阅读说明：本技术 一种钴镍双金属mof纳米管的制备方法 (Preparation method of cobalt-nickel bimetallic MOF (Metal organic framework) nanotubes ) 是由 杨兆艳 徐波 王晓梅 于 2019-09-20 设计创作，主要内容包括：本发明涉及一种钴镍双金属MOF纳米管及其制备方法,属于新型纳米功能材料制备领域。本发明所用材料合成方法为溶液法。具体步骤如下：以N,N-二甲基甲酰胺(DMF)为溶剂,分别配制一定浓度的硝酸钴、硝酸镍、三乙烯二胺溶液。然后分别取一定体积上述所得溶液加入到N,N-二甲基甲酰胺和乙二醇混合溶剂中,在搅拌均匀后向其中加入一定质量的对苯二甲酸固体并超声使其溶解。将上述所得溶液混合后转移到烘箱中加热反应后,经离心、洗涤并真空干燥后得到所述产品。本发明制备方法简便易行,所用原料成本低,实验条件温和适合大规模生产。(The invention relates to a cobalt-nickel bimetallic MOF nanotube and a preparation method thereof, belonging to the field of preparation of novel nanometer functional materials. The material used in the invention is synthesized by a solution method. The method comprises the following specific steps: taking N, N-Dimethylformamide (DMF) as a solvent, and respectively preparing cobalt nitrate, nickel nitrate and triethylene diamine solutions with certain concentrations. Then respectively adding a certain volume of the obtained solution into a mixed solvent of N, N-dimethylformamide and ethylene glycol, uniformly stirring, adding a certain mass of terephthalic acid solid into the mixed solvent, and performing ultrasonic treatment to dissolve the terephthalic acid solid. And mixing the obtained solutions, transferring the mixed solutions into an oven, heating for reaction, centrifuging, washing and drying in vacuum to obtain the product. The preparation method is simple and easy to implement, the cost of the used raw materials is low, the experimental conditions are mild, and the method is suitable for large-scale production.)

1. A cobalt-nickel bimetallic MOF nanotube having a length of about 0.8-1.0 μm and a tube diameter of about 160 nm.

2. A preparation method of cobalt-nickel bimetallic MOF nanotubes is characterized by comprising the following steps:

1) respectively preparing cobalt nitrate, nickel nitrate and triethylene diamine solution with certain concentration by taking N, N-Dimethylformamide (DMF) as a solvent;

2) respectively adding a certain volume of the solution obtained in the step 1) into a mixed solvent of N, N-dimethylformamide and ethylene glycol, uniformly stirring, adding a certain mass of terephthalic acid solid into the mixed solvent, and performing ultrasonic treatment to dissolve the terephthalic acid solid;

3) and 2) mixing the solutions obtained in the step 2), transferring the mixed solutions into an oven, heating and reacting, centrifuging, washing and drying in vacuum to obtain the product.

3. The method for preparing cobalt-nickel bimetallic MOF nanotubes according to claim 2, wherein the solvents used are Ethylene Glycol (EG) and N, N-Dimethylformamide (DMF).

4. The method for preparing cobalt-nickel bimetallic MOF nanotubes according to claim 2, wherein the molar ratio of the cobalt nitrate to the nickel nitrate is in the range of 1: 3 to 3: 1.

5. The method for preparing cobalt-nickel bimetallic MOF nanotubes according to claim 2, wherein the reaction temperature range in the step 3) is 80-100%^oAnd C, the reaction time is 1 to 2 hours.

Technical Field

The invention relates to a metal organic framework nanotube containing two metals of cobalt and nickel and a preparation method thereof, belonging to the technical field of novel inorganic nano functional materials.

Background

Metal-organic frameworks (MOFs) have many advantages of highly ordered structure, large specific surface area, high porosity, easily adjustable composition and structure, etc., so that they exhibit excellent performance in the fields of catalysis, sensing, energy conversion, etc., and have good application value. However, the MOFs materials prepared by the hydrothermal solvothermal method or the solution method are all millimeter-sized, and cannot meet the application requirements in the specific fields of biological imaging, nano catalysis and the like. Therefore, the preparation of the novel nano MOFs material has important significance for expanding the application range and meeting the application requirements in specific fields.

The tubular nano material as a quasi-one-dimensional structure substance has the structural characteristics of ultrahigh surface area-volume ratio, selective exposure of specific crystal faces, many active sites and the like. Meanwhile, the unique electronic structure of the tubular nano material leads the tubular nano material to have excellent catalytic performance, and the tubular nano material is highly concerned by people. In recent years, the preparation and application research of various inorganic nano tubular materials is frequently seen, but the exploration work of the tubular metal organic framework material is still rarely reported. The reason is that the MOFs nanotube with a quasi-one-dimensional structure requires preferential growth along a specific direction in the growth process, and the MOFs material has the characteristic of a three-dimensional structure, so that the contradiction brings great challenges to the preparation of the MOFs nanotube-shaped structure.

The invention adopts a solution method, and successfully prepares an example of the cobalt-nickel bimetallic MOF nanotube by regulating and controlling reaction parameters such as a solvent system, temperature, time and the like. The preparation method is simple and easy to implement, and the prepared cobalt-nickel bimetallic MOF nanotube has the characteristics of regular appearance, uniform size, large specific surface area and the like, and has good application value in the fields of adsorption, catalysis, sensing and the like.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a method for preparing cobalt-nickel bimetallic MOF nanotubes by a solution method. The preparation method has the advantages of simple process, high speed, high efficiency and low cost. The prepared product has uniform size, regular appearance, high specific surface area and high porosity.

The purpose of the invention is realized by the following technical scheme:

1) respectively preparing cobalt nitrate, nickel nitrate and triethylene diamine solution with certain concentration by taking N, N-Dimethylformamide (DMF) as a solvent;

2) adding a certain volume of mixed solvent of N, N-dimethylformamide and ethylene glycol into a glass reaction bottle, then sequentially adding a certain volume of cobalt nitrate, nickel nitrate, triethylene diamine and solution prepared in the step 1), stirring uniformly, adding a certain mass of terephthalic acid solid into the solution, and dissolving the terephthalic acid solid by ultrasonic waves;

3) putting the solution obtained in the step 3) into an oven for heating reaction;

4) centrifuging the reaction mixture obtained in step 3), washing with DMF and ethanol, and then washing at 50 deg.C^oAnd C, vacuum drying to obtain a final product.

The invention has the beneficial effects that:

(1) the invention provides a preparation method of cobalt-nickel bimetallic MOF nanotubes, which is simple and easy to operate and does not need special equipment;

(2) the cobalt-nickel bimetallic MOF nanotube prepared by the method has high product purity, and the preparation efficiency is improved;

(3) the cobalt-nickel bimetallic MOF nanotube prepared by the method has the characteristic of high specific surface area, and has good application value in the fields of dye adsorption, photocatalysis and the like;

(4) the raw materials used in the invention are cheap, the material synthesis cost is low, and the method is suitable for mass production.

Drawings

FIG. 1 is one of a plurality of Transmission Electron Microscope (TEM) photographs of cobalt-nickel bimetallic MOF nanotubes prepared by the method of the present invention taken after observation with a Japanese Electron JEOL-1400 TEM;

FIG. 2 is an X-ray diffraction (XRD) diagram of the cobalt-nickel bimetallic MOF nanotube prepared by the method, and the diffraction peak in the diagram is sharp, so that the purity of the prepared sample is proved to be good.

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.