阅读说明：本技术 一种FeOOH@Ni-BDC电解水催化剂的制备方法 (Preparation method of FeOOH @ Ni-BDC water electrolysis catalyst ) 是由 徐波 杨晓冬 陈亚诞 李超 李村成 于 2019-09-20 设计创作，主要内容包括：本发明涉及一种碳布负载的FeOOH@Ni-BDC复合电解水催化剂及其制备方法,属于新型无机纳米功能材料制备技术领域。本发明以碳布负载的FeOOH纳米片阵列为模板,通过水热法制备在其上包覆Ni-BDC形成FeOOH@Ni-BDC复合催化剂。具体步骤如下：首先通过电沉积法以硫酸亚铁铵,醋酸钠和硫酸钠混合溶液为电解液制得碳布负载的FeOOH纳米片阵列为模板；进一步在溶剂热条件下使用氯化镍和对苯二甲酸形成金属有机骨架并包覆在FeOOH纳米片上制得FeOOH@Ni-BDC复合电解水催化剂。(The invention relates to a carbon cloth loaded FeOOH @ Ni-BDC composite electrolyzed water catalyst and a preparation method thereof, belonging to the technical field of preparation of novel inorganic nano functional materials. The invention takes a carbon cloth loaded FeOOH nanosheet array as a template, and prepares the FeOOH @ Ni-BDC composite catalyst formed by coating Ni-BDC on the carbon cloth loaded FeOOH nanosheet array by a hydrothermal method. The method comprises the following specific steps: firstly, preparing a carbon cloth loaded FeOOH nanosheet array as a template by using an electrodeposition method and using a mixed solution of ammonium ferrous sulfate, sodium acetate and sodium sulfate as an electrolyte; further using nickel chloride and terephthalic acid to form a metal organic framework under the solvothermal condition and coating the metal organic framework on the FeOOH nano-sheet to prepare the FeOOH @ Ni-BDC composite electrolyzed water catalyst.)

1. A preparation method of a carbon cloth loaded FeOOH @ Ni-BDC composite electrolyzed water catalyst is characterized by comprising the following steps:

1) adopting an electrodeposition method, and taking ammonium ferrous sulfate, sodium acetate and sodium sulfate mixed solution as electrolyte to prepare a carbon cloth loaded FeOOH nanosheet array as a template;

2) adding nickel chloride, terephthalic acid and N, N' -dimethylformamide into another reaction kettle, transferring the carbon cloth loaded FeOOH nanosheet array obtained in the step 1 into the reaction kettle, and then preparing the carbon cloth loaded FeOOH @ Ni-BDC composite electrolyzed water catalyst through solvothermal reaction.

2. The preparation method of the carbon cloth supported FeOOH @ Ni-BDC composite electrolyzed water catalyst according to claim 1, wherein the composite catalyst is prepared by using a carbon cloth supported FeOOH nanosheet array as a template.

3. The method of claim 1, wherein the metal organic framework of the composite catalyst is formed from nickel chloride and terephthalic acid under solvothermal conditions.

Technical Field

The invention relates to a FeOOH @ Ni-BDC composite electrolyzed water catalyst and a preparation method thereof, belonging to the technical field of novel inorganic nano functional materials.

Background

In recent years, the problems of energy shortage, environmental pollution and the like are increasingly paid high attention, and the development of a novel clean energy technology is urgent. Electrolyzed water has received wide attention as an effective hydrogen production method. However, from the chemical thermodynamic perspective, the water splitting process belongs to a non-spontaneous chemical reaction and needs an additional overpotential to drive the water splitting process, so that the development of a high-efficiency and stable catalyst has important significance for improving the efficiency of water electrolysis and reducing the consumption of electric energy. At present, most of catalysts with the best catalytic performance for the reaction of electrolyzed water are precious metal materials such as platinum, rhodium, iridium and the like, the price is high, the sources are rare, and the wide utilization of the catalysts is seriously restricted. Recent research results of scientists show that transition metal-based catalysts represented by iron, cobalt and nickel, such as nickel oxide, cobalt sulfide and the like, have excellent water electrolysis performance, and the materials are low in price and suitable for large-scale application. However, the preparation of such catalysts often requires high-temperature heat treatment, and the products inevitably aggregate to some extent, thereby reducing the catalytic activity. Meanwhile, the high-temperature heating process also has the defects of high energy consumption, complex reaction process, incapability of accurate quantitative control and the like.

Iron oxyhydroxide (FeOOH) is often used to prepare electrolytic water catalysts because of its advantages such as exposed active sites, low cost, etc. But FeOOH has poor conductivity, small specific surface area and low mass transfer efficiency, so the catalytic effect is not ideal enough. The metal organic framework has the characteristics of open structure, high specific surface area and the like. The FeOOH and the metal organic framework are combined, so that the coordination effect of the FeOOH and the metal organic framework can be exerted, the advantage complementation is realized, and the composite electrolyzed water catalyst with excellent performance is prepared. The invention combines a metal organic framework (Ni-BDC) formed by nickel chloride and terephthalic acid with FeOOH, develops a preparation method of the composite electrolyzed water catalyst with low cost, simplicity, convenience, practicability and low energy consumption by utilizing the characteristics of the nickel chloride and the FeOOH, and prepares the FeOOH Ni-BDC composite electrolyzed water catalyst with excellent catalytic performance.

Disclosure of Invention

The invention aims to provide a preparation method of a FeOOH @ Ni-BDC composite electrolyzed water catalyst, which has low cost and is simple and easy to implement. The preparation method provided by the invention has the advantages of simple process and low cost, and the prepared FeOOH @ Ni-BDC has excellent electrolytic water catalytic performance and higher practical application value.

The invention aims to realize the preparation method of the FeOOH @ Ni-BDC composite electrolyzed water catalyst by the following technical scheme, which comprises the following steps:

1) respectively carrying out ultrasonic treatment on carbon cloth (2 multiplied by 1 cm) cut in advance for 15 minutes by using 5% hydrochloric acid, acetone and deionized water;

2) immersing the carbon cloth obtained in the step 1 into a mixed solution containing ammonium ferrous sulfate, sodium acetate and sodium sulfate with a certain concentration, and performing electrodeposition under a certain current intensity to prepare a carbon cloth-loaded FeOOH nanosheet array;

3) adding nickel chloride and terephthalic acid in a certain molar ratio into a hydrothermal reaction kettle, adding N, N' -dimethylformamide in a certain volume, and stirring for dissolving;

4) and (3) adding the carbon cloth loaded FeOOH obtained in the step (2) into the reaction kettle solution obtained in the step (3), and then placing the mixture into an oven to be heated to obtain the carbon cloth loaded FeOOH @ Ni-BDC composite electrolyzed water catalyst.

The invention has the beneficial effects that:

(1) the invention provides a preparation method of a novel FeOOH @ Ni-BDC composite electrolytic water catalyst, which comprises the steps of firstly preparing a carbon cloth loaded FeOOH nanosheet array through simple electrodeposition, and then continuously preparing the FeOOH @ Ni-BDC array through a hydrothermal method by taking the carbon cloth loaded FeOOH array as a template. The preparation method is simple and easy to operate, does not need special equipment, has low cost, is suitable for large-scale preparation, and can meet the requirements of practical application;

(2) the product prepared by the method is a carbon cloth loaded FeOOH @ Ni-BDC nanosheet array, the product is regular in appearance and uniform in size, and the carbon cloth is used as a carrier to load a catalyst, so that the method is beneficial to practical application;

(3) the FeOOH @ Ni-BDC composite electrolyzed water catalyst prepared by the invention effectively combines the advantages of the two components, and utilizes the synergistic effect of the two components to obtain the catalyst with excellent catalytic performance and good stability;

(4) the preparation of the invention only needs common equipment in a laboratory, does not need special equipment, and has simple and easy technical process.

Drawings

FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a FeOOH @ Ni-BDC nanosheet array composite electrolytic water catalyst prepared by the method of the present invention taken after being observed with a scanning electron microscope of FEI QUANTA FEG 250;

FIG. 2 is an X-ray diffraction (XRD) pattern of the FeOOH @ Ni-BDC nanosheet array composite electrolytic water catalyst prepared by the method of the present invention.

Detailed Description

The present invention will be described in further detail with reference to the following embodiments, which are not intended to limit the scope of the present invention.