CN-121972191-A - Method for preparing catalyst by adsorbing phosphine through preparation of layered porous metal oxide

Abstract

The invention discloses a method for preparing a catalyst by adsorbing phosphine through preparing a layered porous metal oxide, and belongs to the technical field of electrocatalytic materials. The preparation method comprises the following steps of S1, preparing a nickel source precursor or a cobalt source precursor from a nickel source or a cobalt source, and S2, placing the nickel source precursor or the cobalt source precursor into a quartz tube, placing the quartz tube into a tube furnace, and introducing phosphine to prepare the electrocatalyst containing Ni x1 P y1 or Co x2 P y2 . The layered porous metal oxide prepared by the invention is different from the common metal oxide in the structural superiority, so that the efficient adsorption of phosphine gas can be realized, and the formed layered porous metal nickel phosphide and cobalt phosphide material has wide application prospect in the field of electrocatalytic water decomposition hydrogen production due to the structural superiority.

Inventors

• CUI SHUO
• LIU YANZHANG
• CHENG YU
• CHEN KAI
• JIA LIJUAN
• FENG JIAYU
• WANG FANG
• CAO RUI
• PAN ZIBIN
• NING PING

Assignees

• 云南民族大学

Dates

Publication Date

20260505

Application Date

20260122

Claims (8)

1. 1. A method for preparing an electrocatalyst by preparing a layered porous metal oxide adsorbed phosphine comprising the steps of: S1, preparing a nickel source or cobalt source to obtain a nickel source precursor or cobalt source precursor; And S2, placing the nickel source precursor or the cobalt source precursor into a quartz tube, placing the quartz tube into a tube furnace, and introducing phosphine to prepare the electrocatalyst containing Ni x1 P y1 or Co x2 P y2 .
2. 2. A method of preparing an electrocatalyst by adsorption of phosphine by preparing a layered porous metal oxide according to claim 1, wherein x1=2 or 5, y1=1 or 4, x2=1 or 2, y2=1.
3. 3. A method for preparing an electrocatalyst by adsorption of phosphine by preparing a layered porous metal oxide according to claim 2, wherein the method for preparing the cobalt source precursor comprises the steps of: s1.1, adding Co (CH 3 CO 2 ) 2 ·4H 2 O into H 2 NCONH 2 solution, and stirring to obtain purple solution; S1.2, carrying out hydrothermal treatment on the purple solution, washing and drying to obtain purple powder; And S1.3, roasting, crushing and screening the purple powder to obtain a cobalt source precursor.
4. 4. A method for preparing an electrocatalyst by adsorption of phosphine by preparing a layered porous metal oxide according to claim 2, wherein the method for preparing the nickel source precursor comprises the steps of: S1.4, dissolving Ni (CH 3 CO 2 ) 2 .4H2O and HOCH 2 CH 2 NH 2 in H 2 O to obtain a green solution; s1.5, carrying out hydrothermal treatment on the green solution, washing and drying to obtain green powder; and S1.6, roasting, crushing and screening the green powder to obtain a nickel source precursor.
5. 5. The method for preparing the electrocatalyst by adsorbing phosphine by using the layered porous metal oxide according to claim 3, wherein the concentration of Co (CH 3 CO 2 ) 2 · 4H 2 O is 0.4mol L -1 , the concentration of H 2 NCONH 2 is 0.8mol L -1 , the mass ratio of Co (CH 3 CO 2 ) 2 ·4H 2 O to H 2 NCONH 2 is 1:2), the stirring time is 30-60 minutes, the hydrothermal condition is that the mixture is hydrothermal at 100 ℃ for 10-15 hours, the mixture is washed by deionized water, the drying condition is that the temperature is 60-80 ℃ and the drying time is 5-12 hours, the baking condition is that the temperature is 400-500 ℃ and the drying time is 80-120 minutes, and a 40-60-mesh sieve is selected for sieving.
6. 6. The method for preparing the electrocatalyst by adsorbing phosphine by using the layered porous metal oxide according to claim 3, wherein the concentration of phosphine is 1000ppm to 1050ppm, the phosphating temperature is 300 ℃ to 340 ℃, the flow rate of phosphine is 100mL/min, and the phosphating time is 300min to 360min, so that the electrocatalyst containing Co x2 P y2 is obtained.
7. 7. The method for preparing the electrocatalyst by adsorbing phosphine by using the layered porous metal oxide according to claim 4, wherein the concentration of Ni (CH 3 CO 2 ) 2 · 4H 2 O is 0.4mol L -1 , the mass ratio of Ni (CH 3 CO 2 ) 2 ·4H 2 O to H 2 NCONH 2 and H 2 O is 5:5:17), the stirring time is 30-60 minutes, the hydrothermal condition is that the temperature is 120 ℃ for 24-64 hours, the washing is performed by deionized water, the drying condition is that the temperature is 60-80 ℃ for 5-12 hours, the roasting condition is that the temperature is 400-500 ℃ for 80-120 minutes, and a 40-60 mesh sieve is selected for sieving.
8. 8. The method for preparing the electrocatalyst by adsorbing phosphine by using the layered porous metal oxide according to claim 7, wherein the concentration of phosphine is 1000ppm to 1050ppm, the phosphating temperature is 340 to 380 ℃, the flow rate of phosphine is 100mL/min, and the phosphating time is 300min to 360min, so as to obtain the electrocatalyst containing Ni x1 P y1 .

Description

Method for preparing catalyst by adsorbing phosphine through preparation of layered porous metal oxide Technical Field The invention relates to the technical field of electrocatalytic material engineering, in particular to a method for preparing a catalyst by adsorbing phosphine by preparing layered porous metal oxide. Background The gas sensor has wide application in the fields of environmental quality monitoring, industrial production, indoor gas detection and the like, plays an increasingly important role in production activities and daily living, has the advantages of high response speed, low cost, high sensitivity, long service life and the like, is mainly studied for improving the gas sensitivity of metal oxide materials, mainly comprises three aspects of nano structures, layered porous structures and noble metal surface modification, can increase the surface area of the materials to provide more gas channels and improve the utilization rate of the materials by the three measures, can provide more surface active sites to enable the materials to directly contact target gases, not only increases physical and chemical adsorption, but also greatly shortens response and recovery time, and is a very few porous structures of Co 3O4 and NiO which are important gas sensitive materials due to high sensitivity, low cost and high strength in a plurality of semiconductor metal oxides. Phosphine is a flammable and explosive gas with strong biological toxicity, and is discharged into the atmosphere without treatment to seriously threaten human health and ecological environment, and also indirectly cause greenhouse effect, the tail gas discharged by the phosphorus chemical industry is one of main sources of phosphine in the atmosphere, and the concentration of phosphine in the tail gas discharged by a yellow phosphorus production factory is about 1000ppm, so that PH 3 in the tail gas needs to be effectively treated in order to ensure human health and protect environment. The high-efficiency production of high-purity hydrogen is of great significance in energy technology, for example, the economic production of hydrogen fuel can enable aviation without carbon dioxide emission, but the premise is that hydrogen is realized through a carbon-free technology, compared with methane reforming and coal gasification, electrocatalytic water decomposition provides an environment-friendly hydrogen production mode, the high-efficiency production of high-purity hydrogen can also effectively convert and store intermittent renewable electric energy such as wind energy and solar energy, electrolysis of water consists of two main half-reactions, particularly Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER), a high-efficiency stable catalyst is required for reducing activation energy so as to accelerate kinetics, the traditional use of noble metal catalysts is greatly limited by low availability and high cost of the catalysts, therefore, development of low-cost high-efficiency non-noble metal catalysts for the reactions is very important, a transition metal phosphide electrocatalytic material has excellent conductivity, abundant active sites and lower cost, and the high-efficiency catalyst is proved to be an ideal alternative for the hydrogen production field of electrocatalytic water decomposition, the high-efficiency platinum and platinum-based catalyst is used as an ideal catalyst, and the low-cost phosphorus-containing material is fully realized by the current research of a phosphorus-containing material under the high-chemical-temperature phosphorus-based material and the preparation of a phosphorus-containing material is realized by the high-temperature and a relatively-complex process of preparing phosphorus-containing material through the present heating phosphorus-chemical process. Therefore, the method for preparing the catalyst by preparing the layered porous metal oxide to adsorb phosphine by avoiding secondary pollution and realizing efficient PH 3 adsorption is a technical problem to be solved in the field. Disclosure of Invention The invention aims at providing a method for preparing a catalyst by adsorbing phosphine by preparing a layered porous metal oxide, the layered porous metal oxide material is synthesized while realizing high-efficiency removal of hydrogen phosphide in tail gas, and the electrocatalyst is beneficial to green energy generation. In order to achieve the above purpose, the present invention adopts the following technical scheme: A method for preparing an electrocatalyst by preparing a layered porous metal oxide adsorbing phosphine comprising the steps of: S1, preparing a nickel source or cobalt source to obtain a nickel source precursor or cobalt source precursor; And S2, placing the nickel source precursor or the cobalt source precursor into a quartz tube, placing the quartz tube into a tube furnace, and introducing phosphine to prepare the electrocatalyst containing Ni x1Py1 or