CN-116607165-B - Ni (nickel)11(HPO3)8(OH)6/Mo8O23Foam nickel dual-function composite electrode and preparation method thereof

Abstract

The invention discloses a Ni 11 (HPO 3 ) 8 (OH) 6 /Mo 8 O 23 /foam nickel dual-function composite electrode and a preparation method thereof, wherein a multistage structure composite microsphere formed by assembling a Ni 11 (HPO 3 ) 8 (OH) 6 nano sheet and a Mo 8 O 23 nano sheet is grown on the surface of metal foam nickel in situ by utilizing a simple one-step hydrothermal reaction, a self-supporting composite electrode is constructed, the self-supporting composite electrode is grown on the surface of the metal foam nickel in situ, more exposed active sites and more interface transfer active sites are endowed to a catalyst, and the diffusion of electrolyte, multi-site adsorption of protons and the rapid escape of generated H 2 are facilitated. In addition, the construction of the self-supporting electrode greatly improves the charge migration efficiency, effectively avoids the falling of the catalyst and increases the stability of the electrode. The composite electrode has simple preparation process and low cost. The catalyst is used for preparing high-added-value fine chemicals by electrocatalytic decomposition of water to produce hydrogen and electrocatalytic oxidation of biomass, and has excellent electrocatalytic activity and stability in the aspects of electrocatalytic oxidation of urea, electrocatalytic degradation of organic dye, treatment of organic chemical wastewater and the like.

Inventors

• SONG CAIXIA
• Xing Miaomiao
• SUN RUIHONG
• LIU XIAOYUAN
• WANG DEBAO

Assignees

• 青岛科技大学

Dates

Publication Date

20260512

Application Date

20230524

Claims (1)

1. 1. The Ni 11 (HPO 3 ) 8 (OH) 6 /Mo 8 O 23 /foam nickel dual-function composite electrode is characterized in that the composite electrode is a self-supporting electrode formed by multi-stage structure composite microspheres assembled by Ni 11 (HPO 3 ) 8 (OH) 6 nano sheets and Mo 8 O 23 nano sheets which grow on the surface of metal foam nickel in situ, the dual-function composite electrode is used for producing hydrogen by cathode water reduction and preparing 2, 5-furandicarboxylic acid by selective oxidation of 5-hydroxymethylfurfural of an anode and performing electrooxidation purification treatment on organic chemical wastewater, and the preparation of the composite electrode comprises the following steps: (1) Respectively carrying out ultrasonic cleaning treatment on foam nickel with the size of 1-10 cm x 1-10 cm by using acetone, 0.1M hydrochloric acid, deionized water and ethanol in sequence; (2) Dissolving 0.1-10 mmol of NiCl 2 ·6H 2 O,0.1 – 10 mmol Na 2 MoO 4 ·2H 2 O and 0.5-50 of mmol urea in 15-150 mL of deionized water under stirring; (3) Dissolving 0.1-20 mmol sodium hypophosphite in 15-150 mL deionized water to obtain sodium hypophosphite solution, and adding the solution into the mixed solution obtained in the step (2) under stirring; (4) Transferring the mixed solution obtained in the step (3) and 1-10 pieces of foam nickel treated in the step (1) into a stainless steel reaction kettle with a Teflon lining, preserving the heat of the sealed reaction kettle at 80-200 o ℃ for 0.5-48 h, taking out the foam nickel after the reaction kettle is cooled to room temperature, and washing the foam nickel with deionized water and ethanol to obtain the Ni 11 (HPO 3 ) 8 (OH) 6 / Mo 8 O 23 /foam nickel dual-function composite electrode.

Description

Ni 11(HPO3)8(OH)6/Mo8O23/foam nickel dual-function composite electrode and preparation method thereof Technical Field The invention belongs to the field of new energy, environment and biomass conversion, relates to a composite electrode and a preparation method thereof, in particular to a Ni 11(HPO3)8(OH)6 nano-sheet and Mo 8O23 nano-sheet heterojunction composite electrode grown on a foam nickel metal framework in situ, and further relates to a Ni 11(HPO3)8(OH)6/Mo8O23/foam nickel dual-function composite electrode for preparing new energy of hydrogen and converting biomass and a preparation method thereof. Background Hydrogen, which is a clean, renewable energy carrier, is recognized as the best alternative to traditional energy, and electrolytic water to produce hydrogen is a sustainable, efficient method of producing hydrogen. However, the Hydrogen Evolution Reaction (HER) occurring at the cathode and the Oxygen Evolution Reaction (OER) at the anode during electrolysis are thermodynamically and kinetically slow, resulting in a higher overpotential being required during the electrolytic water hydrogen evolution reaction. Therefore, there is a need in the field of hydrogen production by electrolysis of water to develop electrocatalysts having high catalytic activity and high chemical stability. In the disclosed technology, transition metal compounds are widely used as catalysts for hydrogen production by water electrolysis. Among them, transition metal phosphate catalysts are typical representatives of emerging non-noble metal catalysts because of their low cost, environmental friendliness, high stability, unique physicochemical properties, and tunable versatility. However, the characteristics of poor conductivity and unsatisfactory porosity of transition metal phosphates limit their further catalytic activity and require modification. Molybdenum oxide is an important material in many fields (as an electric, a photocatalyst, other catalysts, etc.), and molybdenum oxide-based materials are diversified in applications in different fields due to the variability of molybdenum and the easy combination with various anions, wherein Mo 8O23 is a multifunctional molybdenum oxide, and attracts attention in the field of catalysis. According to the research, the invention utilizes Ni 11(HPO3)8(OH)6 to be compounded with Mo 8O23 to prepare the efficient composite electrocatalyst. However, at present, mo 8O23 is prepared by either high-temperature reaction, or single-phase Mo 8O23 is difficult to prepare, or expensive reagent is needed, the production cost is high, the process is complex, and the Ni 11(HPO3)8(OH)6/Mo8O23 composite electrocatalyst is difficult to prepare. Therefore, the development and preparation process of the high-efficiency, stable and durable nickel phosphate/Mo 8O23 composite electrocatalyst with simple process and excellent performance are further required. In addition, the progress of the electrolyzed water is limited due to the inherently slower kinetics and higher reaction energy barrier of the electrolyzed water anode OER. Meanwhile, OER's product oxygen has no significant commercial value and is energy and time consuming to remove after mixing with H 2. In this case, the anodic OER is replaced by anodic biomass oxidation, which is attractive due to its low overpotential and high commercial value. 5-Hydroxymethylfurfural (HMF) is an important biomass platform molecule that can be further converted into various useful substances by oxidation reactions, such as oxidation products of 2, 5-furandicarboxylic acid (FDCA) and the like. In the field of high polymer materials, FDCA can replace terephthalic acid to produce bio-based polyester which is biodegradable and has good performance. Since electrocatalytic HMF oxidation is more thermodynamically and kinetically favored than OER, energy conversion efficiency can be improved. Therefore, the use of electrocatalytic HMF oxidation to replace OER reaction is an effective strategy, which can reduce the applied voltage of cathodic hydrogen evolution and produce high added value biomass fine chemicals at the anode. The invention designs a novel Ni 11(HPO3)8(OH)6/Mo8O23 composite electrocatalyst, and grows the novel Ni 11(HPO3)8(OH)6/Mo8O23 composite electrocatalyst on a foam nickel current collector in situ to prepare a Ni 11(HPO3)8(OH)6/Mo8O23/foam nickel self-supporting composite electrode, and the novel Ni 11(HPO3)8(OH)6/Mo8O23/foam nickel self-supporting composite electrode has excellent electrochemical performances when used for electrocatalytic hydrogen production of a cathode, electrocatalytic HMF oxidation of an anode to prepare FDCA, electrocatalytic oxidation of organic matters in water and electrocatalytic degradation of organic dyes. Disclosure of Invention Aiming at the defects that pure-phase Mo 8O23 is difficult to prepare, the conditions are harsh, the process is complex, the cost is high, tight interface coupling is difficult to realize,