阅读说明：本技术 一种类海胆状镍铁膦酸盐光催化剂及其制备方法 (Sea urchin-like nickel-iron phosphonate photocatalyst and preparation method thereof ) 是由 邢伟男 张亭亭 吴光瑜 韩建刚 朱咏莉 马芳 卢然 卫钰涵 李萍萍 于 2020-07-14 设计创作，主要内容包括：本发明公开了一种类海胆状镍铁膦酸盐光催化剂及其制备方法,属于材料制备技术领域。该制备方法包括：(1)将镍铁硝酸盐溶于N,N-二甲基甲酰胺中,得到溶液A；将苯基膦酸用N,N-二甲基甲酰胺溶解,得到溶液B；(2)将溶液A逐滴加入到溶液B中,在溶剂热条件下反应,得到类海胆状镍铁膦酸盐光催化剂。本发明工艺操作简单,结构稳定,可重复性高,能满足实验室和工业需求。该类海胆状镍铁膦酸盐光催化剂具有良好的光催化产氧性能。(The invention discloses a sea urchin-like nickel-iron phosphonate photocatalyst and a preparation method thereof, belonging to the technical field of material preparation. The preparation method comprises the following steps: (1) dissolving nickel iron nitrate in N, N-dimethylformamide to obtain a solution A; dissolving phenylphosphonic acid by using N, N-dimethylformamide to obtain a solution B; (2) and dropwise adding the solution A into the solution B, and reacting under the solvothermal condition to obtain the echinoid nickel iron phosphonate photocatalyst. The invention has simple process operation, stable structure and high repeatability, and can meet the requirements of laboratories and industries. The echinoid nickel iron phosphonate photocatalyst has good photocatalytic oxygen production performance.)

1. A preparation method of a sea urchin-like nickel-iron phosphonate photocatalyst is characterized by comprising the following steps:

(1) dissolving nickel iron nitrate by using N, N-dimethylformamide to obtain a solution A, and dissolving phenylphosphonic acid by using N, N-dimethylformamide to obtain a solution B;

(2) and adding the solution A into the solution B for reaction, centrifuging after the reaction is finished to obtain a precipitate, and washing and drying the precipitate to obtain the echinoid nickel iron phosphonate photocatalyst.

2. The preparation method of the echinoid ferronickel phosphonate photocatalyst according to claim 1, wherein the solution A is prepared by dissolving 1-4 mmol of nickel nitrate in 5-30 mL of N, N-dimethylformamide at room temperature, and the molar ratio of the nickel nitrate to the iron nitrate in the nickel nitrate is 1: 1-3: 1.

3. The method for preparing the sea urchin-like nickel-iron phosphonate photocatalyst according to claim 1, wherein the solution B is dissolved in 10-40 mL of N, N-dimethylformamide per 1-6 mmol of phenylphosphonic acid at room temperature.

4. The method for preparing the sea urchin-like nickel-iron phosphonate photocatalyst according to claim 1, wherein the solution A is continuously stirred and dropwise added into the solution B at room temperature, and the reaction is carried out at 120-200 ℃ for 30-60 h.

5. The method of preparing a echinoid ferronickel phosphonate photocatalyst of any one of claims 1 to 4, to produce an echinoid ferronickel phosphonate photocatalyst.

Technical Field

The invention belongs to the technical field of material preparation, and particularly relates to a sea urchin-like nickel-iron phosphonate photocatalyst and a preparation method thereof.

Background

With the rapid development of industrial society and the increasing improvement of the living standard of people, non-renewable energy sources such as coal, petroleum and the like are being consumed, and the environment pollution and ecological destruction brought by the consumption are threatening the earth on which human beings rely to live. How to solve the above problems also becomes the focus of intense attention. Solar energy is a clean renewable energy source with wide distribution and rich content. Various solar energy conversion and storage technologies have been developed to better utilize solar energy.

The photocatalysis technology is to utilize solar energy, which is clean renewable energy, to decompose and convert pollutants in the environment into nontoxic harmless micromolecules or new renewable energy, and can treat the pollutants and bring clean energy while ensuring no new pollution. Therefore, the photocatalytic technology is considered as an effective means that can solve the problems of global energy shortage and environmental pollution. Water oxidation has been considered the most challenging step as a half-reaction of the photocatalytic water splitting process, mainly it requires a minimum potential of 1.23V to supply electrons and protons to the other half-reaction and eventually form two O-O bonds. Therefore, it is of great importance to develop efficient water oxidation catalysts to meet the harsh water oxidation conditions.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation method of the echinoid-like nickel-iron phosphonate photocatalyst, which has the advantages of simple synthesis steps and convenient operation, can control the formation of the echinoid-like nickel-iron phosphonate by changing reaction conditions, and has wide application prospect. The invention aims to solve another technical problem of providing a sea urchin-like nickel-iron phosphonate photocatalyst which is stable in structure and has good photocatalytic oxygen production performance.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

a preparation method of a sea urchin-like nickel-iron phosphonate photocatalyst comprises the following steps:

(1) dissolving nickel iron nitrate by using N, N-dimethylformamide to obtain a solution A, and dissolving phenylphosphonic acid by using N, N-dimethylformamide to obtain a solution B;

(2) and adding the solution A into the solution B for reaction, centrifuging after the reaction is finished to obtain a precipitate, and washing and drying the precipitate to obtain the echinoid nickel iron phosphonate photocatalyst.

According to the preparation method of the echinoid ferronickel phosphonate photocatalyst, at room temperature, the solution A is prepared by dissolving 1-4 mmol of nickel nitrate iron nitrate into 5-30 mL of N, N-dimethylformamide, and the molar ratio of the nickel nitrate to the iron nitrate in the nickel nitrate is 1: 1-3: 1.

According to the preparation method of the echinoid ferronickel phosphonate photocatalyst, at room temperature, the solution B is prepared by dissolving 1-6 mmol of phenylphosphonic acid in 10-40 mL of N, N-dimethylformamide.

The preparation method of the echinoid ferronickel phosphonate photocatalyst comprises the steps of continuously stirring the solution A and dropwise adding the solution A into the solution B at room temperature, and reacting for 30-60 hours at 120-200 ℃.

The preparation method of the echinoid ferronickel phosphonate photocatalyst prepares the echinoid ferronickel phosphonate photocatalyst.

Has the advantages that: compared with the prior art, the invention has the advantages that:

the sea urchin-like nickel-iron phosphonate photocatalyst disclosed by the invention has the advantages of simple synthesis steps, stable structure, convenience in operation, safety, environmental friendliness, high repeatability and the like. The catalyst has high-efficiency photocatalytic oxygen production performance.

Drawings

FIG. 1 is an SEM image of a sample NiFeP-1;

FIG. 2 is an XRD pattern of a sample NiFeP-1;

FIG. 3 is a diagram showing the photocatalytic oxygen generation performance of NiP, NiFeP-1, NiFeP-2 and NiFeP-3;

FIG. 4 is a FT-IR comparison before and after the photocatalytic reaction of sample NiFeP-1.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.