substrate is added into the weak acid solution prepared in the second step, and then the etching reaction is conducted at the temperature of 10-100 DEG C for 1-10 hours, so that a nickel-based porous nickel precursor is obtained; fourthly, the nickel-based porous nickel precursor is taken out, washed with the deionized water and then dried; and fifthly, the nickel-based porous nickel precursor treated in the fourth step and sodium hypophosphite are placed in the hydrogen and inert gas mixed atmosphere for phosphating treatment at the temperature of 250-400 DEG C, and thus the integrated nickel-based porous nickel phosphide electrode is obtained. By adoption of the solution, the problems that an existing phosphide hydrogen evolution catalyst has few hydrogen evolution active sites and is poor in stability are solved.

Xiong Kun

Papers

Preparation method of integrated nickel-based porous nickel phosphide hydrogen evolution electrode